JP4283396B2 - Cleaning method, cleaning device and cleaning material for chemical reaction vessel - Google Patents

Description

[0001]
BACKGROUND OF THE INVENTION
The present invention belongs to the field of cleaning techniques, in particular, a method and apparatus for cleaning a chemical reaction vessel and a cleaning material capable of removing adhesive resin adhered to the surface to be cleaned in a short time.
[0002]
[Prior art]
Conventionally, when cleaning a surface to which an adhesive resin having low adhesiveness is fixed, a cleaning method by spraying a solvent in which the adhesive resin is soluble or dipping in a solvent is used. For resins that adhere strongly, contact peeling method with a release agent, wiping method with a paste containing an abrasive, sand blasting to remove the adhesive resin, jet method with high pressure water, chemical etching with acid or alkali, hydrolysis Or a manual cutting method is used. These techniques require a long time for cleaning and involve damage to the surface to be cleaned. In addition, since a solvent that adversely affects the human body and the environment is used, further washing is required to prevent the solvent from remaining after washing. In particular, cleaning of reaction vessels and jigs used when manufacturing products with chemical reactions consumes a large amount of solvent and requires a long time for cleaning, so the ratio of cleaning costs to the product price is high. It is.
[0003]
For example, in a reactor used for the production of paints, inks, adhesives, synthetic resins, etc. by polycondensation reaction, the adhesive resin remains on the inner surface of the reaction vessel after the reaction product is taken out from the reaction vessel. That cannot be avoided. The remaining adhesive resin is difficult to remove, but if it is not completely removed, when another type of polymerization reaction is carried out in the reaction vessel, the reaction product and the adhesive resin are mixed, leading to a reduction in product quality. In addition, if a large amount of adhesive resin adheres to a coil or the like that performs temperature control by a polymerization reaction, the overall heat transfer coefficient decreases, and sufficient temperature control becomes difficult.
[0004]
For this reason, the conventional standard washing method uses a solvent that is soluble in the adhesive resin and performs reflux washing every time the polymerization reaction is completed. The reflux washing is performed by heating the solvent filled in the reaction vessel about half to a temperature near the boiling point, evaporating and condensing the solvent to wet the inner wall surface and dissolving the adhesive resin. The evaporated solvent is liquefied and collected in a condenser connected to the upper part of the reaction vessel, and returned to the reaction vessel. This reflux operation is repeated for 60 to 90 minutes. Adhesive resin that cannot be removed by reflux washing is ignored and the next polymerization reaction is performed. After repeated use in the polymerization reaction, washing with an alkaline solution is carried out for at least 16 hours, once every several polymerization reactions, depending on the amount of accumulated resin. Further, the resin is fixed by a human operation by a worker.
[0005]
The degree of resin adhesion varies depending on the polymerization method such as solution polymerization and emulsion polymerization, and also varies depending on the molecular weight of the resin to be produced, the tackiness, the reaction rate, the temperature control of heating by a rapid high-temperature heat source, and the like. In order to prevent resin adhesion, improvements have been made by surface treatment of reaction vessels, handling vessels and jigs, but they are incomplete in terms of temperature controllability and durability.
[0006]
The cleaning cost of the standard cleaning method reaches about 5 million yen / year in a 5000 L reaction vessel. This is because reflux cleaning, alkali cleaning, and stripping work take a long time, and the solvent used for the reflux cleaning cannot be regenerated and is discarded by combustion or discharged into the atmosphere. This is an essential problem in the chemical industry that causes not only costs but also environmental pollution, waste of resources and health hazards to workers.
[0007]
[Problems to be solved by the invention]
Accordingly, the present invention provides a cleaning method for a chemical reaction vessel, an apparatus therefor, and a cleaning material that can reliably remove the adhesive resin fixed to the surface of an object in a short time with a rational closed system that does not require human power. With the goal.
It is another object of the present invention to provide a chemical reaction vessel cleaning method and apparatus and a cleaning material for removing an adhesive resin safely and easily.
[0008]
[Means for Solving the Problems]
The technical idea of the present invention for solving the above problems is as follows:
[1] As an alternative to the conventional mechanical cutting method by human power, a solid substance that can physically attack the adhesive resin without damaging the surface to be cleaned is selected, and this is flowed to peel the adhesive resin. Let
[2] A conventional solvent is used as a dispersion medium for a solid substance, and is used in combination with reflux cleaning to smoothly dissolve, swell, and peel off.
