CN210434006U - Production equipment for producing polyformaldehyde dimethyl ether through partition wall catalytic distillation - Google Patents
Production equipment for producing polyformaldehyde dimethyl ether through partition wall catalytic distillation Download PDFInfo
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Abstract
The utility model relates to a production facility of next door catalytic distillation production polyformaldehyde dimethyl ether, equipment includes next door catalytic distillation tower and product refining tower, its production method, including following step: feeding a methylal solution of trioxymethylene from an upper feed inlet of a main tower of a bulkhead catalytic rectifying tower, feeding raw material methylal from a lower feed inlet of the main tower of the bulkhead catalytic rectifying tower, and carrying out an aldolization reaction on the raw material trioxymethylene and the methylal in the middle of the main tower of the bulkhead catalytic rectifying tower and carrying out vapor-liquid mass transfer; condensing mixed steam obtained from the top of the auxiliary tower of the bulkhead catalytic distillation tower by a condenser; and (3) feeding a polyformaldehyde dimethyl ether crude product discharged from the tower kettle of the bulkhead catalytic rectification tower into the middle part of a product refining tower for rectification separation, and condensing mixed steam obtained from the tower top by a condenser to obtain a polyformaldehyde dimethyl ether product. The utility model discloses take off light integrated going on to same tower with consecutive acetal reaction, product, this equipment has advantages such as the conversion rate is high, the selectivity is high, the energy consumption is low and the equipment investment is few.
Description
Technical Field
The utility model relates to a production field of novel green oxygenated fuel compound and environment-friendly solvent especially relates to a production facility of next door catalytic distillation production polyformaldehyde dimethyl ether.
Background
In recent years, the continuous appearance of haze weather in partial areas of China, particularly in northern areas, seriously threatens the physical and mental health of people, and arouses wide attention of people to the quality of fossil oil products and the emission of automobile exhaust. Compared with an internal combustion type gasoline engine, the compression ignition type diesel engine has higher thermal efficiency and wider application range, but the development of the compression ignition type diesel engine is always limited by the emission problem, mainly the emission problem of nitrogen oxides and particulate matters. Therefore, how to make the exhaust emission of the diesel engine meet the increasingly strict emission regulations on the premise of keeping the economy, the dynamic property and the reliability of the diesel engine becomes a hot spot of research of energy and environment workers at present. The Cetane Number (CN) is an important parameter for representing the combustion performance of diesel oil, the increase of the CN of the diesel oil can obviously reduce the stagnation period of the diesel oil, the CN of the diesel oil in China is generally low at present, and how to increase the CN of the diesel oil to reduce the emission of diesel engine particles and nitrogen oxides becomes an important research subject for energy conservation and emission reduction of automobiles.
Practice proves that the addition of the oxygen-containing compound in the diesel can reduce the emission of nitrogen oxides and particulate matters in the tail gas of the diesel engine. Methanol, dimethyl ether and methylal have been widely studied as diesel additives due to high oxygen content, but the cetane number of methanol is low, which affects the combustion performance of diesel, the low solubility and low boiling point of dimethyl ether make the blend of dimethyl ether and diesel unstable under normal pressure, which requires storage under pressure, and has poor miscibility with diesel, and methylal shows excellent performance in reducing the emission of pollutants in tail gas, but the cetane number, viscosity and boiling point are low, which is not suitable diesel additive.
Polyoxymethylene dimethyl ethers (DMM for short) as a novel oxygen-containing fuel compoundn) Has the chemical formula of CH3O(CH2O)nCH3N is not less than 1, wherein DMM3-8Has a higher cetane number (>76) The diesel additive has the advantages of oxygen content (45-51%), physical and chemical properties close to those of diesel, good intersolubility with the diesel and the like, can be directly added into the diesel for use, does not need to modify the diesel, can effectively improve the combustion condition of the diesel in an engine, improves the heat efficiency, remarkably reduces the emission of nitrogen oxides and particulate matters, can remarkably improve the lubricity of the diesel, and is a novel environment-friendly diesel additive with great application prospect. Research shows that 10-30% of DMM is added into diesel oil3-8The method can reduce the discharge amount of particulate matters in the tail gas by 80-90% and reduce the discharge amount of nitrogen oxides by 50%. At present, the consumption of diesel oil for vehicles in China is over 1.5 hundred million tons every year, and if the diesel oil is added according to a proportion of 15 percent, DMM is added3-8The annual demand will exceed 2250 ten thousand tons, so the product has been classified as a new chemical product for key development in the country.
