WO2019235504A1 - Device for residual-monomer removal - Google Patents
Device for residual-monomer removal Download PDFInfo
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- WO2019235504A1 WO2019235504A1 PCT/JP2019/022256 JP2019022256W WO2019235504A1 WO 2019235504 A1 WO2019235504 A1 WO 2019235504A1 JP 2019022256 W JP2019022256 W JP 2019022256W WO 2019235504 A1 WO2019235504 A1 WO 2019235504A1
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- hot water
- water injection
- slurry
- residual monomer
- pressure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/001—Removal of residual monomers by physical means
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F14/02—Monomers containing chlorine
- C08F14/04—Monomers containing two carbon atoms
- C08F14/06—Vinyl chloride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F6/00—Post-polymerisation treatments
- C08F6/24—Treatment of polymer suspensions
Definitions
- a vinyl chloride monomer contained in a mixture of PVC and an aqueous medium (hereinafter abbreviated as PVC slurry) in the production of a vinyl chloride resin (hereinafter abbreviated as PVC).
- PVC slurry an aqueous medium
- the present invention relates to an apparatus and a method for removing a residual monomer from a slurry containing a vinyl chloride resin, which can efficiently remove a residual monomer mainly composed of).
- PVC is used in a wide range of fields because it is a resin with excellent chemical and physical properties.
- PVC is produced by suspension polymerization, emulsion polymerization, bulk polymerization, and the like, but since it has the advantage of easily removing reaction heat and obtaining a product with less impurities, it is particularly suspended. Polymerization methods and emulsion polymerization methods are widely used.
- the suspension polymerization method and the emulsion polymerization method are usually performed by charging VCM together with an aqueous medium, a dispersant or an emulsifier, a polymerization initiator, and the like into a polymerization vessel equipped with a stirrer and polymerizing the mixture with stirring while maintaining a predetermined temperature. Is called.
- the polymerization reaction is usually not carried out until VCM is 100% converted to PVC, and is stopped at a stage where production efficiency is high, that is, a stage where the polymerization conversion is 80 to 95%.
- the residual monomer in the polymerization vessel is separated and recovered from the PVC slurry (mainly a mixed dispersion of PVC particles and an aqueous medium), but the PVC slurry contains several percent of residual monomer. Is normal.
- the aqueous medium is mechanically separated and dried by hot air drying or other various methods to become PVC powder.
- the separated aqueous medium, exhaust by hot air drying, and the obtained PVC powder contain VCM to the extent that it is problematic for environmental hygiene reasons or is clearly recognized as harmful.
- Patent Document 1 and Patent Document 2 are examples of methods for removing and recovering residual monomers from PVC slurry using a processing tower equipped with a plurality of perforated plate shelves inside and a steam injection port at the bottom. .
- the apparatus for removing residual monomer by the above-mentioned monomer removal method has a hot water jetting apparatus provided at least toward the lower surface of the porous plate directly below the porous plate in each chamber. While the PVC slurry is sequentially flowing down along the processing path on the perforated plate, the slurry is moved from the hole of the perforated plate to the lower chamber due to the pressure fluctuation in the chamber due to the decrease in the system temperature or the fluctuation of the steam flow rate. The PVC may fall and clog the holes, and the slurry may scatter and adhere to the wall.
- the hot water injection by the hot water injection device can wash away the slurry adhering to the holes and wall surfaces of the perforated plate, thus preventing these problems.
- the hot water injection device of the residual monomer removing device is an important device, and for example, Patent Document 2 has been proposed for the hot water injection device and method.
- Patent Documents 3 to 5 a cylindrical tower main body, a plurality of perforated plates provided in the vertical direction of the tower main body, and a plurality of porous plates formed on the perforated plates as bottom surfaces, respectively.
- a plurality of perforated plates, a slurry introduction port provided on the upper side of the uppermost perforated plate, and the perforations so as to sequentially flow the slurry from the upper perforated plate to the lower perforated plate.
- a removal device has been proposed.
- this pressure is the hot water injection nozzle provided at the inlet of each chamber.
- the opening degree is adjusted with a manual valve so that the indicated value of the pressure gauge connected to is a predetermined pressure.
- a predetermined pressure may not be ensured due to fluctuations in the outlet pressure of the hot water pump.
- a sight glass is attached to the side of each room. It is installed and the inside can be observed.
- scattered slurry may adhere and the inside becomes difficult to see.
- the cleaning nozzle for cleaning the sight glass is connected from the hot water injection ring, but since it is connected from the lower side of the hot water injection ring, the hot water in the hot water injection ring is not removed even after the hot water injection cleaning is completed. Since the hot water drips from the sight glass washing nozzle until it comes off and hits the sight glass, the inside cannot be observed until the hot water in the hot water injection ring is removed.
- the configuration of the residual monomer removing apparatus of the present invention is as follows.
- a cylindrical tower body 4 a plurality of perforated plates 34 provided in the vertical direction in the tower body, a plurality of chambers 16 to 21 formed on each of the perforated plates as a bottom surface, and a slurry introduction pipe 22, 23, a downflow pipe 36 for sequentially flowing the slurry downward from the perforated plate in the upper chamber, a water vapor introduction pipe 10 provided at the bottom of the tower body, and a gas outlet 11 at the top of the tower body It is effective for a hot water injection device including the condensing device 6 provided, the slurry discharge port 24 provided in the lowermost porous plate, and a hot water injection ring 38 immediately below the porous plate and including the hot water injection ring.
- a device for adjusting the pressure (the pressure control valve 32 or the hot water pump 8 with an inverter control function), and the upper part of the hot water injection ring 38 of the hot water injection device Or phosphorus
- the present invention includes the following items.
- a cylindrical tower body and a plurality of perforated plates provided in the vertical direction of the tower body; A plurality of chambers formed on each of the porous plates as a bottom surface; A slurry inlet provided above the uppermost porous plate among the plurality of porous plates; A lower part provided between the perforated plates so as to sequentially flow the slurry from the perforated plate of the upper chamber to the perforated plate of the lower chamber; A water vapor inlet provided at the bottom of the tower body; A condenser provided outside the tower body via a gas transfer pipe in the tower top chamber of the tower body; A slurry outlet provided in a lowermost porous plate among the plurality of porous plates; It has a hot water injection device provided directly below the perforated plate toward the lower surface of the perforated plate, In the residual monomer removing apparatus for removing the residual monomer from the polyvinyl chloride-containing slurry containing the residual monomer after the completion
- the residual monomer is removed from the polyvinyl chloride-containing slurry containing the residual monomer after completion of the polymerization, and the injection pressure in the hot water injection device is set to a predetermined pressure. Therefore, the hot water injection pressure can be adjusted by installing a pressure control valve or by controlling the output of the hot water pump with inverter control. In addition, the use of an inverter leads to energy saving.
- each chamber is observed by installing a cleaning nozzle for cleaning the sight glass in each chamber on the hot water injection ring provided in the hot water injection device. can do.
- the cleaning nozzle for cleaning the sight glass included in the hot water injection ring is a nozzle inserted from the lower side or connected from the upper side of the hot water injection ring, It is possible to observe the internal state of each chamber without waiting for the hot water accumulated in the hot water injection ring to escape from the washing nozzle. Also, by storing hot water in the hot water injection ring, the difference between the indoor temperature and the hot water temperature in the hot water injection ring is reduced. Leads to prevention.
- FIG. 3 is a detailed view of the residual monomer removal treatment tower. It is a hot water injection ring expansion longitudinal cross-sectional view. It is the whole warm water injection ring seen from the upper surface. It is a longitudinal cross-sectional view of the sight glass washing pipe
- FIG. 3 is a longitudinal sectional view of a sight glass cleaning tube inserted and connected from the lower part of a hot water injection ring.
- This device has a cylindrical tower body 4, a plurality of porous plates 34 provided in the vertical direction of the tower body 4, each having a large number of pores, and the porous plate as a bottom surface.
- 23, a downflow pipe 36 provided between the perforated plates so as to sequentially flow the slurry from the perforated plate in the upper chamber to the perforated plate in the lower chamber, and the water vapor introducing pipe 10 provided at the bottom of the tower body.
- a hot water injection ring 38 as a hot water injection means installed directly below each porous plate is provided directly below the porous plate.
- the inner diameter of the tower body 4 is 200 to 10,000 mm, and the height of the tower is 2 to 20 times, more preferably 5 to 15 times the inner diameter. If necessary, the inner diameters of the chambers in the tower may be different.
- a tower bottom and a perforated plate, a perforated plate and a perforated plate located immediately above the perforated plate, or a space defined by the perforated plate and the top of the tower is referred to as a chamber.
- the number of chambers required for residual monomer treatment is determined by the residence time required when removing residual monomer from the PVC slurry.
- Perforated plate Each of the perforated plate 34 having a large number of pores has several dam plates 35 provided vertically on the surface thereof, and forms a chamber (space) between the lower surface of the upper perforated plate.
- the pores of the perforated plate are opened so that the monomer removal treatment is performed by water vapor injected from the pores when the PVC slurry flows on the perforated plate.
- the size of the pores is such that the PVC slurry does not flow down through the pores, and the pores are not clogged, and the water vapor pressure and the amount of water vapor introduced so that the water vapor injected from below constantly passes uniformly. Is set in consideration of
- the pores opened in the perforated plate have a diameter of 5 mm or less, preferably 0.5 to 2 mm, more preferably 0.7 to 1.5 mm.
- the aperture ratio (total pore area / porous plate area) of the porous plate is 0.001 to 10%, preferably 0.04 to 4%, more preferably 0.2 to 2%.
- the opening ratio is within this range, the PVC particles existing in the PVC slurry flowing on the perforated plate shelf are sufficiently stirred, so that the residual monomers are removed from the PVC particles by the PVC particles settling.
- the efficiency can be prevented from decreasing and the fluidity of the PVC slurry can be prevented from decreasing.
- the dam plate 35 is for ensuring a processing passage through which the PVC slurry can flow on the perforated plate.
- weir plates are installed alternately, The PVC slurry flows on the perforated shelves for a certain period of time by the processing passage formed by the weir plate, and during that time, the PVC slurry is subjected to the demonomer treatment with water vapor supplied from below.
- Hot water injection apparatus Moreover, the hot water injection apparatus is installed in the tower main body 4 of the residual monomer removal apparatus of this invention.
- a hot water injection ring 38 as a hot water injection device forms a pipe into a predetermined shape (FIG. 4) and is provided directly below the perforated plate 34, respectively. Clean the bottom of the plate and the inner wall of the tower.
- the number of spray nozzles and the position of the nozzle hole 39 are not particularly limited, but it is preferable that the intersecting angles a and b (FIG. 3) with the vertical line of the spray nozzle are set in the range of 10 to 60 degrees.
- the pressure difference between the pressure in the hot water jet ring and the pressure in the room in which the hot water is jetted is 0.02 MPaG or more, preferably 0.05 MPaG or more. Is appropriate. If the differential pressure is within this range, the hot water injection pressure control with which a sufficient washing effect can be obtained without increasing the hot water consumption can be achieved by automatically controlling the hot water circulation line pressure by converting the hot water pump 8 into an inverter, or This is possible by automatically controlling the pressure control valve 32.
- the sight glass 33 cleaning tube 37 is suitably connected from the upper part of the hot water injection ring 38 as shown in FIG. 5, or inserted from the lower part of the hot water injection ring 38 as shown in FIG. .
- the hot water remaining in the hot water cleaning ring hangs down from the sight glass cleaning nozzle and hits the sight glass even after the cleaning is completed, so that the inside cannot be observed from the sight glass.
- the temperature difference between the room temperature and the temperature of the hot water is large, the room temperature fluctuates and the pressure fluctuates at the time of cleaning, so that the upper or lower porous plate may cause liquid leakage.
- hot water is stored in the hot water injection ring by connecting the sight glass cleaning tube from the upper part of the hot water injection ring or inserting it from the lower part of the hot water injection ring, the temperature difference between the room and the hot water in the ring will be Since it becomes smaller, it leads to prevention of liquid leakage from the perforated plate.
- Hot water injection ring The shape of the pipe of the hot water injection ring 38 as a hot water injection device is usually like the Greek letter ⁇ type or ⁇ type or spiral type, star type or sheep intestine type (ninety nine folds). A multiple ring type (FIG. 4) having the same center alternately may be used.
- the hot water injection ring 38 may be installed parallel to the perforated plate 34 and stored inside the tower. However, if the hot water injection ring 38 is too close to the inner wall of the tower main body, the washed away PVC particles may block the gap. It is good to install so that the outer diameter may be at a distance of 20 mm or more away from the inner wall to the inside.
- the outer diameter of the hot water injection ring 38 is preferably 150 to 8000 mm.
- the flow rate of the PVC slurry introduced into the tower is preferably adjusted to be 0.1 to 300 m 3 / h (more preferably 1 to 100 m 3 / h) per 1 m 2 of the area of the porous plate 34.
- the PVC slurry introduced into the tower is preferably preheated to 50 to 100 ° C. by the heat exchanger 3. This preheating improves the residual monomer removal efficiency.
- the difficulty of removing the monomer from the PVC slurry is due to the structure of the PVC particles in the PVC slurry. When the pore volume ratio in the PVC particles is large, the contact between the PVC particles and water vapor is good and the monomer is easily removed, and when the pore volume ratio is small, the monomer removal is difficult.