[3] The cleaning method using the cleaning material according to the present invention is industrially easily and safely formed into a closed system.
[0009]
That is, the chemical reaction vessel cleaning method according to the present invention is a mixed solvent (3) 100 comprising a good solvent for dissolving and swelling the adhesive resin fixed to the surface to be cleaned and a poor solvent for curing the swollen adhesive resin. A step of filling the reaction vessel (1) with a cleaning material comprising 10 parts by weight of a solid substance having a maximum length of 0.1 to 50 mm that does not dissolve in the mixed solvent (3); (1) The step of flowing in and the adhesive resin (9) fixed to the inner wall surface (1a) of the reaction vessel (1) is dissolved, infiltrated and swollen with the mixed solvent (3) and together with the mixed solvent (3) The flowing solid substance (4) collided with the inner wall surface (1a) of the reaction vessel (1) to physically peel the swollen adhesive resin (9), and the dissolved and peeled together with the cleaning material. Removing the adhesive resin (9) from the reaction vessel (1).
[0010]
The chemical reaction container cleaning apparatus according to the present invention cleans and removes the adhesive resin (9) fixed to the inner wall surface (1a) of the reaction container (1) from the inner wall surface (1a) by a chemical reaction. In the present invention, a mixed solvent (3) composed of a good solvent for dissolving and swelling the adhesive resin (9) and a poor solvent for curing the swollen adhesive resin, and a solid that physically separates the adhesive resin (9). Adhesive resin (9) swollen by supplying a supply device (23, 7) for supplying the substance (4) to the reaction vessel (1) and a cleaning material containing the mixed solvent (3) and the solid substance (4). A stirrer (2) for causing the solid substance (4) to collide with the separator, a separator (22) for separating the cleaning material used for washing into the mixed solvent (3) and the solid substance (4), and the separated mixed solvent A filter (20) for removing the adhesive resin (9) from (3) to purify the mixed solvent (3), and a storage tank for storing the purified mixed solvent (3) and the separated solid substance (4) (5, 6).
[0011]
The cleaning material according to the present invention comprises a good solvent for dissolving and swelling the adhesive resin (9) fixed to the surface (1a) to be cleaned, a poor solvent for curing the swollen adhesive resin, and the surface (1a) to be cleaned. ) And a solid substance (4) that physically peels off the adhesive resin (9). As used herein, the term “good solvent” refers to a solvent that has a high ability to dissolve solutes. The term “poor solvent” refers to a solvent having a small ability to dissolve a solute. Since the adhesive resin (9) is dissolved and removed with a good solvent, the adhesive resin (9) firmly adhered to the surface of the object is swollen and collided with the solid substance (4) to physically peel off. The adhesive resin (9) fixed to the surface (1a) can be reliably and automatically removed. Therefore, it is possible to remove not only a soluble resin that can be removed with a good solvent but also a resin that is insoluble in a good solvent without the operator performing scraping work.
[0012]
DETAILED DESCRIPTION OF THE INVENTION
DESCRIPTION OF THE PREFERRED EMBODIMENTS Embodiments of a chemical reaction vessel cleaning method and apparatus and cleaning material according to the present invention will be described below with reference to FIGS.
[0013]
The cleaning material according to the present invention comprises a solvent (3) that dissolves and swells the adhesive resin (9) fixed to the surface (1a) to be cleaned, and the adhesive resin (9) that collides with the surface (1a) to be cleaned. And a solid substance (4) that physically exfoliates. Solvent (3) is a good solvent, esters such as ethyl acetate and butyl acetate, ketones such as acetone, methyl ethyl ketone and methyl isobutyl ketone, halides such as trichloroethylene and carbon tetrachloride, aromatic hydrocarbons such as toluene and xylene, One or more of alcohols such as isopropyl alcohol, alkalis such as sodium hydroxide, and water. If necessary, organic amino compounds such as dimethylaminoethanol, diethylaminoethanol and triethylamine, organic acids such as acetic acid, surfactants and ammonia can also be used. Furthermore, a low molecular weight acrylic resin, polyester resin and vinyl chloride resin may be added to the solvent (3) in order to adjust the viscosity of the solvent (3) and promote dissolution of the adhesive resin (9).