The synthesis process of the polyoxymethylene dimethyl ether is a series of consecutive acetal reactions, and products are distributed in DMM1-DMM8The effective component is DMM3-8. The aldolization reaction is a typical acid catalytic reaction, the commonly used catalyst at present mainly comprises liquid acid such as sulfuric acid, trifluoromethanesulfonic acid, hydrochloric acid, hydrofluoric acid and the like, and as the acid has strong corrosivity and toxicity, the problems of equipment corrosion, unreasonable distribution of reaction products, difficulty in separating homogeneous reaction products and the catalyst and the like exist. The prior report of using acidic cation exchange resin solid acid as a catalyst to produce polyoxymethylene dimethyl ethers. For example, Chinese patents CN107915605A, CN107915603A, CN109651098A and CN102786397A disclose cation exchange resins as catalystsThe method for producing the polyoxymethylene dimethyl ether, however, the solid acids have the defects of low temperature resistance, poor catalytic activity, low selectivity and the like.
The catalytic rectification method of trioxymethylene and methylal couples the reaction process and the rectification separation in the tower, so that the serial acetal reaction and the product separation process are carried out simultaneously, the concentration of reactants in the reaction section is improved, the product is timely separated from the reaction section, the reaction balance is promoted to move forward, the conversion rate and the selectivity of the serial acetal reaction are improved, and the energy consumption is reduced. Because the reactant in the consecutive acetal reaction system is a low boiling point component, the tower top component of the catalytic rectifying tower is the raw material methylal DMM1And DMM2The top of the tower needs total reflux operation, and all reaction liquid enters the rectifying tower from the bottom of the catalytic rectifying tower to be refined. However, the light components with higher concentration exist in the bottom of the catalytic distillation tower at the same time, so that the reverse reaction is promoted, and the catalytic distillation conversion rate and selectivity are low.
SUMMERY OF THE UTILITY MODEL
Technical problem to be solved
In order to solve the problems in the prior art, the utility model provides a production device for producing polyformaldehyde dimethyl ether by catalytic rectification of a partition wall, which uses a polymerization ionic liquid as a catalyst, and has high temperature resistance and good catalytic activity; meanwhile, the bulkhead catalytic distillation equipment is manufactured by arranging the partition plate in the conventional catalytic distillation tower, so that the light component methylal DMM can be separated in time1And DMM2And the reverse reaction is inhibited, and the energy consumption and the equipment investment are effectively reduced.
(II) technical scheme
In order to achieve the above object, the utility model discloses a main technical scheme include:
a production facility of next door catalytic distillation production polyformaldehyde dimethyl ether, it includes: next door catalytic distillation tower and product refining tower, well upper portion in the next door catalytic distillation tower is equipped with a vertical baffle, the upper end of vertical baffle with the interior top of next door catalytic distillation tower is connected, and vertical baffle separates into three region with next door catalytic distillation tower internal partitioning: a main tower formed by the middle upper part of the bulkhead catalytic rectifying tower and the left side of the vertical clapboard, an auxiliary tower formed by the middle upper part of the bulkhead catalytic rectifying tower and the right side of the vertical clapboard, and a public stripping section at the lower part of the bulkhead catalytic rectifying tower;
the bottom of the bulkhead catalytic rectifying tower is provided with a bulkhead catalytic rectifying tower extraction outlet corresponding to the public stripping section, the top of the bulkhead catalytic rectifying tower is provided with a main tower top extraction product corresponding to the main tower, and the upper part of the bulkhead catalytic rectifying tower is provided with a methylal feeding port, a trioxymethylene feeding port and a main tower reflux port corresponding to the main tower; the top of the bulkhead catalytic rectifying tower is provided with an auxiliary tower top extraction port corresponding to the auxiliary tower, and the top of the bulkhead catalytic rectifying tower is provided with an auxiliary tower reflux port corresponding to the auxiliary tower; the trioxymethylene feeding port is connected with a trioxymethylene feeding pipe;
the top of the product refining tower is provided with a product outlet, and the middle of the product refining tower is provided with a polyformaldehyde dimethyl ether DMM3-8A crude product feeding hole, wherein a product refining tower reflux opening is formed in the upper part of the product refining tower, and a high-boiling discharge opening is formed in the bottom of the product refining tower;
the top gas phase outlet of the main tower at the top of the catalytic distillation tower of the bulkhead is connected with a main tower condenser of the catalytic distillation tower of the bulkhead through a gas phase pipe at the top of the main tower of the catalytic distillation tower of the bulkhead, the outlet end of the main tower condenser of the catalytic distillation tower of the bulkhead is connected with a reflux port of the main tower through a reflux pipe of the main tower of the catalytic distillation tower of the bulkhead, the top gas phase outlet of the auxiliary tower at the top of the catalytic distillation tower of the bulkhead is connected with a condenser of the auxiliary tower of the catalytic distillation tower of the bulkhead through a gas phase pipe at the top of the auxiliary tower of the catalytic distillation tower of the bulkhead, and the outlet end of the condenser of the auxiliary tower of the catalytic distillation tower of the; the outlet end of the auxiliary tower condenser of the bulkhead catalytic rectifying tower is communicated with a light component feeding pipe connected to a methylal feeding hole through an auxiliary tower top outlet pipe of the bulkhead catalytic rectifying tower, and the outlet pipe of the auxiliary tower top of the bulkhead catalytic rectifying tower, a bulkhead catalytic rectifying tower return pipe and the outlet end of the auxiliary tower condenser of the bulkhead catalytic rectifying tower are connected by a three-way joint; the light component feeding pipe is connected with a methylal feeding pipe; the extraction port of the bulkhead catalytic distillation tower is connected with bulkhead catalytic distillationThe other end of the distillation tower kettle extraction pipe and the polyformaldehyde dimethyl ether DMM are catalyzed by the partition wall3-8The feed inlets of the coarse products are connected;
a product outlet at the top of the product refining tower is connected with a product refining tower condenser through a product refining tower top gas phase pipe, an outlet end of the product refining tower condenser is connected with a product refining tower reflux opening through a product refining tower reflux pipe, an outlet end of the product refining tower condenser is connected with a product refining tower top extraction pipe, and the product refining tower reflux pipe, the product refining tower top extraction pipe and the outlet end of the product refining tower condenser are connected through a three-way connector; and a high-boiling discharge port at the bottom of the product refining tower is connected with a product refining tower kettle extraction pipe.