- the residence time of the PVC slurry in the tower is determined by the degree of difficulty of depolymerization of the PVC slurry as described above, the unreacted monomer concentration contained in the PVC slurry introduced into the tower, and the treatment at the PVC slurry outlet 24. It is determined by the set value of the residual monomer concentration later.
- the residence time of the PVC slurry in the tower is long, residual monomers can be removed from the PVC particles present in the PVC slurry to a high degree.
- the residence time is too long, the PVC particles are colored due to thermal deterioration. Therefore, it is not preferable to contact the PVC slurry with water vapor more than necessary. Therefore, it is necessary to adjust the residence time in accordance with the degree of difficulty of the monomer removal of the PVC slurry.
- the PVC slurry introduced into the tower main body from the slurry introduction pipe 22 or 23 as the slurry introduction part passes through the processing passage defined by the weir plate 35 on the porous plate 34, passes through the flow down pipe 36, and the chamber below it. Is introduced onto the perforated plate 34.
- the slurry introduced onto the perforated plate 34 subsequently passes on the treatment path on the perforated plate 34 and further flows through the flow down pipe 36 onto the perforated plate 34 below. After passing through the processing passage to the lowermost porous plate 34 in this way, it is discharged from the PVC slurry discharge port 24 provided in the lowermost porous plate 34 to the outside of the tower.
- the porous plate 34 in the present invention is not particularly limited in the number of the dam plates 35 and the width of the processing passage.
- the height of the flowing PVC increases and exceeds the dam plate. Since the slurry is mixed, it is necessary to appropriately set the number of dam plates and the width of the processing passage in order to prevent deterioration of the product quality.
- a water vapor introduction pipe 10 is connected to the tower bottom chamber 15, and the water vapor injected from the water vapor introduction port 10 flows into the PVC slurry flowing on the porous shelf plate through the pores of the porous plate. Infused.
- the amount of water vapor introduced at this time is 1 to 100 kg / h, preferably 5 to 50 kg / h, per 1 m 3 of the PVC slurry. If the amount of introduced steam is within this range, the residual monomer in the PCV slurry can be efficiently removed without settling of the PVC particles in the PVC slurry. Moreover, if the amount of introduced steam is within this range, the occurrence of splashing of the PVC slurry is suppressed, and no flooding occurs. Moreover, if the amount of introduced steam is within this range, the balance between the amount of introduced steam and the effect of removing residual monomers in the PVC slurry is good.
- adjusting the temperature of the PVC slurry leads to obtaining high-quality PVC.
- the water vapor temperature, the amount of water vapor introduced, and the pressure in the tower are adjusted so that the temperature of the slurry flowing on the perforated plate is 50 to 150 ° C., preferably 70 to 120 ° C., more preferably 80 to 110 ° C. It is desirable. If the temperature of the PVC slurry is within this range, it is possible to prevent the coloring due to thermal degradation of the PVC particles and maintain high quality while maintaining the removal efficiency of the residual monomer.
- the mixed gas of the monomer gas and water vapor removed in the residual monomer removing apparatus flows into the condenser 6 through the gas transfer pipe connected to the tower top chamber 21, where most of the water vapor is condensed and condensed water. Is dropped back into the residual monomer removal treatment tower. At that time, the mixed gas of the monomer gas and water vapor rising from the tower top chamber comes into countercurrent contact with the flowing condensed water, and the condensed water is heated. Furthermore, the loss of energy can be prevented by introducing the cooling water 13 introduced into the condenser 6 from the condenser 6 to the hot water tank 7 through the cooling water outlet hot water supply pipe 14 and using it as hot water for hot water washing.
- the PVC slurry from which the residual monomer has been removed by the residual monomer removal processing tower 4 is discharged from the PVC slurry discharge port 24 and fed into the pump 9. Thereafter, the PVC slurry passes through the heat exchanger 3 and is stored in the PVC slurry tank.
- the hot water injection process using the hot water injection device in the residual monomer removal treatment tower is performed during the PVC slurry feed and during the washing water feed after the feed is completed.
- the hot water jet cleaning is performed in order from the lower chamber 16 to the upper chamber.
- the cleaning of the chamber 16 is started again.
- the chamber 15 when the hot water jet cleaning valve 31 in the tower bottom chamber is opened during the PVC slurry feed and the hot water jet cleaning is performed, the temperature in the chamber 15 is lowered and the pressure is also lowered. Since leakage occurs, hot water jet cleaning is not performed during PVC slurry feed.
- Example 1 Hot water jet pressure control by inverter control of hot water pump output
- the hot water pump 8 is started and the inverter output has a minimum value of 100 m 3 / h which is a circulation amount that can keep the temperature distribution in the hot water tank 7 uniform.
- the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the indoor pressure is 0.05 MPaG to 0.08 MPaG. Automatically control the output.
- the inverter output control of the hot water pump 8 is switched to the manual mode, and the output value is fixed at the current output value. Then, the hot water jet cleaning valve 30 in the chamber 16 is opened for 8 seconds. 4).
- the inverter output of the warm water pump 8 is returned to the minimum value of 100 m 3 / h, which is a circulation amount that can keep the temperature distribution in the warm water tank 7 uniform, and this state is maintained for 2 to 10 minutes. 5).
- the hot water jet cleaning valve 29 By opening and closing the hot water jet cleaning valve 29 one stage higher by the same operation as the above 2 to 4, the lower side of the perforated plate under the chamber 17 and the chamber 18 is cleaned. 6). The same operations as in 2 to 5 above are repeated, and hot water jet cleaning is performed in order from the lower chamber to the upper chamber.
- Example 2 Control of hot water jet pressure by control of circulating pressure control valve
- the hot water pump 8 is started and the circulation pressure control valve 32 opening output is fully opened.
- the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the room pressure becomes an appropriate pressure, and the circulation pressure control valve 32 opening output is automatically controlled.
- the circulation pressure control valve 32 is switched to the manual mode, and the opening degree output value is fixed.
- the hot water jet cleaning valve 30 in the chamber 16 is opened for 8 seconds. 4). After the warm water jet cleaning valve 30 is closed, the circulation pressure control valve 32 opening output is fully opened. Keep this state for 2-10 minutes. 5).
- Example 3 (Washing with a sight glass washing tube connected from the top of the hot water injection ring) The cleaning of the sight glass 33 in each chamber is performed simultaneously with the hot water jet cleaning in each chamber. Since the sight glass cleaning tube is connected from the upper part of the hot water jet ring, the hot water will not hang down from the sight glass cleaning nozzle indefinitely after the hot water jet cleaning is completed. In addition, since warm water is stored in the warm water jet ring, the temperature difference between the room during washing and the warm water in the ring is as small as 1 ° C. or less, and no liquid leaks from the porous plate.
- Example 4 (Washing with a sight glass washing tube inserted from the bottom of the hot water injection ring and connected) Similar to the third embodiment, when the hot water jet cleaning is completed, the hot water does not hang down from the sight glass cleaning nozzle indefinitely. Moreover, liquid leakage from the perforated plate does not occur.
- a pressure gauge and a manual valve are provided at the hot water injection ring inlet provided at the inlet of each chamber in order to ensure an appropriate hot water injection pressure at the time of hot water jet cleaning.
- the opening degree was adjusted with a manual valve so that the predetermined pressure was 0.05 MPaG to 0.08 MPaG.
- a predetermined pressure may not be ensured due to fluctuations in the outlet pressure of the hot water pump.
- the hot water circulation line requires an automatic valve for shutoff in the return line to ensure the hot water circulation pressure.
- the sight glass cleaning pipe is connected to the lower side of the hot water injection ring, so even if the hot water injection cleaning is completed, the hot water in the hot water injection ring is completely discharged until the sight glass cleaning nozzle is removed. Hot water dripped from it, hitting the sight glass, and the inside could not be observed. Also, depending on the chamber, the temperature difference between the hot water in the chamber and the ring is as large as 5 ° C. or more, and thus liquid leakage of the porous plate occurred during hot water jet cleaning.
- the residual monomer removing apparatus of the present invention can be used for a vinyl chloride resin manufacturing apparatus.
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Abstract
A device for residual-monomer removal by which residual monomers can be efficiently removed from a slurry containing a vinyl-chloride-based resin, while preventing the residual monomers from being discharged from the process. The device for residual-monomer removal comprises: a column body 4; a plurality of perforated plates 34 disposed along the vertical direction within the column body; a plurality of chambers 16-21 formed respectively over the perforated plates serving as bottom surfaces; slurry introduction pipes 22 and 23; flow pipes 36 for causing the slurry to flow downward successively from the perforated plate beneath an upper chamber; a steam introduction pipe 10 disposed in the bottom part of the column body; a condenser 6 disposed over the upper part of the column body, with a gas discharge port 11 disposed therebetween; a slurry discharge port 24 provided to the lowermost perforated plate; and warm-water ejectors disposed just beneath the perforated plates and each including a warm-water ejection ring 38. Each warm-water ejector is provided with: a pressure gauge 40 for monitoring the ejection pressure to effectively conduct the ejection; a device for adjusting the pressure (a pressure control valve 32 or a warm-water pump 8 with inverter control); and a sight-glass-washing nozzle 37 connected to the upper part of the warm-water ejection ring 38 of the warm-water ejector or inserted into the ring.
Description
本発明は、塩化ビニル系樹脂（以下、ＰＶＣと略称する。）の製造に際し、ＰＶＣと水性媒体の混合物（以下、ＰＶＣスラリーと略称する。）に含まれる塩化ビニルモノマー（以下、ＶＣＭと略称する）等を主とする残留モノマーを効率よく除去することができる、塩化ビニル系樹脂含有スラリーからの残留モノマー除去装置および除去方法に関するものである。
In the present invention, a vinyl chloride monomer (hereinafter abbreviated as VCM) contained in a mixture of PVC and an aqueous medium (hereinafter abbreviated as PVC slurry) in the production of a vinyl chloride resin (hereinafter abbreviated as PVC). The present invention relates to an apparatus and a method for removing a residual monomer from a slurry containing a vinyl chloride resin, which can efficiently remove a residual monomer mainly composed of).
ＰＶＣは、化学的にも物理的にも優れた特性を備えた樹脂であることから、幅広い分野に使用されている。一般に、ＰＶＣは、懸濁重合法、乳化重合法、塊状重合法等によって製造されるが、反応熱を除去しやすく、不純物の少ない製品を得ることができるという利点があることから、特に懸濁重合法や乳化重合法が広く用いられている。
PVC is used in a wide range of fields because it is a resin with excellent chemical and physical properties. In general, PVC is produced by suspension polymerization, emulsion polymerization, bulk polymerization, and the like, but since it has the advantage of easily removing reaction heat and obtaining a product with less impurities, it is particularly suspended. Polymerization methods and emulsion polymerization methods are widely used.
懸濁重合法や乳化重合法は、通常、ＶＣＭを、水性媒体、分散剤または乳化剤、および重合開始剤等と共に攪拌機付き重合器内に仕込み、所定温度に保ちながら攪拌下に重合させることによって行われる。重合反応は、通常、ＶＣＭが１００％転化してＰＶＣとなるまで実施されることはなく、製造効率の良い段階、すなわち重合転化率８０～９５％の段階で停止される。重合反応終了後、重合器内の残留モノマーはＰＶＣスラリー（主としてＰＶＣ粒子と水性媒体の混合分散液）と分離して回収されるが、ＰＶＣスラリーには数％の残留モノマーが含まれているのが普通である。
The suspension polymerization method and the emulsion polymerization method are usually performed by charging VCM together with an aqueous medium, a dispersant or an emulsifier, a polymerization initiator, and the like into a polymerization vessel equipped with a stirrer and polymerizing the mixture with stirring while maintaining a predetermined temperature. Is called. The polymerization reaction is usually not carried out until VCM is 100% converted to PVC, and is stopped at a stage where production efficiency is high, that is, a stage where the polymerization conversion is 80 to 95%. After the polymerization reaction is completed, the residual monomer in the polymerization vessel is separated and recovered from the PVC slurry (mainly a mixed dispersion of PVC particles and an aqueous medium), but the PVC slurry contains several percent of residual monomer. Is normal.
このように、残留モノマーを含むＰＶＣスラリーは、水性媒体が機械的に分離され、熱風乾燥その他種々の方法で乾燥されてＰＶＣ粉末となる。このとき、分離された水性媒体、熱風乾燥による排気、および得られたＰＶＣ粉末には、環境衛生上の理由で問題となるか、または明らかに有害と認められる程度のＶＣＭが含まれる。
Thus, in the PVC slurry containing the residual monomer, the aqueous medium is mechanically separated and dried by hot air drying or other various methods to become PVC powder. At this time, the separated aqueous medium, exhaust by hot air drying, and the obtained PVC powder contain VCM to the extent that it is problematic for environmental hygiene reasons or is clearly recognized as harmful.
このような製造上生じる排出物およびＰＶＣ粉末中のＶＣＭを完全に除去するか、または環境衛生上無害な程度までその含有量を低下させるために、種々の方法が提案されている。例えば、内部に複数の多孔板製棚段と底部に水蒸気噴入口を装着した処理塔を用いて、ＰＶＣスラリーから残留モノマーを除去回収する方法としては、例えば特許文献１および特許文献２があげられる。
Various methods have been proposed in order to completely remove the effluent generated in the production and the VCM in the PVC powder, or to reduce the content thereof to a degree that is not harmful to environmental hygiene. For example, Patent Document 1 and Patent Document 2 are examples of methods for removing and recovering residual monomers from PVC slurry using a processing tower equipped with a plurality of perforated plate shelves inside and a steam injection port at the bottom. .