[0014]
The solid substance (4) is a solid resin having a cylindrical shape, a spherical shape, a polyhedral shape, a confetti shape or a tetrapod shape, and has a maximum length of 0.1 to 50 mm. When the maximum length of the solid substance (4) is less than 0.1 mm, the solid substance (9) is separated when the separated adhesive resin (9) is separated to reuse the solvent (3) and the solid substance (4). It becomes difficult to completely separate 4) and the adhesive resin (9). If the maximum length of the solid substance (4) exceeds 50 mm, the number of collisions between the reaction container (1), which is the surface (1a) to be cleaned, and the inner wall surface (1a) of the pipe, and the solid substance (4) decreases. The peelability of the adhesive resin (9) fixed to the inner wall surface (1a) is lowered. If the thickness exceeds 50 mm, solid substances (not shown) in the concavo-convex portions in the reaction vessel (1), for example, the gaps between the concavo-convex portions (not shown) at the connection point between the shaft (2a) of the stirrer (2) and the stirring blade (2b). 4) will not enter and dead space that cannot collide will increase.
[0015]
The solid material (4) may be any material that is insoluble in the solvent (3) and softer than the inner wall surface (1a), and gives an appropriate impact to the adhesive resin (9) fixed to the inner wall surface (1a). A material having an impact strength of 20 to 220 J / m is preferable. Polyolefin resin, polyester resin, phenol resin, melamine resin, urea resin, epoxy resin, silicone resin or fluororesin can be used, among which polyethylene, polypropylene, polyethylene terephthalate or polytetra- mer having high density, high heat resistance and strong mechanical strength Pellets such as fluoroethylene are preferred. The density of the solid substance (4) is 0.92 × 10 ^{3 to} 0.96 × 10 ³ kg / m ³ for polyethylene and 0.85 × 10 ^{3 to} 0.92 × 10 ³ kg for polypropylene. / m ^3, in ^{1.37 × 10 3 ~1.38 × 10 3} kg / m 3 and made of polytetrafluoroethylene is made of polyethylene terephthalate was 2.1~2.3g / cm ^3, solvent (3) The dispersibility is good, and repeated soft attack by flow is effectively performed. The solid substance (4) can be an organic material, an inorganic material, a metal or a composite thereof as long as it is a material that is inexpensive and has an appropriate hardness, specific gravity, thermal stability, and wear resistance, in addition to the resin. Those having a specific gravity capable of being dispersed in (3) are preferred.
[0016]
The relationship between the solvent (3) and the solid substance (4) is that 50 to 90 parts by weight of the solvent (3) and 10 to 50 parts by weight of the solid substance (4) are matched to the properties of the adhesive resin (9). Just choose. The density ratio of the solvent (3) and the solid substance (4) alone is 1: 0.9 to 1.4. If the density ratio of the solid substance (4) alone to the solvent (3) 1 is less than 0.9, the solid substance (4) floats in the solvent (3), and the lower part of the reaction vessel (1) The inner wall (1a) cannot be cleaned sufficiently. When the ratio of the density of the solid substance (4) alone to the solvent (3) 1 exceeds 1.4, the solid substance (4) settles in the solvent (3) and stays in the upper part of the reaction vessel (1). The wall (1a) cannot be cleaned sufficiently. In addition, the flow rate of the solid substance (4) becomes slow, and the impact force and the number of collisions with respect to the adhesive resin (9) are reduced. For the same reason, the density ratio of the mixed solvent (3) and the solid substance (4), which will be described later, is 1: 0.9 to 1.4.
[0017]
Since the adhesive resin (9) to be removed by the cleaning material according to the present invention is physically peeled off by the solid substance (4), the type of the adhesive resin (9) is not particularly limited. An effective effect is achieved by the production of acrylic resin, polyester resin, urethane resin, vinyl chloride resin, polystyrene or ABS resin widely used in the industry or the production of modified resin by a combination of these resins (reaction vessel ( 1) Resin fixed inside the pipe.