これらの方法は、底面が多孔板で構成され、該多孔板上に千鳥状の処理通路をなすように堰板が設置された多孔板製棚段を用い、ＰＶＣスラリーを、これらの多孔板製棚段上の処理通路に沿って順次流下させ、その間に、ＰＶＣスラリーを、多孔板の細孔を通じて、下から噴入してくる水蒸気に曝し、ＰＶＣスラリーが含有している残留モノマーを蒸発分離するものである。
These methods use a perforated plate shelf having a bottom surface made of a perforated plate, and a weir plate installed on the perforated plate so as to form a staggered processing passage, and the PVC slurry is made of these perforated plates. The PVC slurry is allowed to flow down sequentially along the processing path on the shelf, while the PVC slurry is exposed to water vapor injected from below through the pores of the perforated plate, and the residual monomer contained in the PVC slurry is evaporated and separated. To do.
一般に、このように残留モノマーを除去回収する方法を脱モノマー法といい、現在では、この脱モノマー法が主流を占めている。
上記脱モノマー法による残留モノマー除去装置には、各室の多孔板の真下に少なくとも該多孔板の下面に向けて設けられた温水噴射装置を有している。ＰＶＣスラリーを、多孔板上の処理通路に沿って順次流下させている間に、系内温度の低下または蒸気流量の変動等により、室内の圧力変動によってスラリーが多孔板の孔から下の室に降下してＰＶＣが孔に詰まることがあり、またスラリーが壁面に飛び散って付着することがある。そのままにしておくと、多孔板の孔が閉塞し水蒸気の吹込みが不均一となるため運転が不安定となりＰＶＣスラリー中の残留モノマー除去が不十分となる。また、壁面に付着したＰＶＣは熱によって変色し異物コンタミとして品質に悪い影響を与える。温水噴射装置による温水噴射は、多孔板の孔や壁面に付着したスラリーを洗い流すことができるため、これらの問題を防止している。 In general, such a method of removing and recovering residual monomers is called a demonomer method, and at present, this demonomer method dominates.
The apparatus for removing residual monomer by the above-mentioned monomer removal method has a hot water jetting apparatus provided at least toward the lower surface of the porous plate directly below the porous plate in each chamber. While the PVC slurry is sequentially flowing down along the processing path on the perforated plate, the slurry is moved from the hole of the perforated plate to the lower chamber due to the pressure fluctuation in the chamber due to the decrease in the system temperature or the fluctuation of the steam flow rate. The PVC may fall and clog the holes, and the slurry may scatter and adhere to the wall. If it is left as it is, the holes of the perforated plate are closed and the water vapor is not uniformly blown, so that the operation becomes unstable, and the residual monomer removal in the PVC slurry becomes insufficient. In addition, PVC attached to the wall surface is discolored by heat and has a bad influence on quality as foreign matter contamination. The hot water injection by the hot water injection device can wash away the slurry adhering to the holes and wall surfaces of the perforated plate, thus preventing these problems.
上記脱モノマー法による残留モノマー除去装置には、各室の多孔板の真下に少なくとも該多孔板の下面に向けて設けられた温水噴射装置を有している。ＰＶＣスラリーを、多孔板上の処理通路に沿って順次流下させている間に、系内温度の低下または蒸気流量の変動等により、室内の圧力変動によってスラリーが多孔板の孔から下の室に降下してＰＶＣが孔に詰まることがあり、またスラリーが壁面に飛び散って付着することがある。そのままにしておくと、多孔板の孔が閉塞し水蒸気の吹込みが不均一となるため運転が不安定となりＰＶＣスラリー中の残留モノマー除去が不十分となる。また、壁面に付着したＰＶＣは熱によって変色し異物コンタミとして品質に悪い影響を与える。温水噴射装置による温水噴射は、多孔板の孔や壁面に付着したスラリーを洗い流すことができるため、これらの問題を防止している。 In general, such a method of removing and recovering residual monomers is called a demonomer method, and at present, this demonomer method dominates.
The apparatus for removing residual monomer by the above-mentioned monomer removal method has a hot water jetting apparatus provided at least toward the lower surface of the porous plate directly below the porous plate in each chamber. While the PVC slurry is sequentially flowing down along the processing path on the perforated plate, the slurry is moved from the hole of the perforated plate to the lower chamber due to the pressure fluctuation in the chamber due to the decrease in the system temperature or the fluctuation of the steam flow rate. The PVC may fall and clog the holes, and the slurry may scatter and adhere to the wall. If it is left as it is, the holes of the perforated plate are closed and the water vapor is not uniformly blown, so that the operation becomes unstable, and the residual monomer removal in the PVC slurry becomes insufficient. In addition, PVC attached to the wall surface is discolored by heat and has a bad influence on quality as foreign matter contamination. The hot water injection by the hot water injection device can wash away the slurry adhering to the holes and wall surfaces of the perforated plate, thus preventing these problems.
このように、該残留モノマー除去装置の温水噴射装置は重要な装置であり、該温水噴射装置及び方法については、例えば特許文献２が提案されている。
Thus, the hot water injection device of the residual monomer removing device is an important device, and for example, Patent Document 2 has been proposed for the hot water injection device and method.
さらに、近年、特許文献３から５のような、筒状の塔本体と、該塔本体の垂直方向に設けられた複数の多孔板と、該多孔板をそれぞれ底面としてその上に形成された複数の室と、前記複数の多孔板のうち最上部の多孔板の上側に設けられたスラリー導入口と、上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように前記多孔板間に設けられた流下部と、塔本体の底部に設けられた水蒸気導入口と、塔本体の塔頂室にガス移送管を介して該塔本体の外部に設けられた凝縮装置と、前記複数の多孔板のうち最下部の多孔板に設けられたスラリー排出口と、多孔板の真下に、少なくとも該多孔板の下面に向けて設けられた温水噴射装置とを有している、残留モノマー除去装置が提案されている。
Furthermore, in recent years, as in Patent Documents 3 to 5, a cylindrical tower main body, a plurality of perforated plates provided in the vertical direction of the tower main body, and a plurality of porous plates formed on the perforated plates as bottom surfaces, respectively. A plurality of perforated plates, a slurry introduction port provided on the upper side of the uppermost perforated plate, and the perforations so as to sequentially flow the slurry from the upper perforated plate to the lower perforated plate. A lower part provided between the plates, a water vapor inlet provided at the bottom of the tower body, a condenser provided outside the tower body via a gas transfer pipe in the tower top chamber of the tower body, Residual monomer having a slurry discharge port provided in a lowermost porous plate among a plurality of porous plates, and a hot water injection device provided at least toward the lower surface of the porous plate immediately below the porous plate A removal device has been proposed.
その中で、温水噴射洗浄時は適切な温水噴射量を確保するために、各室の温水噴射圧力を維持することが必要となるが、この圧力は、各室入口に設けられた温水噴射ノズルに接続された圧力計の指示値が所定の圧力になるように手動弁で開度を調整している。しかしながら、温水ポンプの出口圧力の変動により、所定の圧力を確保できない場合があった。
Among them, it is necessary to maintain the hot water injection pressure in each chamber in order to secure an appropriate hot water injection amount during hot water injection cleaning, and this pressure is the hot water injection nozzle provided at the inlet of each chamber. The opening degree is adjusted with a manual valve so that the indicated value of the pressure gauge connected to is a predetermined pressure. However, a predetermined pressure may not be ensured due to fluctuations in the outlet pressure of the hot water pump.
また、残留モノマー除去装置の定期的な運転状態の確認や運転が不安定になったとき等に、各室内部のスラリーレベルやバブリング状態を目視で確認するため、各室の側面にサイトグラスが設置されており、内部を観察することができる。しかし、サイトグラスは、飛散したスラリーが付着することがあり内部が見えづらくなる。そのためサイトグラスを洗浄するための洗浄ノズルを、温水噴射リングから接続しているが、温水噴射リングの下側から接続しているため、温水噴射洗浄が終了しても、温水噴射リング内の温水が抜けるまでサイトグラス洗浄ノズルから温水が垂れてそれがサイトグラスに当たるので、温水噴射リング内の温水が抜けるまで内部を観察することができない。
In addition, in order to visually check the slurry level and bubbling state in each room when the operation status of the residual monomer removal device is regularly checked or unstable, a sight glass is attached to the side of each room. It is installed and the inside can be observed. However, in the sight glass, scattered slurry may adhere and the inside becomes difficult to see. For this reason, the cleaning nozzle for cleaning the sight glass is connected from the hot water injection ring, but since it is connected from the lower side of the hot water injection ring, the hot water in the hot water injection ring is not removed even after the hot water injection cleaning is completed. Since the hot water drips from the sight glass washing nozzle until it comes off and hits the sight glass, the inside cannot be observed until the hot water in the hot water injection ring is removed.
さらに、室内の温度と温水の温度の温度差が大きいときは、洗浄時に室内の温度が変動し圧力も変動するため、その室の上の多孔板或いは下の多孔板が液漏れを起こすことがある。
Furthermore, when the temperature difference between the room temperature and the temperature of the hot water is large, the room temperature fluctuates and the pressure fluctuates during cleaning, and the porous plate above or below the chamber may cause liquid leakage. is there.
残留モノマーを工程外に排出することを防止しながら、且つ塩化ビニル系樹脂含有スラリーから残留モノマーを効率よく除去することができる残留モノマー除去装置が求められている。
There is a need for a residual monomer removal apparatus that can efficiently remove residual monomer from a slurry containing vinyl chloride resin while preventing residual monomer from being discharged out of the process.
本発明の残留モノマー除去装置の構成は以下のとおりである。筒状の塔本体４と、該塔本体内の垂直方向に設けられた複数の多孔板３４と、該多孔板をそれぞれ底面としてその上に形成された複数の室１６～２１と、スラリー導入管２２，２３と、上方の室の多孔板から下方へスラリーを順次流下させる流下管３６と、塔本体の底部に設けられた水蒸気導入管１０と、塔本体の上部にガス排出口１１を介して設けられた凝縮装置６と、最下部の多孔板に設けられたスラリー排出口２４と、多孔板の真下に、温水噴射リング３８を有し、且つ温水噴射リングを含む温水噴射装置には効果的に行うための噴射圧力監視用の圧力計４０と、その圧力を調整する為の装置（圧力制御弁３２、またはインバーター制御機能付き温水ポンプ８）、さらに温水噴射装置の温水噴射リング３８上部から接続した或いはリング内に挿入したサイトグラス洗浄ノズル３７を設ける。
The configuration of the residual monomer removing apparatus of the present invention is as follows. A cylindrical tower body 4, a plurality of perforated plates 34 provided in the vertical direction in the tower body, a plurality of chambers 16 to 21 formed on each of the perforated plates as a bottom surface, and a slurry introduction pipe 22, 23, a downflow pipe 36 for sequentially flowing the slurry downward from the perforated plate in the upper chamber, a water vapor introduction pipe 10 provided at the bottom of the tower body, and a gas outlet 11 at the top of the tower body It is effective for a hot water injection device including the condensing device 6 provided, the slurry discharge port 24 provided in the lowermost porous plate, and a hot water injection ring 38 immediately below the porous plate and including the hot water injection ring. Connected to the pressure gauge 40 for monitoring the injection pressure, a device for adjusting the pressure (the pressure control valve 32 or the hot water pump 8 with an inverter control function), and the upper part of the hot water injection ring 38 of the hot water injection device Or phosphorus The sight glass cleaning nozzles 37 inserted within provided.
上記課題を解決するため、本発明は以下の項を含む。
［１］筒状の塔本体と
該塔本体の垂直方向に設けられた複数の多孔板と、
該多孔板をそれぞれ底面としてその上に形成された複数の室と、
前記複数の多孔板のうち最上部の多孔板の上側に設けられたスラリー導入口と、
上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように前記多孔板間に設けられた流下部と、
塔本体の底部に設けられた水蒸気導入口と、
塔本体の塔頂室にガス移送管を介して該塔本体の外部に設けられた凝縮装置と、
前記複数の多孔板のうち最下部の多孔板に設けられたスラリー排出口と、
多孔板の真下に、少なくとも該多孔板の下面に向けて設けられた温水噴射装置と
を有している、
重合終了後の残留モノマーを含むポリ塩化ビニル含有スラリーから残留モノマーを除去する、残留モノマー除去装置において、
その温水噴射装置には、適切な噴射量の温水を噴射するために、噴射圧力を監視する圧力計、及びその噴射圧力を制御する為の装置を装着する
ことを特徴とする、残留モノマー除去装置。 In order to solve the above problems, the present invention includes the following items.
[1] A cylindrical tower body and a plurality of perforated plates provided in the vertical direction of the tower body;
A plurality of chambers formed on each of the porous plates as a bottom surface;
A slurry inlet provided above the uppermost porous plate among the plurality of porous plates;
A lower part provided between the perforated plates so as to sequentially flow the slurry from the perforated plate of the upper chamber to the perforated plate of the lower chamber;
A water vapor inlet provided at the bottom of the tower body;
A condenser provided outside the tower body via a gas transfer pipe in the tower top chamber of the tower body;
A slurry outlet provided in a lowermost porous plate among the plurality of porous plates;
It has a hot water injection device provided directly below the perforated plate toward the lower surface of the perforated plate,
In the residual monomer removing apparatus for removing the residual monomer from the polyvinyl chloride-containing slurry containing the residual monomer after the completion of the polymerization,
The hot water injection device is equipped with a pressure gauge for monitoring the injection pressure and a device for controlling the injection pressure in order to inject an appropriate amount of hot water, and a residual monomer removing device. .
［１］筒状の塔本体と
該塔本体の垂直方向に設けられた複数の多孔板と、
該多孔板をそれぞれ底面としてその上に形成された複数の室と、
前記複数の多孔板のうち最上部の多孔板の上側に設けられたスラリー導入口と、
上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように前記多孔板間に設けられた流下部と、
塔本体の底部に設けられた水蒸気導入口と、
塔本体の塔頂室にガス移送管を介して該塔本体の外部に設けられた凝縮装置と、
前記複数の多孔板のうち最下部の多孔板に設けられたスラリー排出口と、
多孔板の真下に、少なくとも該多孔板の下面に向けて設けられた温水噴射装置と
を有している、
重合終了後の残留モノマーを含むポリ塩化ビニル含有スラリーから残留モノマーを除去する、残留モノマー除去装置において、
その温水噴射装置には、適切な噴射量の温水を噴射するために、噴射圧力を監視する圧力計、及びその噴射圧力を制御する為の装置を装着する
ことを特徴とする、残留モノマー除去装置。 In order to solve the above problems, the present invention includes the following items.
[1] A cylindrical tower body and a plurality of perforated plates provided in the vertical direction of the tower body;
A plurality of chambers formed on each of the porous plates as a bottom surface;
A slurry inlet provided above the uppermost porous plate among the plurality of porous plates;
A lower part provided between the perforated plates so as to sequentially flow the slurry from the perforated plate of the upper chamber to the perforated plate of the lower chamber;
A water vapor inlet provided at the bottom of the tower body;
A condenser provided outside the tower body via a gas transfer pipe in the tower top chamber of the tower body;
A slurry outlet provided in a lowermost porous plate among the plurality of porous plates;
It has a hot water injection device provided directly below the perforated plate toward the lower surface of the perforated plate,
In the residual monomer removing apparatus for removing the residual monomer from the polyvinyl chloride-containing slurry containing the residual monomer after the completion of the polymerization,
The hot water injection device is equipped with a pressure gauge for monitoring the injection pressure and a device for controlling the injection pressure in order to inject an appropriate amount of hot water, and a residual monomer removing device. .
［２］噴射圧力を制御する為の装置が、圧力制御弁または温水供給ポンプ出力をインバーター制御化し温水噴射圧力を調節する装置である、［１］記載の残留モノマー除去装置。
[2] The residual monomer removing apparatus according to [1], wherein the apparatus for controlling the injection pressure is an apparatus for adjusting the hot water injection pressure by inverter-controlling the output of the pressure control valve or the hot water supply pump.
［３］前記温水噴射装置に備えられている温水噴射リングに、各室に１箇所以上設置しているサイトグラスを洗浄するための洗浄ノズルを有する［１］または［２］に記載の残留モノマー除去装置。
[3] The residual monomer according to [1] or [2], wherein the hot water injection ring provided in the hot water injection device has a cleaning nozzle for cleaning one or more sight glasses installed in each chamber. Removal device.
［４］前記温水噴射リングに有するサイトグラスを洗浄するための洗浄ノズルが、該温水噴射リングの上側から接続している、［３］に記載の残留モノマー除去装置。
[4] The residual monomer removing apparatus according to [3], wherein a cleaning nozzle for cleaning the sight glass included in the hot water injection ring is connected from the upper side of the hot water injection ring.
［５］前記温水噴射リングに有するサイトグラスの洗浄する為の洗浄ノズルが、該温水噴射リングの内部に挿入されるように接続されている［３］に記載の残留モノマー除去装置。
[5] The residual monomer removing device according to [3], wherein a cleaning nozzle for cleaning the sight glass included in the hot water injection ring is connected to be inserted into the hot water injection ring.
［１］または［２］に記載の発明によれば、重合終了後の残留モノマーを含むポリ塩化ビニル含有スラリーから残留モノマーの除去装置であって、温水噴射装置における噴射圧力を所定の圧力にする為、圧力制御弁の設置または温水ポンプの出力をインバーター制御化することにより温水噴射圧力を調整することができる。また、インバーターを使用することで、省エネにもつながる。
According to the invention described in [1] or [2], the residual monomer is removed from the polyvinyl chloride-containing slurry containing the residual monomer after completion of the polymerization, and the injection pressure in the hot water injection device is set to a predetermined pressure. Therefore, the hot water injection pressure can be adjusted by installing a pressure control valve or by controlling the output of the hot water pump with inverter control. In addition, the use of an inverter leads to energy saving.
［３］に記載の発明によれば、前記温水噴射装置に備えられている温水噴射リングに、各室のサイトグラスを洗浄するための洗浄ノズルを設置したことにより、各室の内部状況を観察することができる。
According to the invention described in [3], the internal state of each chamber is observed by installing a cleaning nozzle for cleaning the sight glass in each chamber on the hot water injection ring provided in the hot water injection device. can do.
［４］または［５］に記載の発明によれば、前記温水噴射リングに有するサイトグラスを洗浄するための洗浄ノズルを下側から挿入したノズルにする事または温水噴射リングの上側から接続したため、温水噴射リング内に溜まった温水が洗浄ノズルから抜けるのを待つことなく、各室の内部状況を観察することができる。また、温水を温水噴射リングに貯めておくことにより室内の温度と該温水噴射リング内の温水温度の差が小さくなるので、温水噴射洗浄時に室内の圧力変動が緩和され、多孔板からの液漏れ防止につながる。
According to the invention described in [4] or [5], since the cleaning nozzle for cleaning the sight glass included in the hot water injection ring is a nozzle inserted from the lower side or connected from the upper side of the hot water injection ring, It is possible to observe the internal state of each chamber without waiting for the hot water accumulated in the hot water injection ring to escape from the washing nozzle. Also, by storing hot water in the hot water injection ring, the difference between the indoor temperature and the hot water temperature in the hot water injection ring is reduced. Leads to prevention.
本発明の残留モノマー除去装置において、ＰＶＣスラリーから残留モノマーを除去する方法を、図１～６に基づいて説明するが、本発明はこれに限定されるのもではない。
The method for removing residual monomer from the PVC slurry in the residual monomer removing apparatus of the present invention will be described with reference to FIGS. 1 to 6, but the present invention is not limited to this.
１．残留モノマー除去装置の構成
この装置は筒状の塔本体４と該塔本体４の垂直方向に設けられた、それぞれ多数の細孔を有する複数の多孔板３４と、該多孔板をそれぞれ底面としてその上に形成された複数の室１６～２１と、前記複数の多孔板のうち塔頂室２１下の多孔板或いは室１９下の多孔板の上側に設けられたスラリー導入部としてのスラリー導入口２２、２３と、上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように該多孔板間に設けられた流下管３６と、塔本体の底部に設けられた水蒸気導入管１０と、塔本体の頂部にガス移送口１１を介して設けられた凝縮器６と、該凝縮器出口に設けられた残留モノマーガス移送管１２と、前記複数の多孔板のうち最下部の多孔板に設けられたＰＶＣスラリー排出口２４と、各多孔板の真下に、該多孔板の真下に向けて設置された温水噴射手段としての温水噴射リング３８とを有している。 1. Configuration of Residual Monomer Removal Device This device has acylindrical tower body 4, a plurality of porous plates 34 provided in the vertical direction of the tower body 4, each having a large number of pores, and the porous plate as a bottom surface. A plurality of chambers 16 to 21 formed above, and a slurry inlet 22 as a slurry inlet provided above the porous plate below the tower top chamber 21 or the porous plate below the chamber 19 among the plurality of porous plates. , 23, a downflow pipe 36 provided between the perforated plates so as to sequentially flow the slurry from the perforated plate in the upper chamber to the perforated plate in the lower chamber, and the water vapor introducing pipe 10 provided at the bottom of the tower body. A condenser 6 provided at the top of the tower body via a gas transfer port 11, a residual monomer gas transfer pipe 12 provided at the outlet of the condenser, and a lowermost porous plate among the plurality of porous plates PVC slurry outlet 24 provided in In addition, a hot water injection ring 38 as a hot water injection means installed directly below each porous plate is provided directly below the porous plate.
この装置は筒状の塔本体４と該塔本体４の垂直方向に設けられた、それぞれ多数の細孔を有する複数の多孔板３４と、該多孔板をそれぞれ底面としてその上に形成された複数の室１６～２１と、前記複数の多孔板のうち塔頂室２１下の多孔板或いは室１９下の多孔板の上側に設けられたスラリー導入部としてのスラリー導入口２２、２３と、上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように該多孔板間に設けられた流下管３６と、塔本体の底部に設けられた水蒸気導入管１０と、塔本体の頂部にガス移送口１１を介して設けられた凝縮器６と、該凝縮器出口に設けられた残留モノマーガス移送管１２と、前記複数の多孔板のうち最下部の多孔板に設けられたＰＶＣスラリー排出口２４と、各多孔板の真下に、該多孔板の真下に向けて設置された温水噴射手段としての温水噴射リング３８とを有している。 1. Configuration of Residual Monomer Removal Device This device has a
１－１．塔本体
塔本体４の内径は、２００～１００００ｍｍで、塔高さは内径に対して２～２０倍、より好ましくは５～１５倍である。また、必要により塔内の各室の内径が異なっていてもよい。残留モノマー除去処理塔４において、塔底と多孔板、多孔板とその直上部に位置する多孔板、または多孔板と塔頂に区切られた空間を室という。残留モノマーの処理に必要な室数は、ＰＶＣスラリーから残留モノマーを除去する時に必要とされる滞留時間により決定される。 1-1. Tower body The inner diameter of thetower body 4 is 200 to 10,000 mm, and the height of the tower is 2 to 20 times, more preferably 5 to 15 times the inner diameter. If necessary, the inner diameters of the chambers in the tower may be different. In the residual monomer removal processing tower 4, a tower bottom and a perforated plate, a perforated plate and a perforated plate located immediately above the perforated plate, or a space defined by the perforated plate and the top of the tower is referred to as a chamber. The number of chambers required for residual monomer treatment is determined by the residence time required when removing residual monomer from the PVC slurry.
塔本体４の内径は、２００～１００００ｍｍで、塔高さは内径に対して２～２０倍、より好ましくは５～１５倍である。また、必要により塔内の各室の内径が異なっていてもよい。残留モノマー除去処理塔４において、塔底と多孔板、多孔板とその直上部に位置する多孔板、または多孔板と塔頂に区切られた空間を室という。残留モノマーの処理に必要な室数は、ＰＶＣスラリーから残留モノマーを除去する時に必要とされる滞留時間により決定される。 1-1. Tower body The inner diameter of the
１－２．多孔板
多数の細孔を有する多孔板３４は、それぞれその表面に、数個の堰板３５が垂直に設けられ、上部の多孔板の下面との間に室（空間）を形成している。多孔板の細孔は、ＰＶＣスラリーが、多孔板上を流動する際、細孔より噴入してくる水蒸気によって、脱モノマー処理が行われるように、開けられたものである。細孔の大きさは、ＰＶＣスラリーが細孔を通して流下せず、しかも細孔が閉塞することがなく、下方から噴入してくる水蒸気が絶えず均一に通過するように、水蒸気圧および水蒸気導入量を考慮して設定される。 1-2. Perforated plate Each of theperforated plate 34 having a large number of pores has several dam plates 35 provided vertically on the surface thereof, and forms a chamber (space) between the lower surface of the upper perforated plate. The pores of the perforated plate are opened so that the monomer removal treatment is performed by water vapor injected from the pores when the PVC slurry flows on the perforated plate. The size of the pores is such that the PVC slurry does not flow down through the pores, and the pores are not clogged, and the water vapor pressure and the amount of water vapor introduced so that the water vapor injected from below constantly passes uniformly. Is set in consideration of
多数の細孔を有する多孔板３４は、それぞれその表面に、数個の堰板３５が垂直に設けられ、上部の多孔板の下面との間に室（空間）を形成している。多孔板の細孔は、ＰＶＣスラリーが、多孔板上を流動する際、細孔より噴入してくる水蒸気によって、脱モノマー処理が行われるように、開けられたものである。細孔の大きさは、ＰＶＣスラリーが細孔を通して流下せず、しかも細孔が閉塞することがなく、下方から噴入してくる水蒸気が絶えず均一に通過するように、水蒸気圧および水蒸気導入量を考慮して設定される。 1-2. Perforated plate Each of the
多孔板に開けられる細孔は、直径５ｍｍ以下、好ましくは、０．５～２ｍｍ、より好ましくは０．７～１．５ｍｍである。また、多孔板の開口率（総細孔面積／多孔板面積）は、０．００１～１０％、好ましくは０．０４～４％、より好ましくは０．２～２％である。
開口率がこの範囲であると、多孔板製棚段上を流動するＰＶＣスラリー中に存在するＰＶＣ粒子が十分に攪拌されるため、ＰＶＣ粒子が沈降することによる、ＰＶＣ粒子からの残留モノマーの除去効率が低下やＰＶＣスラリーの流動性の低下が防止できる。また、開口率がこの範囲であると、ＰＣＶスラリーが細孔から流下する現象（以下、液漏れという。）が生じることがなく、液漏れが防止できるために、液漏れ防止のために多量の水蒸気量を浪費するようなこともない。
堰板３５は、多孔板上に、ＰＶＣスラリーが流動できる処理通路を確保するためのものである。多孔板３４の上面に、堰板が互い違いに設置されており、
堰板により形成された処理通路により、ＰＶＣスラリーは、多孔棚板上で一定時間流動し、その間、下方から供給される水蒸気による脱モノマー処理を受ける。 The pores opened in the perforated plate have a diameter of 5 mm or less, preferably 0.5 to 2 mm, more preferably 0.7 to 1.5 mm. The aperture ratio (total pore area / porous plate area) of the porous plate is 0.001 to 10%, preferably 0.04 to 4%, more preferably 0.2 to 2%.