[0018]
In the embodiment of the present invention, a poor solvent for curing the adhesive resin (9) swollen by permeation is included. When the mixed solvent (3) containing a good solvent and a poor solvent is used, the detergency is further enhanced. That is, when the adhesive resin (9) is composed of a gel component and a sol component having a low molecular weight, the sol component dissolves well in a good solvent, but the gel component absorbs a large amount of good solvent and swells. The gel that swells after absorbing a large amount of good solvent maintains its state of adhering to the inner wall surface (1a) without eluting from the good solvent, increasing flexibility. It is difficult to mitigate the mechanical impact and scrape off the adhesive resin (9) from the inner wall surface (1a). On the other hand, a poor solvent having a small ability to dissolve a solute limits the amount of good solvent absorbed by the gel and hardens the swollen gel. As a result, the sol content is dissolved with a good solvent and the gel content is swollen, and after the swollen gel content is cured with a poor solvent, the adhesive resin ( 9) can be completely removed from the inner wall surface (1a). When the mixed solvent (3) is stirred with the stirrer (2) as shown in FIG. 1, the solid substance (4) collides with the adhesive resin (9) as shown in FIG. 2, and the adhesive resin (9) Can be completely peeled from the inner wall surface (1a) of the reaction vessel (1). The poor solvent is one or more of alcohol, petroleum ether, aliphatic hydrocarbon, and water.
[0019]
The combination of the good solvent and the poor solvent that are the mixed solvent (3) is determined by the adhesive resin (9). Adhesive resin (9) is a monomer having an ethylenically unsaturated double bond capable of emulsion polymerization, suspension polymerization and solution polymerization, such as vinyl chloride, vinyl acetate, styrene, methyl methacrylate, butyl acrylate, isooctyl acrylate Or when adhering to the inner wall surface (1a) by the polymerization reaction of acrylonitrile, one or more good solvents of ester, ketone, alkyl halide and aromatic hydrocarbon, alcohol, petroleum ether and aliphatic hydrocarbon One or more poor solvents are used. Polymerization reaction of a monomer whose adhesive resin (9) has a functional group having an ethylenically unsaturated double bond as a main component, for example, acrylic acid, methacrylic acid, 2-hydroxyethyl acrylate, acrylamide or N-methylolacrylamide When adhering to the inner wall surface (1a), one or more good solvents such as esters, ketones, alkyl halides, aromatic hydrocarbons, alcohols and water and petroleum ethers and aliphatic hydrocarbons or Two or more poor solvents are used. As described above, the good solvent and the poor solvent are determined by the chemical components of the adhesive resin (9), and there are solvents that can be either a good solvent or a poor solvent such as alcohol.
[0020]
The combination of the good solvent, the poor solvent and the solid substance (4) is, for example, a mixture of 20 to 70% by weight of an ester having a molecular weight of 100 or less which is a good solvent and 30 to 80% by weight of an alcohol having 1 to 6 carbon atoms which is a poor solvent. 100 parts by weight of the solvent (3) and 10 to 30 parts by weight of the solid substance (4) having a maximum length of 0.1 to 50 mm. If the ester having a molecular weight of 100 or less, which is a good solvent, is less than 20% by weight, dissolution of the sol contained in the adhesive resin (9) becomes insufficient, and the solubility does not change even if it exceeds 70% by weight. Further, if the alcohol having 1 to 6 carbon atoms, which is a poor solvent, is less than 30% by weight, the gel component swollen by the good solvent cannot be completely cured and the flexibility is maintained, so that the solid substance (4) It becomes difficult to physically peel off by colliding. Even if it exceeds 80% by weight, no further curing occurs. When the solid substance (4) of 0.1 to 50 mm is less than 10 parts by weight with respect to 100 parts by weight of the mixed solvent (3), the content of the solid substance (4) contained in the reaction vessel (1) is small, The number of collisions between the solid substance (4) and the inner wall surface (1a) of the reaction vessel (1) decreases, and the peelability of the adhesive resin (9) decreases. If it exceeds 30 parts by weight, the content of the solid substance (4) contained in the reaction vessel (1) is large and heavy, the flow rate of the solid substance (4) becomes slow, and the solid substance (4) becomes intense and the inner wall (1a) Since it does not collide with the film, the peelability is reduced.
[0021]
As shown in FIG. 3, the cleaning apparatus for cleaning the reaction vessel (1) using the cleaning material physically removes the solvent (3) and the adhesive resin (9) for dissolving and swelling the adhesive resin (9). The supply device (23, 7) for supplying the solid material (4) to be separated into the reaction vessel (1) and the cleaning material containing the solvent (3) and the solid material (4) are flowed as shown in FIG. A stirrer (2) for causing the solid substance (4) to collide with the swollen adhesive resin (9), and a separator (22) for separating the cleaning material used for washing into the solvent (3) and the solid substance (4). ), A filter (20) that purifies the solvent (3) by removing the adhesive resin (9) from the separated solvent (3), and the purified solvent (3) and the separated solid substance (4) Storage tanks (5, 6).
[0022]
The solvent pump (23), which is a supply device for the solvent (3), is connected between the solvent tank (5), which is a storage tank for the solvent (3), and the reaction vessel (1). 3) is supplied to the reaction vessel (1). The feeder (7), which is a supply device for the solid substance (4), is connected between the bucket tank (6), which is a storage tank for the solid substance (4), and the reaction vessel (1). Material (4) is fed to the reaction vessel (1). As shown in FIG. 1, the stirrer (2) includes a shaft (2a) to which a rotational motion is given from a motor (2c), a stirring blade (2b) connected to the shaft (2a), and a solvent (3 ) And solid material (4). The cleaning material after cleaning is accommodated in the bucket tank (6), and the solvent (3) and the solid substance are separated by a flat separator (22) formed between the bucket tank (6) and the diatomaceous earth charging tank (10). (4). The separator (22) is formed of a punching metal or a metal net having an opening on the entire surface so that the solid substance (4) cannot pass through. In the filter (20), filter paper is arranged on the outer surface or inner surface of a plurality of filter plates (20a) formed inside, and diatomaceous earth having a particle diameter of 3 to 5 μm is about 0.1% by weight of the solvent (3). Pre-coated as a filter aid. In addition, a circulation pump (24) for returning the solvent (3) purified by the filter (20) into the reaction vessel (1) and circulating between the filter (20) and the reaction vessel (1) is provided. Furthermore, in order to prevent the filtration rate of the filter (20) from decreasing early, as a pretreatment of the filter (20), the strainer (21) has higher separation accuracy than the separator (22) and lower filtration accuracy than the filter (20). Can be placed.
[0023]
The method of cleaning the reaction vessel (1) according to the present invention using the cleaning material and the cleaning apparatus is composed of 50 to 90 parts by weight of the solvent (3) and a solid having a maximum length of 0.1 to 50 mm that does not dissolve in the solvent (3). The reaction container (1) is filled with a cleaning material consisting of 10 to 50 parts by weight of the substance (4). When the solid substance (4) is less than 10 parts by weight, the number of collisions between the solid substance (4) and the inner wall surface (1a) of the reaction vessel (1) is reduced, and the peelability of the adhesive resin (9) is lowered. . When the solid substance (4) exceeds 50 parts by weight, the flow rate of the solid substance (4) becomes slow, and the solid substance (4) does not collide with the inner wall surface (1a) violently, so that the peelability is lowered. As the solvent (3), a mixed solution of an organic solvent, particularly a mixed solvent (3) containing a poor solvent such as methanol may be used in order to enhance the detergency.
[0024]
Next, the cleaning material filled in the reaction vessel (1) is stirred and fluidized with a stirrer (2) as shown in FIG. As a result, the adhesive resin (9) adhering to the inner wall surface (1a) of the reaction vessel (1) is dissolved, infiltrated and swelled by the solvent (3), and the solid substance (4) flowing together with the solvent (3) is reacted. The swollen adhesive resin (9) is physically peeled by colliding with the inner wall surface (1a) of the container. After completion of the stirring, the adhesive resin (9) dissolved and peeled off together with the cleaning material is removed from the reaction vessel (1).
[0025]
In the present invention, the step of recovering the cleaning material used for cleaning from the reaction vessel (1), the step of separating the solid material (4) from the recovered cleaning material, the separated solid material (4) and the solvent (3) may be supplied to the reaction vessel (1), and a step of flowing the cleaning material in the reaction vessel (1) may be included. In addition, the cleaning material used for cleaning is filtered to remove the adhesive resin (9), the solvent (3) and the solid substance (4) are mixed to adjust and regenerate the cleaning material, and the regeneration Reusing the cleaned cleaning material.
[0026]
【Example】
An example of the cleaning method using the cleaning material and the cleaning apparatus according to the present invention applied to the cleaning of the solvent type acrylic resin polymerization reaction vessel will be described.