When the opening ratio is within this range, the PVC particles existing in the PVC slurry flowing on the perforated plate shelf are sufficiently stirred, so that the residual monomers are removed from the PVC particles by the PVC particles settling. The efficiency can be prevented from decreasing and the fluidity of the PVC slurry can be prevented from decreasing. In addition, when the opening ratio is within this range, the phenomenon that the PCV slurry flows down from the pores (hereinafter referred to as “liquid leakage”) does not occur and the liquid leakage can be prevented. There is no waste of water vapor.
Thedam plate 35 is for ensuring a processing passage through which the PVC slurry can flow on the perforated plate. On the upper surface of the perforated plate 34, weir plates are installed alternately,
The PVC slurry flows on the perforated shelves for a certain period of time by the processing passage formed by the weir plate, and during that time, the PVC slurry is subjected to the demonomer treatment with water vapor supplied from below.
開口率がこの範囲であると、多孔板製棚段上を流動するＰＶＣスラリー中に存在するＰＶＣ粒子が十分に攪拌されるため、ＰＶＣ粒子が沈降することによる、ＰＶＣ粒子からの残留モノマーの除去効率が低下やＰＶＣスラリーの流動性の低下が防止できる。また、開口率がこの範囲であると、ＰＣＶスラリーが細孔から流下する現象（以下、液漏れという。）が生じることがなく、液漏れが防止できるために、液漏れ防止のために多量の水蒸気量を浪費するようなこともない。
堰板３５は、多孔板上に、ＰＶＣスラリーが流動できる処理通路を確保するためのものである。多孔板３４の上面に、堰板が互い違いに設置されており、
堰板により形成された処理通路により、ＰＶＣスラリーは、多孔棚板上で一定時間流動し、その間、下方から供給される水蒸気による脱モノマー処理を受ける。 The pores opened in the perforated plate have a diameter of 5 mm or less, preferably 0.5 to 2 mm, more preferably 0.7 to 1.5 mm. The aperture ratio (total pore area / porous plate area) of the porous plate is 0.001 to 10%, preferably 0.04 to 4%, more preferably 0.2 to 2%.
When the opening ratio is within this range, the PVC particles existing in the PVC slurry flowing on the perforated plate shelf are sufficiently stirred, so that the residual monomers are removed from the PVC particles by the PVC particles settling. The efficiency can be prevented from decreasing and the fluidity of the PVC slurry can be prevented from decreasing. In addition, when the opening ratio is within this range, the phenomenon that the PCV slurry flows down from the pores (hereinafter referred to as “liquid leakage”) does not occur and the liquid leakage can be prevented. There is no waste of water vapor.
The
The PVC slurry flows on the perforated shelves for a certain period of time by the processing passage formed by the weir plate, and during that time, the PVC slurry is subjected to the demonomer treatment with water vapor supplied from below.
１－３．温水噴射装置
また、本発明の残留モノマー除去装置の塔本体４内には、温水噴射装置が設置されている。温水噴射装置としての温水噴射リング３８が、パイプを所定の形に成形（図４）し、多孔板３４の直下にそれぞれ設けられているが、所定時間毎に噴射ノズルから温水を噴射し、多孔板の下面や塔内壁を洗浄する。噴射ノズルの数やノズル孔３９の位置に、特に制限はないが、噴射ノズルの鉛直線との交差角度ａ，ｂ（図３）が、１０～６０度の範囲に設定することが好ましい。
温水に充分な噴出速度ひいては洗浄力を与えるために、温水噴出時の温水噴射リング内の圧力とその温水噴射をする室内の圧力の差圧は０．０２ＭＰａＧ以上好ましくは０．０５ＭＰａＧ以上であることが適当である。差圧がこの範囲であれば、温水消費量が増大することもなく、十分な洗浄効果が得られる温水噴射の圧力制御は、温水ポンプ８をインバーター化して温水循環ライン圧力を自動制御させる、或いは圧力制御弁３２を自動制御させることにより、可能となる。 1-3. Hot water injection apparatus Moreover, the hot water injection apparatus is installed in the towermain body 4 of the residual monomer removal apparatus of this invention. A hot water injection ring 38 as a hot water injection device forms a pipe into a predetermined shape (FIG. 4) and is provided directly below the perforated plate 34, respectively. Clean the bottom of the plate and the inner wall of the tower. The number of spray nozzles and the position of the nozzle hole 39 are not particularly limited, but it is preferable that the intersecting angles a and b (FIG. 3) with the vertical line of the spray nozzle are set in the range of 10 to 60 degrees.
In order to give a sufficient jetting speed to the hot water and thus a cleaning power, the pressure difference between the pressure in the hot water jet ring and the pressure in the room in which the hot water is jetted is 0.02 MPaG or more, preferably 0.05 MPaG or more. Is appropriate. If the differential pressure is within this range, the hot water injection pressure control with which a sufficient washing effect can be obtained without increasing the hot water consumption can be achieved by automatically controlling the hot water circulation line pressure by converting the hot water pump 8 into an inverter, or This is possible by automatically controlling thepressure control valve 32.
また、本発明の残留モノマー除去装置の塔本体４内には、温水噴射装置が設置されている。温水噴射装置としての温水噴射リング３８が、パイプを所定の形に成形（図４）し、多孔板３４の直下にそれぞれ設けられているが、所定時間毎に噴射ノズルから温水を噴射し、多孔板の下面や塔内壁を洗浄する。噴射ノズルの数やノズル孔３９の位置に、特に制限はないが、噴射ノズルの鉛直線との交差角度ａ，ｂ（図３）が、１０～６０度の範囲に設定することが好ましい。
温水に充分な噴出速度ひいては洗浄力を与えるために、温水噴出時の温水噴射リング内の圧力とその温水噴射をする室内の圧力の差圧は０．０２ＭＰａＧ以上好ましくは０．０５ＭＰａＧ以上であることが適当である。差圧がこの範囲であれば、温水消費量が増大することもなく、十分な洗浄効果が得られる温水噴射の圧力制御は、温水ポンプ８をインバーター化して温水循環ライン圧力を自動制御させる、或いは圧力制御弁３２を自動制御させることにより、可能となる。 1-3. Hot water injection apparatus Moreover, the hot water injection apparatus is installed in the tower
In order to give a sufficient jetting speed to the hot water and thus a cleaning power, the pressure difference between the pressure in the hot water jet ring and the pressure in the room in which the hot water is jetted is 0.02 MPaG or more, preferably 0.05 MPaG or more. Is appropriate. If the differential pressure is within this range, the hot water injection pressure control with which a sufficient washing effect can be obtained without increasing the hot water consumption can be achieved by automatically controlling the hot water circulation line pressure by converting the hot water pump 8 into an inverter, or This is possible by automatically controlling the
１－４．サイトグラスの洗浄管
サイトグラス３３の洗浄管３７は、図５の通り温水噴射リング３８の上部から接続する、或いは図６の通り温水噴射リング３８の下部から挿入して接続することが適切である。温水噴射リングの下側から接続すると、洗浄が終了しても温水洗浄リング内に残った温水がサイトグラス洗浄ノズルから垂れてサイトグラスに当たるため、サイトグラスから内部を観察できなくなる。また、室内の温度と温水の温度の温度差が大きいときは、洗浄時に室内の温度が変動し圧力も変動するため、その上の多孔板或いは下の多孔板が液漏れを起こすことがある。サイトグラス洗浄管を温水噴射リングの上部から接続する或いは温水噴射リングの下部から挿入して接続することにより温水を温水噴射リング内に貯めておけば、室内とそのリング内の温水の温度差が小さくなっていくために、多孔板の液漏れ防止につながる。 1-4. Sight Glass Cleaning Tube Thesight glass 33 cleaning tube 37 is suitably connected from the upper part of the hot water injection ring 38 as shown in FIG. 5, or inserted from the lower part of the hot water injection ring 38 as shown in FIG. . When connected from the lower side of the hot water injection ring, the hot water remaining in the hot water cleaning ring hangs down from the sight glass cleaning nozzle and hits the sight glass even after the cleaning is completed, so that the inside cannot be observed from the sight glass. Further, when the temperature difference between the room temperature and the temperature of the hot water is large, the room temperature fluctuates and the pressure fluctuates at the time of cleaning, so that the upper or lower porous plate may cause liquid leakage. If hot water is stored in the hot water injection ring by connecting the sight glass cleaning tube from the upper part of the hot water injection ring or inserting it from the lower part of the hot water injection ring, the temperature difference between the room and the hot water in the ring will be Since it becomes smaller, it leads to prevention of liquid leakage from the perforated plate.
サイトグラス３３の洗浄管３７は、図５の通り温水噴射リング３８の上部から接続する、或いは図６の通り温水噴射リング３８の下部から挿入して接続することが適切である。温水噴射リングの下側から接続すると、洗浄が終了しても温水洗浄リング内に残った温水がサイトグラス洗浄ノズルから垂れてサイトグラスに当たるため、サイトグラスから内部を観察できなくなる。また、室内の温度と温水の温度の温度差が大きいときは、洗浄時に室内の温度が変動し圧力も変動するため、その上の多孔板或いは下の多孔板が液漏れを起こすことがある。サイトグラス洗浄管を温水噴射リングの上部から接続する或いは温水噴射リングの下部から挿入して接続することにより温水を温水噴射リング内に貯めておけば、室内とそのリング内の温水の温度差が小さくなっていくために、多孔板の液漏れ防止につながる。 1-4. Sight Glass Cleaning Tube The
１－５．温水噴射リング
温水噴射装置としての温水噴射リング３８のパイプの平面形状は、通常、ギリシャ文字のΩ型もしくはΦ型または渦巻型、星形または羊腸型（九十九折り）の様なもので、交互に中心を同じくする多重リング型（図４）でも良い。温水噴射リング３８は、多孔板３４と平行に設置され、塔内部に納まればよいが、塔本体内壁に接近し過ぎると、洗い流されたＰＶＣ粒子等が間隙を閉塞する恐れがあるので、塔内壁から内側へ２０ｍｍ以上離れる距離に、その外径がくるように設置すると良い。温水噴射リング３８の外径は１５０～８０００ｍｍが好ましい。 1-5. Hot water injection ring The shape of the pipe of the hotwater injection ring 38 as a hot water injection device is usually like the Greek letter Ω type or Φ type or spiral type, star type or sheep intestine type (ninety nine folds). A multiple ring type (FIG. 4) having the same center alternately may be used. The hot water injection ring 38 may be installed parallel to the perforated plate 34 and stored inside the tower. However, if the hot water injection ring 38 is too close to the inner wall of the tower main body, the washed away PVC particles may block the gap. It is good to install so that the outer diameter may be at a distance of 20 mm or more away from the inner wall to the inside. The outer diameter of the hot water injection ring 38 is preferably 150 to 8000 mm.
温水噴射装置としての温水噴射リング３８のパイプの平面形状は、通常、ギリシャ文字のΩ型もしくはΦ型または渦巻型、星形または羊腸型（九十九折り）の様なもので、交互に中心を同じくする多重リング型（図４）でも良い。温水噴射リング３８は、多孔板３４と平行に設置され、塔内部に納まればよいが、塔本体内壁に接近し過ぎると、洗い流されたＰＶＣ粒子等が間隙を閉塞する恐れがあるので、塔内壁から内側へ２０ｍｍ以上離れる距離に、その外径がくるように設置すると良い。温水噴射リング３８の外径は１５０～８０００ｍｍが好ましい。 1-5. Hot water injection ring The shape of the pipe of the hot
２．ＰＶＣスラリーから残留モノマーを除去する方法
ＰＶＣスラリータンク１に一時蓄えられた懸濁重合または乳化重合により得られたＰＶＣスラリーは、ＰＶＣスラリーフィードポンプ２によって熱交換器３に導かれ、熱交換器３内で所定温度に加熱された後、ＰＶＣスラリー導入管２２或いは２３から残留モノマー除去処理塔４内へ導入される。 2. Method for Removing Residual Monomer from PVC Slurry The PVC slurry obtained by suspension polymerization or emulsion polymerization temporarily stored in thePVC slurry tank 1 is led to the heat exchanger 3 by the PVC slurry feed pump 2, and the heat exchanger 3 After being heated to a predetermined temperature, the residual monomer removal treatment tower 4 is introduced from the PVC slurry introduction pipe 22 or 23.