[0027]
After removing the acrylic resin polymerized in the reaction vessel (1) shown in FIG. 3 from the reaction vessel (1), the acrylic resin (9) adhering to the inner wall surface (1a) of the reaction vessel (1) is removed. As a previous step, reflux washing was performed with toluene as a good solvent. The method of reflux cleaning is as described above. Thereafter, the reaction vessel (1) was cleaned using a cleaning material containing the mixed solvent (3) and the solid substance (4). The composition of the mixed solvent (3) 5100 kg was 50% by weight of ethyl acetate, 900 kg of a solid (4) polyethylene resin having 25% by weight of isopropyl alcohol and 25% by weight of methanol and having a cylindrical shape (diameter 3 mm × height 2 mm) was used.
[0028]
In the mixed solvent (3), ethyl acetate is a good solvent, and isopropyl alcohol and methanol are poor solvents. The cylindrical solid material can be used by simply cutting polyethylene resin that has been injection-molded into a long rod shape with an appropriate size, and scraping properties of acrylic resin (9) attached to the inner wall surface (1a) Is good. The frequency of washing the reaction vessel (1) with the cleaning material according to the present invention varies depending on the amount of the acrylic resin (9) attached, but in this example, it was carried out once every 30 polymerization reactions.
[0029]
At the time of washing, 5100 kg of the mixed solvent (3) is supplied from the solvent tank (5) by the solvent pump (23) to the 6000 L reaction vessel (1) shown in FIG. The reaction vessel (1) was supplied from the tank (6) by the feeder (7). The mixed solvent (3) was sprayed in a shower from the nozzle (8a) of the upper ring (8) in the reaction vessel (1) and filled into the reaction vessel (1). Next, the temperature of the filled cleaning material was maintained at 50 ° C., and the cleaning material was stirred with a stirrer (2) as shown in FIG. As a result, the acrylic resin (9) adhering to the inner wall surface (1a) is dissolved and removed by the solvent (3), and at the same time, the remaining acrylic resin (9) that has not been removed by dissolution is collided with the solid substance (4). It peeled from the wall surface (1a). Stirring was performed at a speed of 20 to 80 rpm for 5 to 8 hours, and half of the time was reversed so that the solid substance (4) collided with the inner wall surface (1a) efficiently. Stirring was completed by setting the temperature to 30 ° C. and the stirring speed to 20 rpm before the stirring was completed.
[0030]
After the stirring, the valve (11) is opened, the mixed solvent (3) containing the solid substance (4) and the peeled acrylic resin (9) is extracted from the reaction vessel (1) into the bucket tank (6), and the mixed solvent ( 3) passed through the opening of the separator (22) and was stored in the diatomaceous earth charging tank (10) together with the bucket tank (6). The mixed solvent (3) in the diatomite charging tank (10) was returned to the reaction vessel (1) by the circulation pump (24) with the valves (15) and (13) opened. This circulation was performed for 30 to 40 minutes, and 2 kg of diatomaceous earth was charged into the diatomaceous earth charging tank (10) when the solid substance (4) in the reaction vessel (1) was almost extracted. At the same time, the valves (11) and (13) were closed, the valve (14) was opened, and diatomaceous earth was precoated on the filter (20) with the circulation pump (24). When the mixed solvent (3) containing diatomaceous earth almost disappeared in the diatomaceous earth charging tank (10), 4 kg of diatomaceous earth was further introduced into the reaction vessel (1) from the inlet (not shown), the valve (12) was opened, the valve ( 15) was closed and the filter (20) was precoated. Thereby, the mixed solvent (3) was circulated again through the paths of the reaction vessel (1), the strainer (21), the circulation pump (24), the filter (20), and the reaction vessel (1). At this time, the acrylic resin (9) having a large particle size contained in the mixed solvent (3) is separated by the strainer (21), and the acrylic resin (9) having a small particle size is filtered by the filter (20). The mixed solvent (3) can always be supplied to the reaction vessel (1) in a purified state. After circulating with the mixed solvent (3) for 90 minutes, the valve (16) was closed, the valve (17) was opened, and the mixed solvent (3) was returned to the solvent tank (5). The mixed solvent (3) is filtered with high accuracy by the filter (20) pre-coated with diatomaceous earth, so the performance as a solvent does not deteriorate, and every 4 to 5 years, except for replenishing the shortage. Replace it. The solid material (4) can also be reused, and a replenishment amount of about 5% per year is sufficient. Finally, the inside of the reaction vessel (1) was rinsed with toluene to complete the washing of the reaction vessel (1).