ＰＶＣスラリータンク１に一時蓄えられた懸濁重合または乳化重合により得られたＰＶＣスラリーは、ＰＶＣスラリーフィードポンプ２によって熱交換器３に導かれ、熱交換器３内で所定温度に加熱された後、ＰＶＣスラリー導入管２２或いは２３から残留モノマー除去処理塔４内へ導入される。 2. Method for Removing Residual Monomer from PVC Slurry The PVC slurry obtained by suspension polymerization or emulsion polymerization temporarily stored in the
塔内に導入するＰＶＣスラリーの流量は、多孔板３４の面積１ｍ２当たり０．１～３００ｍ３／ｈ（より好ましくは１～１００ｍ３／ｈ）になるように調整することが好ましい。塔内に導入するＰＶＣスラリーは、熱交換器３によって、５０～１００℃に予熱されていることが望ましい。この予熱によって残留モノマー除去効率が向上する。
ＰＶＣスラリーからモノマーを除去する難易度は、ＰＶＣスラリー中のＰＶＣ粒子の構造に起因する。ＰＶＣ粒子内の細孔容積率が大きい場合には、ＰＶＣ粒子と水蒸気の接触が良好で脱モノマーし易く、細孔容積率が小さい場合は、脱モノマーし難くなる。ＰＶＣスラリーの塔内の滞留時間は、上述のようなＰＶＣスラリーの脱モノマーの難易度と、塔内に導入されるＰＶＣスラリー中に含まれる未反応モノマー濃度と、ＰＶＣスラリー排出口２４での処理後の残留モノマー濃度の設定値によって決定される。 The flow rate of the PVC slurry introduced into the tower is preferably adjusted to be 0.1 to 300 m 3 / h (more preferably 1 to 100 m 3 / h) per 1 m 2 of the area of theporous plate 34. The PVC slurry introduced into the tower is preferably preheated to 50 to 100 ° C. by the heat exchanger 3. This preheating improves the residual monomer removal efficiency.
The difficulty of removing the monomer from the PVC slurry is due to the structure of the PVC particles in the PVC slurry. When the pore volume ratio in the PVC particles is large, the contact between the PVC particles and water vapor is good and the monomer is easily removed, and when the pore volume ratio is small, the monomer removal is difficult. The residence time of the PVC slurry in the tower is determined by the degree of difficulty of depolymerization of the PVC slurry as described above, the unreacted monomer concentration contained in the PVC slurry introduced into the tower, and the treatment at thePVC slurry outlet 24. It is determined by the set value of the residual monomer concentration later.
ＰＶＣスラリーからモノマーを除去する難易度は、ＰＶＣスラリー中のＰＶＣ粒子の構造に起因する。ＰＶＣ粒子内の細孔容積率が大きい場合には、ＰＶＣ粒子と水蒸気の接触が良好で脱モノマーし易く、細孔容積率が小さい場合は、脱モノマーし難くなる。ＰＶＣスラリーの塔内の滞留時間は、上述のようなＰＶＣスラリーの脱モノマーの難易度と、塔内に導入されるＰＶＣスラリー中に含まれる未反応モノマー濃度と、ＰＶＣスラリー排出口２４での処理後の残留モノマー濃度の設定値によって決定される。 The flow rate of the PVC slurry introduced into the tower is preferably adjusted to be 0.1 to 300 m 3 / h (more preferably 1 to 100 m 3 / h) per 1 m 2 of the area of the
The difficulty of removing the monomer from the PVC slurry is due to the structure of the PVC particles in the PVC slurry. When the pore volume ratio in the PVC particles is large, the contact between the PVC particles and water vapor is good and the monomer is easily removed, and when the pore volume ratio is small, the monomer removal is difficult. The residence time of the PVC slurry in the tower is determined by the degree of difficulty of depolymerization of the PVC slurry as described above, the unreacted monomer concentration contained in the PVC slurry introduced into the tower, and the treatment at the
塔内のＰＶＣスラリーの滞留時間が長いと、ＰＶＣスラリー中に存在するＰＶＣ粒子から残留モノマーを高度に除去することができるが、長すぎるとＰＶＣの粒子が熱劣化による着色を引き起こしてしまう。従って、ＰＶＣスラリーの必要以上の水蒸気との接触は好ましくない。そこで、滞留時間をＰＶＣスラリーの脱モノマー性の難易度に合わせて調整する必要がある。
If the residence time of the PVC slurry in the tower is long, residual monomers can be removed from the PVC particles present in the PVC slurry to a high degree. However, if the residence time is too long, the PVC particles are colored due to thermal deterioration. Therefore, it is not preferable to contact the PVC slurry with water vapor more than necessary. Therefore, it is necessary to adjust the residence time in accordance with the degree of difficulty of the monomer removal of the PVC slurry.
スラリー導入部としてのスラリー導入管２２或いは２３から塔本体内に導入されたＰＶＣスラリーは、多孔板３４上の堰板３５で区画された処理通路を通過し、流下管３６を通りその下の室の多孔板３４上に導入される。多孔板３４上に導入されたスラリーは、続いて、多孔板３４上の処理通路上を通過し、さらに流下管３６を通ってその下の多孔板３４上へ流入する。こうして最下部の多孔板３４までの処理通路を通過した後、最下部の多孔板３４に設けられたＰＶＣスラリー排出口２４から塔外へ排出される。
The PVC slurry introduced into the tower main body from the slurry introduction pipe 22 or 23 as the slurry introduction part passes through the processing passage defined by the weir plate 35 on the porous plate 34, passes through the flow down pipe 36, and the chamber below it. Is introduced onto the perforated plate 34. The slurry introduced onto the perforated plate 34 subsequently passes on the treatment path on the perforated plate 34 and further flows through the flow down pipe 36 onto the perforated plate 34 below. After passing through the processing passage to the lowermost porous plate 34 in this way, it is discharged from the PVC slurry discharge port 24 provided in the lowermost porous plate 34 to the outside of the tower.
本発明における多孔板３４は、堰板３５の数や処理通路の幅に特に制限はないが、流動するＰＶＣの液高さが増し、堰板を越えしてしまうことにより、滞留時間の異なるＰＶＣスラリーが混在するために、製品の品質を低下させることを防止するために、堰板の数と処理通路の幅を適正に設定する必要がある。
本発明の装置は、塔底室１５に水蒸気導入管１０を接続しており、水蒸気導入口１０から噴射される水蒸気が、多孔板の細孔を通して、多孔棚板上を流動するＰＶＣスラリー中に吹き込まれる。この時の水蒸気導入量は、ＰＶＣスラリー１ｍ３当たり、１～１００Ｋｇ／ｈ、好ましくは５～５０Ｋｇ／ｈである。水蒸気導入量がこの範囲であれば、ＰＶＣスラリー中のＰＶＣ粒子が沈降することなく、ＰＣＶスラリー中の残留モノマーを効率良く除去することができる。また、水蒸気導入量がこの範囲であれば、ＰＶＣスラリーの飛沫発生が抑えられ、フラッディングが生ずることがない。また、水蒸気導入量がこの範囲であれば、水蒸気導入量とＰＶＣスラリー中の残留モノマーの除去効果のバランスが良い。 Theporous plate 34 in the present invention is not particularly limited in the number of the dam plates 35 and the width of the processing passage. However, the height of the flowing PVC increases and exceeds the dam plate. Since the slurry is mixed, it is necessary to appropriately set the number of dam plates and the width of the processing passage in order to prevent deterioration of the product quality.
In the apparatus of the present invention, a watervapor introduction pipe 10 is connected to the tower bottom chamber 15, and the water vapor injected from the water vapor introduction port 10 flows into the PVC slurry flowing on the porous shelf plate through the pores of the porous plate. Infused. The amount of water vapor introduced at this time is 1 to 100 kg / h, preferably 5 to 50 kg / h, per 1 m 3 of the PVC slurry. If the amount of introduced steam is within this range, the residual monomer in the PCV slurry can be efficiently removed without settling of the PVC particles in the PVC slurry. Moreover, if the amount of introduced steam is within this range, the occurrence of splashing of the PVC slurry is suppressed, and no flooding occurs. Moreover, if the amount of introduced steam is within this range, the balance between the amount of introduced steam and the effect of removing residual monomers in the PVC slurry is good.
本発明の装置は、塔底室１５に水蒸気導入管１０を接続しており、水蒸気導入口１０から噴射される水蒸気が、多孔板の細孔を通して、多孔棚板上を流動するＰＶＣスラリー中に吹き込まれる。この時の水蒸気導入量は、ＰＶＣスラリー１ｍ３当たり、１～１００Ｋｇ／ｈ、好ましくは５～５０Ｋｇ／ｈである。水蒸気導入量がこの範囲であれば、ＰＶＣスラリー中のＰＶＣ粒子が沈降することなく、ＰＣＶスラリー中の残留モノマーを効率良く除去することができる。また、水蒸気導入量がこの範囲であれば、ＰＶＣスラリーの飛沫発生が抑えられ、フラッディングが生ずることがない。また、水蒸気導入量がこの範囲であれば、水蒸気導入量とＰＶＣスラリー中の残留モノマーの除去効果のバランスが良い。 The
In the apparatus of the present invention, a water
また、ＰＶＣスラリーの温度を調整することが、高品質のＰＶＣを得ることにつながる。一般に、多孔板上を流動するスラリーの温度は、５０～１５０℃、好ましくは７０～１２０℃、より好ましくは８０～１１０℃になるように、水蒸気温度と水蒸気導入量及び塔内圧力を調整することが望ましい。ＰＶＣスラリーの温度がこの範囲であれば、残留モノマーの除去効率を維持しながら、ＰＶＣ粒子の熱劣化による着色などを防止し、高品質を維持できる。
Also, adjusting the temperature of the PVC slurry leads to obtaining high-quality PVC. In general, the water vapor temperature, the amount of water vapor introduced, and the pressure in the tower are adjusted so that the temperature of the slurry flowing on the perforated plate is 50 to 150 ° C., preferably 70 to 120 ° C., more preferably 80 to 110 ° C. It is desirable. If the temperature of the PVC slurry is within this range, it is possible to prevent the coloring due to thermal degradation of the PVC particles and maintain high quality while maintaining the removal efficiency of the residual monomer.
残留モノマー除去装置内で除去されたモノマーガスと水蒸気の混合ガスは、塔頂室２１に連結されたガス移送管を経て凝縮器６に流入し、ここで水蒸気の大部分は凝縮され、凝縮水は残留モノマー除去処理塔内に落下して戻される。その時、塔頂室より上昇してくるモノマーガスと水蒸気の混合ガスと流下する凝縮水が向流接触し、凝縮水は加温される。さらに、凝縮器６に導入された冷却水１３を凝縮器６から冷却水出口温水供給管１４を経て温水タンク７に導き、温水洗浄用の温水として用いることによりエネルギーのロスを防止できる。残留モノマー除去処理塔４によって残留モノマーが除去されたＰＶＣスラリーはＰＶＣスラリー排出口２４から排出され、ポンプ９に送り込まれる。その後、ＰＶＣスラリーは熱交換器３を経て、ＰＶＣスラリータンクに蓄えられる。
The mixed gas of the monomer gas and water vapor removed in the residual monomer removing apparatus flows into the condenser 6 through the gas transfer pipe connected to the tower top chamber 21, where most of the water vapor is condensed and condensed water. Is dropped back into the residual monomer removal treatment tower. At that time, the mixed gas of the monomer gas and water vapor rising from the tower top chamber comes into countercurrent contact with the flowing condensed water, and the condensed water is heated. Furthermore, the loss of energy can be prevented by introducing the cooling water 13 introduced into the condenser 6 from the condenser 6 to the hot water tank 7 through the cooling water outlet hot water supply pipe 14 and using it as hot water for hot water washing. The PVC slurry from which the residual monomer has been removed by the residual monomer removal processing tower 4 is discharged from the PVC slurry discharge port 24 and fed into the pump 9. Thereafter, the PVC slurry passes through the heat exchanger 3 and is stored in the PVC slurry tank.
以下実施例を用いて本発明を具体的に説明するが、本発明はこれによって限定されるものではない。
Hereinafter, the present invention will be specifically described by way of examples, but the present invention is not limited thereto.
残留モノマー除去処理塔における温水噴射装置を使った温水噴射工程はＰＶＣスラリーフィード中とフィード終了後の洗浄水フィード中に実施される。
また温水噴射洗浄は、下の室１６から上の室に順番に温水噴射洗浄を行う。塔頂室の洗浄が終了すれば、また室１６の洗浄から開始される。室１５については、ＰＶＣスラリーフィード中に、塔底室の温水噴射洗浄弁３１を開放して温水噴射洗浄を行うと、室１５内の温度が低下し圧力も低下して上の多孔板から液漏れを起こすので、ＰＶＣスラリーフィード中に温水噴射洗浄は行わない。 The hot water injection process using the hot water injection device in the residual monomer removal treatment tower is performed during the PVC slurry feed and during the washing water feed after the feed is completed.
In the hot water jet cleaning, the hot water jet cleaning is performed in order from thelower chamber 16 to the upper chamber. When cleaning of the top chamber is completed, the cleaning of the chamber 16 is started again. As for the chamber 15, when the hot water jet cleaning valve 31 in the tower bottom chamber is opened during the PVC slurry feed and the hot water jet cleaning is performed, the temperature in the chamber 15 is lowered and the pressure is also lowered. Since leakage occurs, hot water jet cleaning is not performed during PVC slurry feed.