[0031]
After the completion of washing, the inside of the reaction vessel (1) was observed and compared with the state before washing according to the present invention. The state of the inner wall (1a) by the naked eye and finger touch before washing is that the adhesive resin (9) is fixed to the entire surface with a thickness of 0.1 to 1.0 mm, has a rough feeling, and the visual glossy state is Although it was in a frosted state, the state of the inner wall surface (1a) by the naked eye and the finger touch after washing has no sticking of the adhesive resin (9) on the entire surface, there is a smooth feeling, and the visual glossy state is a metallic mirror gloss was there. Since the inner wall surface (1a) after washing according to the present invention has no adhesive resin (9) on the entire surface and is washed to a glossy state, the cleaning material according to the present invention is used to clean the reaction vessel (1). It was confirmed that the adhesive resin (9) could be completely removed by washing the inner wall surface (1a).
[0032]
In this embodiment, the following effects can be obtained.
[1] Due to the synergistic effect of dissolution, permeation and swelling with the mixed solvent (3) of the good and poor solvents, and peeling with the solid substance (4), the adhesive resin (9) in the reaction vessel (1) is almost eliminated. Can be completely removed.
[2] Since impurities do not adhere to the inner wall surface (1a) of the reaction vessel (1) after removal of the adhesive resin (9), the reaction yield and quality of the next reaction product can be improved.
[3] Since the worker does not need to perform the peeling work in the reaction vessel (1), the working environment is improved.
[4] The conventional two-day cleaning operation can be shortened to about 12 hours, the cleaning time of the reaction vessel (1) can be shortened, and the operating rate can be improved.
[5] Since the solvent cost and labor cost can be saved, the cleaning cost can be greatly reduced.
[0033]
【The invention's effect】
As described above, in the present invention, the adhesive resin can be reliably removed in a short time to improve the cleaning efficiency and product quality, and to reduce the cleaning cost.
[Brief description of the drawings]
FIG. 1 is a schematic view showing a state in which a reaction vessel is cleaned with a cleaning material according to the present invention. FIG. 2 is an enlarged view of an inner wall surface of the reaction vessel shown in FIG. Flow diagram for cleaning [Explanation of symbols]
(1) ・ ・ Reaction vessel, (1a) ・ ・ Surface (inner wall surface), (2) ・ ・ Agitator, (2a) ・ ・ Shaft, (2b) ・ ・ Agitator blade, (2C) ・ ・ Motor, ( 3) ・ ・ Solvent (mixed solvent), (4) ・ ・ Solid material, (5) ・ ・ Container tank (solvent tank), (6) ・ ・ Container tank (bucket tank), (7) ・ ・ Feeder, ( 8) ・ ・ Upper ring, (8a) ・ ・ Nozzle, (9) ・ ・ Adhesive resin (acrylic resin), (10) ・ ・ Diatomite filling tank, (11) to (17) ・ ・ Valve, (20)・ ・ Filter, (20a) ・ ・ Filter plate, (21) ・ ・ Strainer, (22) ・ ・ Separator, (23) ・ ・ Solvent pump, (24) ・ ・ Circulating pump,

Claims (19)

100 parts by weight of a mixed solvent composed of a good solvent for dissolving and swelling the adhesive resin fixed to the surface to be cleaned and a poor solvent for curing the swollen adhesive resin, and a maximum length of 0.1 to 0.1 not dissolved in the mixed solvent Filling a reaction vessel with a cleaning material consisting of 10 to 30 parts by weight of a 50 mm solid substance;
Flowing the cleaning material in the reaction vessel;
Dissolve, permeate, and swell the adhesive resin that adheres to the inner wall surface of the reaction vessel with a mixed solvent, and collide the solid substance that flows with the mixed solvent against the inner wall surface of the reaction vessel to physically peel the swollen adhesive resin. And a process of
A method for cleaning a chemical reaction container, comprising a step of removing the dissolved and peeled adhesive resin from the reaction container together with the cleaning material. Recovering the cleaning material used for cleaning from the reaction vessel;
Separating the solid material from the recovered cleaning material;
Supplying the separated solid substance and the mixed solvent to the reaction vessel;
The method for cleaning a chemical reaction container according to claim 1, further comprising a step of flowing a cleaning material in the reaction container. Filtering the cleaning material used for cleaning to remove the adhesive resin;
Adjusting and regenerating the cleaning material by mixing the mixed solvent and the solid substance;