また温水噴射洗浄は、下の室１６から上の室に順番に温水噴射洗浄を行う。塔頂室の洗浄が終了すれば、また室１６の洗浄から開始される。室１５については、ＰＶＣスラリーフィード中に、塔底室の温水噴射洗浄弁３１を開放して温水噴射洗浄を行うと、室１５内の温度が低下し圧力も低下して上の多孔板から液漏れを起こすので、ＰＶＣスラリーフィード中に温水噴射洗浄は行わない。 The hot water injection process using the hot water injection device in the residual monomer removal treatment tower is performed during the PVC slurry feed and during the washing water feed after the feed is completed.
In the hot water jet cleaning, the hot water jet cleaning is performed in order from the
［実施例１］
（温水ポンプ出力のインバーター制御による温水噴出圧力制御）
１．温水ポンプ８を起動し、インバーター出力は、温水タンク７内の温度分布が均一に保てる循環量となる最低の値１００ｍ３／ｈであるとする。
２．温水噴射１分前に、温水循環ライン圧力の設定を温水噴射圧力と室内圧力との差圧が適正な値０．０５ＭＰａＧから０．０８ＭＰａＧとなるための温水循環ライン圧力にして、温水ポンプのインバーター出力を自動制御する。
３．温水ポンプ８のインバーター出力制御を手動モードに切り替えて、出力値をその時点の出力値で固定する。そして室１６の温水噴射洗浄弁３０を８秒間開放する。
４．温水噴射洗浄弁３０閉止後、温水ポンプ８のインバーター出力は、温水タンク７内の温度分布が均一に保てる循環量となる最低の値１００ｍ３／ｈに戻し、２～１０分間この状態を保つ。
５．上記２～４と同様の操作により１段上の温水噴射洗浄弁２９の開閉動作を行い、室１７及び室１８下の多孔板下側を洗浄する。
６．上記２～５と同様の操作を繰り返し、下の室から上の室に順番に温水噴射洗浄を行う。 [Example 1]
(Hot water jet pressure control by inverter control of hot water pump output)
1. It is assumed that the hot water pump 8 is started and the inverter output has a minimum value of 100 m 3 / h which is a circulation amount that can keep the temperature distribution in thehot water tank 7 uniform.
2. 1 minute before the hot water injection, the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the indoor pressure is 0.05 MPaG to 0.08 MPaG. Automatically control the output.
3. The inverter output control of the hot water pump 8 is switched to the manual mode, and the output value is fixed at the current output value. Then, the hot waterjet cleaning valve 30 in the chamber 16 is opened for 8 seconds.
4). After the warm waterinjection washing valve 30 is closed, the inverter output of the warm water pump 8 is returned to the minimum value of 100 m 3 / h, which is a circulation amount that can keep the temperature distribution in the warm water tank 7 uniform, and this state is maintained for 2 to 10 minutes.
5). By opening and closing the hot water jet cleaning valve 29 one stage higher by the same operation as the above 2 to 4, the lower side of the perforated plate under thechamber 17 and the chamber 18 is cleaned.
6). The same operations as in 2 to 5 above are repeated, and hot water jet cleaning is performed in order from the lower chamber to the upper chamber.
（温水ポンプ出力のインバーター制御による温水噴出圧力制御）
１．温水ポンプ８を起動し、インバーター出力は、温水タンク７内の温度分布が均一に保てる循環量となる最低の値１００ｍ３／ｈであるとする。
２．温水噴射１分前に、温水循環ライン圧力の設定を温水噴射圧力と室内圧力との差圧が適正な値０．０５ＭＰａＧから０．０８ＭＰａＧとなるための温水循環ライン圧力にして、温水ポンプのインバーター出力を自動制御する。
３．温水ポンプ８のインバーター出力制御を手動モードに切り替えて、出力値をその時点の出力値で固定する。そして室１６の温水噴射洗浄弁３０を８秒間開放する。
４．温水噴射洗浄弁３０閉止後、温水ポンプ８のインバーター出力は、温水タンク７内の温度分布が均一に保てる循環量となる最低の値１００ｍ３／ｈに戻し、２～１０分間この状態を保つ。
５．上記２～４と同様の操作により１段上の温水噴射洗浄弁２９の開閉動作を行い、室１７及び室１８下の多孔板下側を洗浄する。
６．上記２～５と同様の操作を繰り返し、下の室から上の室に順番に温水噴射洗浄を行う。 [Example 1]
(Hot water jet pressure control by inverter control of hot water pump output)
1. It is assumed that the hot water pump 8 is started and the inverter output has a minimum value of 100 m 3 / h which is a circulation amount that can keep the temperature distribution in the
2. 1 minute before the hot water injection, the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the indoor pressure is 0.05 MPaG to 0.08 MPaG. Automatically control the output.
3. The inverter output control of the hot water pump 8 is switched to the manual mode, and the output value is fixed at the current output value. Then, the hot water
4). After the warm water
5). By opening and closing the hot water jet cleaning valve 29 one stage higher by the same operation as the above 2 to 4, the lower side of the perforated plate under the
6). The same operations as in 2 to 5 above are repeated, and hot water jet cleaning is performed in order from the lower chamber to the upper chamber.
［実施例２］
（循環圧力制御弁の制御による温水噴出圧力制御）
１．温水ポンプ８を起動し、循環圧力制御弁３２開度出力を全開にする。
２．温水噴射１分前に、温水循環ライン圧力の設定を温水噴射圧力と室内圧力との差圧が適正な圧力となるための温水循環ライン圧力にして、循環圧力制御弁３２開度出力を自動制御する。
３．循環圧力制御弁３２を手動モードに切り替えて、開度出力値を固定する。そして室１６の温水噴射洗浄弁３０を８秒間開放する。
４．温水噴射洗浄弁３０閉止後、循環圧力制御弁３２開度出力を全開にする。２～１０分間この状態を保つ。
５．上記２～４と同様の操作により１段上の温水噴射洗浄弁２９の開閉動作を行い、室１７及び室１８下の多孔板下側を洗浄する。
６．上記２～５と同様の操作を繰り返し、下の室から上の室に順番に温水噴射洗浄を行う。 [Example 2]
(Control of hot water jet pressure by control of circulating pressure control valve)
1. The hot water pump 8 is started and the circulationpressure control valve 32 opening output is fully opened.
2. 1 minute before the hot water injection, the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the room pressure becomes an appropriate pressure, and the circulationpressure control valve 32 opening output is automatically controlled. To do.
3. The circulationpressure control valve 32 is switched to the manual mode, and the opening degree output value is fixed. Then, the hot water jet cleaning valve 30 in the chamber 16 is opened for 8 seconds.
4). After the warm waterjet cleaning valve 30 is closed, the circulation pressure control valve 32 opening output is fully opened. Keep this state for 2-10 minutes.
5). By opening and closing the hot water jet cleaning valve 29 one stage higher by the same operation as the above 2 to 4, the lower side of the perforated plate under thechamber 17 and the chamber 18 is cleaned.
6). The same operations as in 2 to 5 above are repeated, and hot water jet cleaning is performed in order from the lower chamber to the upper chamber.
（循環圧力制御弁の制御による温水噴出圧力制御）
１．温水ポンプ８を起動し、循環圧力制御弁３２開度出力を全開にする。
２．温水噴射１分前に、温水循環ライン圧力の設定を温水噴射圧力と室内圧力との差圧が適正な圧力となるための温水循環ライン圧力にして、循環圧力制御弁３２開度出力を自動制御する。
３．循環圧力制御弁３２を手動モードに切り替えて、開度出力値を固定する。そして室１６の温水噴射洗浄弁３０を８秒間開放する。
４．温水噴射洗浄弁３０閉止後、循環圧力制御弁３２開度出力を全開にする。２～１０分間この状態を保つ。
５．上記２～４と同様の操作により１段上の温水噴射洗浄弁２９の開閉動作を行い、室１７及び室１８下の多孔板下側を洗浄する。
６．上記２～５と同様の操作を繰り返し、下の室から上の室に順番に温水噴射洗浄を行う。 [Example 2]
(Control of hot water jet pressure by control of circulating pressure control valve)
1. The hot water pump 8 is started and the circulation
2. 1 minute before the hot water injection, the hot water circulation line pressure is set to the hot water circulation line pressure so that the differential pressure between the hot water injection pressure and the room pressure becomes an appropriate pressure, and the circulation
3. The circulation
4). After the warm water
5). By opening and closing the hot water jet cleaning valve 29 one stage higher by the same operation as the above 2 to 4, the lower side of the perforated plate under the
6). The same operations as in 2 to 5 above are repeated, and hot water jet cleaning is performed in order from the lower chamber to the upper chamber.
［実施例３］
（温水噴射リング上部から接続されたサイトグラス洗浄管での洗浄）
各室のサイトグラス３３の洗浄は、各室の温水噴射洗浄が行われるときに、同時に行われる。サイトグラス洗浄管は温水噴射リングの上部から接続しているので、温水噴射洗浄が終了すれば、サイトグラス洗浄ノズルから温水がいつまでも垂れることはない。また、温水を温水噴射リング内に貯めておくので、洗浄時の室内とそのリング内の温水の温度差が１℃以下と小さくなり、多孔板の液漏れは発生しない。 [Example 3]
(Washing with a sight glass washing tube connected from the top of the hot water injection ring)
The cleaning of thesight glass 33 in each chamber is performed simultaneously with the hot water jet cleaning in each chamber. Since the sight glass cleaning tube is connected from the upper part of the hot water jet ring, the hot water will not hang down from the sight glass cleaning nozzle indefinitely after the hot water jet cleaning is completed. In addition, since warm water is stored in the warm water jet ring, the temperature difference between the room during washing and the warm water in the ring is as small as 1 ° C. or less, and no liquid leaks from the porous plate.
（温水噴射リング上部から接続されたサイトグラス洗浄管での洗浄）
各室のサイトグラス３３の洗浄は、各室の温水噴射洗浄が行われるときに、同時に行われる。サイトグラス洗浄管は温水噴射リングの上部から接続しているので、温水噴射洗浄が終了すれば、サイトグラス洗浄ノズルから温水がいつまでも垂れることはない。また、温水を温水噴射リング内に貯めておくので、洗浄時の室内とそのリング内の温水の温度差が１℃以下と小さくなり、多孔板の液漏れは発生しない。 [Example 3]
(Washing with a sight glass washing tube connected from the top of the hot water injection ring)
The cleaning of the
［実施例４］
（温水噴射リング下部から挿入して接続されたサイトグラス洗浄管での洗浄）
実施例３と同様に、温水噴射洗浄が終了すれば、サイトグラス洗浄ノズルから温水がいつまでも垂れることはない。また、多孔板の液漏れは発生しない。 [Example 4]
(Washing with a sight glass washing tube inserted from the bottom of the hot water injection ring and connected)
Similar to the third embodiment, when the hot water jet cleaning is completed, the hot water does not hang down from the sight glass cleaning nozzle indefinitely. Moreover, liquid leakage from the perforated plate does not occur.
（温水噴射リング下部から挿入して接続されたサイトグラス洗浄管での洗浄）
実施例３と同様に、温水噴射洗浄が終了すれば、サイトグラス洗浄ノズルから温水がいつまでも垂れることはない。また、多孔板の液漏れは発生しない。 [Example 4]
(Washing with a sight glass washing tube inserted from the bottom of the hot water injection ring and connected)
Similar to the third embodiment, when the hot water jet cleaning is completed, the hot water does not hang down from the sight glass cleaning nozzle indefinitely. Moreover, liquid leakage from the perforated plate does not occur.
［比較例１］
従来の方法では、温水噴射洗浄時は適切な温水噴射圧力を確保するために、各室入口に設けられた温水噴射リング入口に圧力計と手動弁を設けて、各室の圧力の指示値が所定の圧力０．０５ＭＰａＧから０．０８ＭＰａＧになるように手動弁で開度を調整していた。しかしながら、温水ポンプの出口圧力の変動により、所定の圧力を確保できない場合があった。さらに、温水循環ラインには温水循環圧力を確保するために循環帰りラインに遮断用の自動弁が必要であり、各室洗浄時は各室の温水噴射洗浄自動弁を開放して、温水循環遮断弁を閉止していたが、弁の開閉のタイミングによって、配管のハンマーリングを起こし、これにより配管及び弁の振動、ひいては配管または弁のフランジから温水洩れを起こすことがあった。 [Comparative Example 1]
In the conventional method, a pressure gauge and a manual valve are provided at the hot water injection ring inlet provided at the inlet of each chamber in order to ensure an appropriate hot water injection pressure at the time of hot water jet cleaning. The opening degree was adjusted with a manual valve so that the predetermined pressure was 0.05 MPaG to 0.08 MPaG. However, a predetermined pressure may not be ensured due to fluctuations in the outlet pressure of the hot water pump. In addition, the hot water circulation line requires an automatic valve for shutoff in the return line to ensure the hot water circulation pressure. When cleaning each room, open the hot water jet cleaning automatic valve in each room to shut off the hot water circulation. Although the valve was closed, the hammering of the pipe was caused by the timing of opening and closing of the valve, which sometimes caused vibration of the pipe and the valve, and thus leakage of hot water from the pipe or the flange of the valve.
従来の方法では、温水噴射洗浄時は適切な温水噴射圧力を確保するために、各室入口に設けられた温水噴射リング入口に圧力計と手動弁を設けて、各室の圧力の指示値が所定の圧力０．０５ＭＰａＧから０．０８ＭＰａＧになるように手動弁で開度を調整していた。しかしながら、温水ポンプの出口圧力の変動により、所定の圧力を確保できない場合があった。さらに、温水循環ラインには温水循環圧力を確保するために循環帰りラインに遮断用の自動弁が必要であり、各室洗浄時は各室の温水噴射洗浄自動弁を開放して、温水循環遮断弁を閉止していたが、弁の開閉のタイミングによって、配管のハンマーリングを起こし、これにより配管及び弁の振動、ひいては配管または弁のフランジから温水洩れを起こすことがあった。 [Comparative Example 1]
In the conventional method, a pressure gauge and a manual valve are provided at the hot water injection ring inlet provided at the inlet of each chamber in order to ensure an appropriate hot water injection pressure at the time of hot water jet cleaning. The opening degree was adjusted with a manual valve so that the predetermined pressure was 0.05 MPaG to 0.08 MPaG. However, a predetermined pressure may not be ensured due to fluctuations in the outlet pressure of the hot water pump. In addition, the hot water circulation line requires an automatic valve for shutoff in the return line to ensure the hot water circulation pressure. When cleaning each room, open the hot water jet cleaning automatic valve in each room to shut off the hot water circulation. Although the valve was closed, the hammering of the pipe was caused by the timing of opening and closing of the valve, which sometimes caused vibration of the pipe and the valve, and thus leakage of hot water from the pipe or the flange of the valve.
［比較例２］
従来のサイトグラス洗浄については、サイトグラス洗浄管が温水噴射リングの下側に接続しているため、温水噴射洗浄が終了しても、温水噴射リング内の温水が完全に抜けるまでサイトグラス洗浄ノズルから温水が垂れてそれがサイトグラスに当たり、内部を観察することができなかった。また、室によっては室内とそのリング内の温水の温度差が５℃以上と大きいため、温水噴射洗浄時に多孔板の液漏れが発生していた。 [Comparative Example 2]
For conventional sight glass cleaning, the sight glass cleaning pipe is connected to the lower side of the hot water injection ring, so even if the hot water injection cleaning is completed, the hot water in the hot water injection ring is completely discharged until the sight glass cleaning nozzle is removed. Hot water dripped from it, hitting the sight glass, and the inside could not be observed. Also, depending on the chamber, the temperature difference between the hot water in the chamber and the ring is as large as 5 ° C. or more, and thus liquid leakage of the porous plate occurred during hot water jet cleaning.
従来のサイトグラス洗浄については、サイトグラス洗浄管が温水噴射リングの下側に接続しているため、温水噴射洗浄が終了しても、温水噴射リング内の温水が完全に抜けるまでサイトグラス洗浄ノズルから温水が垂れてそれがサイトグラスに当たり、内部を観察することができなかった。また、室によっては室内とそのリング内の温水の温度差が５℃以上と大きいため、温水噴射洗浄時に多孔板の液漏れが発生していた。 [Comparative Example 2]
For conventional sight glass cleaning, the sight glass cleaning pipe is connected to the lower side of the hot water injection ring, so even if the hot water injection cleaning is completed, the hot water in the hot water injection ring is completely discharged until the sight glass cleaning nozzle is removed. Hot water dripped from it, hitting the sight glass, and the inside could not be observed. Also, depending on the chamber, the temperature difference between the hot water in the chamber and the ring is as large as 5 ° C. or more, and thus liquid leakage of the porous plate occurred during hot water jet cleaning.
本発明の残留モノマー除去装置は、塩化ビニル系樹脂の製造装置に使用できる。
The residual monomer removing apparatus of the present invention can be used for a vinyl chloride resin manufacturing apparatus.
１…ＰＶＣスラリータンク
２…ＰＶＣスラリーフィードポンプ
３…熱交換器
４…残留モノマー除去処理塔
５…ＰＶＣスラリータンク
６…凝縮器
７…温水タンク
８…温水ポンプ
９…ポンプ
１０…水蒸気導入管
１１…ガス排出口
１２…残留モノマーガス移送管
１３…冷却水
１４…冷却水出口温水供給管
１５…塔底室
１６～２０…室
２１…塔頂室
２２，２３…ＰＶＣスラリー導入管
２４…ＰＶＣスラリー排出口
２５～３０…温水噴射洗浄弁
３１…塔底室の温水噴射洗浄弁
３２…温水循環圧力制御弁
３３…サイトグラス（各室とも同番号）
３４…多孔板（各室とも同番号）
３５…堰板（各室とも同番号）
３６…流下管（各室とも同番号）
３７…サイトグラス洗浄管（各室とも同番号）
３８…温水噴射リング（各室とも同番号）
３９…ノズル孔
４０…圧力計 DESCRIPTION OFSYMBOLS 1 ... PVC slurry tank 2 ... PVC slurry feed pump 3 ... Heat exchanger 4 ... Residual monomer removal processing tower 5 ... PVC slurry tank 6 ... Condenser 7 ... Hot water tank 8 ... Hot water pump 9 ... Pump 10 ... Water vapor introduction pipe 11 ... Gas outlet 12 ... Residual monomer gas transfer pipe 13 ... Cooling water 14 ... Cooling water outlet hot water supply pipe 15 ... Tower bottom chamber 16-20 ... Chamber 21 ... Tower top chambers 22, 23 ... PVC slurry introduction pipe 24 ... PVC slurry exhaust Outlet 25 to 30 ... Warm water jet cleaning valve 31 ... Warm water jet cleaning valve 32 in tower bottom chamber ... Hot water circulation pressure control valve 33 ... Sight glass (same number for each chamber)
34 ... Perforated plate (same number for each chamber)
35 ... Dam plate (same number for each room)
36 ... Downflow pipe (same number for each room)
37 ... Sight glass tube (same number in each room)
38 ... Hot water jet ring (same number for each room)
39 ...Nozzle hole 40 ... Pressure gauge
２…ＰＶＣスラリーフィードポンプ
３…熱交換器
４…残留モノマー除去処理塔
５…ＰＶＣスラリータンク
６…凝縮器
７…温水タンク
８…温水ポンプ
９…ポンプ
１０…水蒸気導入管
１１…ガス排出口
１２…残留モノマーガス移送管
１３…冷却水
１４…冷却水出口温水供給管
１５…塔底室
１６～２０…室
２１…塔頂室
２２，２３…ＰＶＣスラリー導入管
２４…ＰＶＣスラリー排出口
２５～３０…温水噴射洗浄弁
３１…塔底室の温水噴射洗浄弁
３２…温水循環圧力制御弁
３３…サイトグラス（各室とも同番号）
３４…多孔板（各室とも同番号）
３５…堰板（各室とも同番号）
３６…流下管（各室とも同番号）
３７…サイトグラス洗浄管（各室とも同番号）
３８…温水噴射リング（各室とも同番号）
３９…ノズル孔
４０…圧力計 DESCRIPTION OF
34 ... Perforated plate (same number for each chamber)
35 ... Dam plate (same number for each room)
36 ... Downflow pipe (same number for each room)
37 ... Sight glass tube (same number in each room)
38 ... Hot water jet ring (same number for each room)
39 ...
Claims (5)
- 筒状の塔本体と
該塔本体の垂直方向に設けられた複数の多孔板と、
該多孔板をそれぞれ底面としてその上に形成された複数の室と、
前記複数の多孔板のうち最上部の多孔板の上側に設けられたスラリー導入口と、
上方の室の多孔板から下方の室の多孔板へスラリーを順次流下させるように前記多孔板間に設けられた流下部と、
塔本体の底部に設けられた水蒸気導入口と、
塔本体の塔頂室にガス移送管を介して該塔本体の外部に設けられた凝縮装置と、
前記複数の多孔板のうち最下部の多孔板に設けられたスラリー排出口と、
多孔板の真下に、少なくとも該多孔板の下面に向けて設けられた温水噴射装置と
を有している、
重合終了後の残留モノマーを含むポリ塩化ビニル含有スラリーから残留モノマーを除去する、残留モノマー除去装置において、
その温水噴射装置には、適切な噴射量の温水を噴射するために、噴射圧力を監視する圧力計、及びその噴射圧力を制御する為の装置を装着する
ことを特徴とする、残留モノマー除去装置。 A cylindrical tower body and a plurality of perforated plates provided in the vertical direction of the tower body;
A plurality of chambers formed on each of the porous plates as a bottom surface;
A slurry inlet provided above the uppermost porous plate among the plurality of porous plates;
A lower part provided between the perforated plates so as to sequentially flow the slurry from the perforated plate of the upper chamber to the perforated plate of the lower chamber;
A water vapor inlet provided at the bottom of the tower body;
A condenser provided outside the tower body via a gas transfer pipe in the tower top chamber of the tower body;
A slurry outlet provided in a lowermost porous plate among the plurality of porous plates;
It has a hot water injection device provided directly below the perforated plate toward the lower surface of the perforated plate,
In the residual monomer removing apparatus for removing the residual monomer from the polyvinyl chloride-containing slurry containing the residual monomer after completion of the polymerization,
The hot water injection device is equipped with a pressure gauge for monitoring the injection pressure and a device for controlling the injection pressure in order to inject an appropriate amount of hot water, and a residual monomer removing device. . - 噴射圧力を制御する為の装置が、圧力制御弁または温水供給ポンプ出力をインバーター制御化し温水噴射圧力を調節する装置である、請求項１記載の残留モノマー除去装置。 The residual monomer removing device according to claim 1, wherein the device for controlling the injection pressure is a device for adjusting the hot water injection pressure by controlling the output of the pressure control valve or the hot water supply pump with an inverter.
- 前記温水噴射装置に備えられている温水噴射リングに、各室に１箇所以上設置しているサイトグラスを洗浄するための洗浄ノズルを有する請求項１または２に記載の残留モノマー除去装置。 3. The residual monomer removing device according to claim 1, wherein the hot water injection ring provided in the hot water injection device has a cleaning nozzle for cleaning one or more sight glasses installed in each chamber.
- 前記温水噴射リングに有するサイトグラスを洗浄するための洗浄ノズルが、該温水噴射リングの上側から接続している、請求項３に記載の残留モノマー除去装置。 The residual monomer removing device according to claim 3, wherein a cleaning nozzle for cleaning the sight glass included in the hot water injection ring is connected from the upper side of the hot water injection ring.
- 前記温水噴射リングに有するサイトグラスの洗浄する為の洗浄ノズルが、該温水噴射リングの内部に挿入されるように接続されている請求項３に記載の残留モノマー除去装置。 The residual monomer removing apparatus according to claim 3, wherein a cleaning nozzle for cleaning the sight glass included in the hot water injection ring is connected so as to be inserted into the hot water injection ring.
Priority Applications (4)
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| AU2019280943A AU2019280943B2 (en) | 2018-06-07 | 2019-06-05 | Device for residual-monomer removal |
| KR1020207027679A KR20210018991A (en) | 2018-06-07 | 2019-06-05 | Residual monomer removal device |
| JP2020523134A JPWO2019235504A1 (en) | 2018-06-07 | 2019-06-05 | Residual monomer remover |
| CN201980022174.9A CN111918884B (en) | 2018-06-07 | 2019-06-05 | Residual monomer removing device |
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| JP2018-109500 | 2018-06-07 |
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| JP (1) | JPWO2019235504A1 (en) |
| KR (1) | KR20210018991A (en) |
| CN (1) | CN111918884B (en) |
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| WO2022019574A1 (en) * | 2020-07-22 | 2022-01-27 | 한화솔루션 주식회사 | Apparatus for removing residual monomers |
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| JPS5622305A (en) * | 1979-08-01 | 1981-03-02 | Chisso Corp | Monomer removal from vinyl chloride resin slurry by steaming and apparatus therefor |
| JPH06107723A (en) * | 1992-09-25 | 1994-04-19 | Chisso Corp | Production of resin powder with low content of residual vinyl monomer by steam treatment of vinyl chloride resin slurry and its apparatus |
| JPH0938602A (en) * | 1995-07-31 | 1997-02-10 | Sanyo Electric Co Ltd | Washing machine |
| JPH0948815A (en) * | 1995-08-04 | 1997-02-18 | Chisso Corp | Apparatus for removing residual monomer and removal of residual monomer using the apparatus |
| JPH10338708A (en) * | 1997-06-06 | 1998-12-22 | Chisso Corp | Apparatus for removing unreacted monomer from polyvinyl chloride-containing slurry and removal |
| JPH11100410A (en) * | 1997-09-29 | 1999-04-13 | Nippon Zeon Co Ltd | Operation for recovering unreacted monomer from vinyl chloride polymer latex |
| JP2006160845A (en) * | 2004-12-06 | 2006-06-22 | Asahi Kasei Chemicals Corp | Method for producing water-absorbing resin |
| JP2008145096A (en) * | 2006-11-17 | 2008-06-26 | Chugoku Electric Power Co Inc:The | Hot water supply system and hot water supply method |
| JP2014128338A (en) * | 2012-12-28 | 2014-07-10 | Morita Holdings Corp | Hot water supply device |
| JP2018084384A (en) * | 2016-11-24 | 2018-05-31 | 大阪瓦斯株式会社 | Water heater with mist function |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022019574A1 (en) * | 2020-07-22 | 2022-01-27 | 한화솔루션 주식회사 | Apparatus for removing residual monomers |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111918884B (en) | 2023-05-16 |
| CN111918884A (en) | 2020-11-10 |
| JPWO2019235504A1 (en) | 2021-06-10 |
| TW202012461A (en) | 2020-04-01 |
| AU2019280943A1 (en) | 2020-11-12 |
| KR20210018991A (en) | 2021-02-19 |
| AU2019280943B2 (en) | 2024-06-13 |
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