The method for cleaning a chemical reaction container according to claim 1, further comprising a step of reusing the regenerated cleaning material.   The method for cleaning a chemical reaction container according to any one of claims 1 to 3, wherein the adhesive resin is a resinous substance attached to the inner wall surface of the reaction container.   The mixed solvent is 20 to 70% by weight of an ester having a molecular weight of 100 or less, which is a good solvent, and 30 to 80% by weight of an alcohol having 1 to 6 carbon atoms, which is a poor solvent. Cleaning method for chemical reaction vessel.   The method for cleaning a chemical reaction container according to any one of claims 1 to 5, wherein the solid substance is formed into a cylindrical shape, a spherical shape, a polyhedral shape, a confetti shape or a tetrapod shape.   The method for cleaning a chemical reaction container according to any one of claims 1 to 6, wherein the solid substance is a polyolefin resin, a polyester resin, a phenol resin, a melamine resin, a urea resin, an epoxy resin, a silicon resin, or a fluororesin.   The method for cleaning a chemical reaction container according to claim 7, wherein the solid substance is polyethylene, polypropylene, polyethylene terephthalate, or polytetrafluoroethylene. In the chemical reaction container cleaning apparatus for cleaning and removing the adhesive resin fixed to the inner wall surface of the reaction container from the inner wall surface by a chemical reaction,
A supply device for supplying a reaction vessel with a mixed solvent composed of a good solvent for dissolving and swelling the adhesive resin and a poor solvent for curing the swollen adhesive resin, and a solid substance for physically peeling the adhesive resin;
A stirrer that causes a cleaning material containing a mixed solvent and a solid substance to flow and collides the solid substance with the swollen adhesive resin;
A separator that separates the cleaning material used for cleaning into a mixed solvent and a solid substance;
A filter that purifies the mixed solvent by removing the adhesive resin from the separated mixed solvent;
A cleaning apparatus for a chemical reaction container, comprising: a purified mixed solvent and a storage tank for storing a separated solid substance.   The apparatus for cleaning a chemical reaction container according to claim 9, further comprising a circulation pump for returning the mixed solvent purified by the filter into the reaction container and circulating between the filter and the reaction container.   A good solvent that dissolves and swells the adhesive resin that adheres to the surface to be cleaned, a poor solvent that cures the swollen adhesive resin, and a solid substance that impacts the surface to be cleaned and physically separates the adhesive resin And a cleaning material for a chemical reaction vessel.   The cleaning material for a chemical reaction container according to claim 11, wherein the poor solvent is one or more of alcohol, petroleum ether, aliphatic hydrocarbon, and water.   The cleaning material for a chemical reaction container according to claim 11 or 12, wherein the good solvent is one or more of esters, ketones, halides, aromatic hydrocarbons, alcohols, alkalis and water.   The cleaning material for a chemical reaction container according to any one of claims 11 to 13, wherein the solid substance is formed in a cylindrical shape, a spherical shape, a polyhedral shape, a confetti shape, or a tetrapod shape.   The cleaning material for a chemical reaction container according to any one of claims 11 to 14, wherein the solid substance is a polyolefin resin, a polyester resin, a phenol resin, a melamine resin, a urea resin, an epoxy resin, a silicon resin, or a fluorine resin.   The cleaning material for a chemical reaction container according to claim 15, wherein the solid substance is polyethylene, polypropylene, polyethylene terephthalate, or polytetrafluoroethylene.   The cleaning material for a chemical reaction container according to any one of claims 11 to 16, wherein the adhesive resin is a resin fixed to surfaces in the reaction container and the pipe.   100 parts by weight of a mixed solvent containing 20 to 70% by weight of an ester having a molecular weight of 100 or less which is a good solvent and 30 to 80% by weight of an alcohol having 1 to 6 carbon atoms which is a poor solvent, and a solid having a maximum length of 0.1 to 50 mm The cleaning material for a chemical reaction container according to any one of claims 11 to 17, comprising 10 to 30 parts by weight of a substance.   The cleaning material for a chemical reaction container according to any one of claims 11 to 18, wherein the density ratio of the mixed solvent and the solid substance is 1: 0.9 to 1.4.

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