Furthermore, the public stripping section of the bulkhead catalytic rectifying tower passes through a first circulating reboiling pipeline, a bulkhead catalytic rectifying tower reboiler is connected to the first circulating reboiling pipeline, and the outlet end of the bulkhead catalytic rectifying tower reboiler is communicated with the public stripping section of the bulkhead catalytic rectifying tower.
Furthermore, the product refining tower is externally connected with a product refining tower reboiler through a second circulating reboiling pipeline, and the outlet end of the product refining tower reboiler is connected with the lower part of the product refining tower.
Further, the vertical partition is eccentrically disposed in the divided wall catalytic distillation column such that a cross-sectional area ratio of the sub-column to the main column is greater than or equal to 0.32 and less than 1.0.
Further, the column internals types of the divided wall catalytic distillation column comprise trays or packing or a combination of trays and packing; the main tower at the upper part of the bulkhead catalytic rectifying tower consists of a rectifying section positioned above a trioxymethylene feed inlet, a reaction section positioned between the trioxymethylene feed inlet and a methylal feed inlet and a stripping section positioned below the methylal feed inlet, wherein the reaction section is filled with a polymeric ionic liquid catalyst, the reaction section is provided with 12-24 theoretical plates, the rectifying section is provided with 8-18 theoretical plates, and the stripping section is provided with 10-16 theoretical plates; 18-32 theoretical plates are arranged on the auxiliary tower at the upper part of the bulkhead catalytic rectifying tower; and a common stripping section at the lower part of the bulkhead catalytic rectifying tower is provided with 12-38 theoretical plates.
Further, the product refining tower is composed of a DMM (dimethyl ether) positioned in polyformaldehyde3-8A product rectifying section above the feed inlet of the crude product and a DMM positioned above the polyoxymethylene dimethyl ether3-8And the product stripping section below the crude product feeding port is formed, the type of the tower internals of the product refining tower is tower plates or fillers, the number of theoretical plates of the product rectifying section is 15-32, and the number of theoretical plates of the product stripping section is 10-24.
(III) advantageous effects
The utility model has the advantages that: 1. by arranging the partition plate in the conventional catalytic rectifying tower to manufacture the bulkhead catalytic rectifying equipment, the light component methylal DMM can be separated in time1And DMM2And the like, inhibiting the pseudo reaction, saving the energy consumption by 20-38 percent and saving the equipment investment by 24-40 percent.
2. Under the condition of the equipment, the product after reaction is well distributed, the utilization rate of raw materials is high, the conversion rate of trioxymethylene is 100 percent, and DMM (dimethyl formamide)3-8The selectivity is over 92 percent.
Drawings
Fig. 1 is a schematic view of the overall structure of an embodiment of the present invention.
[ description of reference ]
T1 is a bulkhead catalytic rectifying tower, A is a rectifying section, B is a reaction section, C is a stripping section, D is a public stripping section, and E is an auxiliary tower rectifying section; t2 is a product refining tower; e1 is a main tower condenser of a bulkhead catalytic distillation tower; e2 is a condenser of a secondary tower of the bulkhead catalytic distillation tower; e3 is a reboiler of a bulkhead catalytic distillation tower; e4 is a product refining tower condenser; e5 is a reboiler of the product refining tower; PL01 is a trioxymethylene feeding pipe, PL02 is a methylal feeding pipe, PL03 is a light component feeding pipe, PL04 is a bulkhead catalytic rectifying tower main tower top gas phase pipe, PL05 is a bulkhead catalytic rectifying tower main tower return pipe, PL06 is a bulkhead catalytic rectifying tower auxiliary tower top gas phase pipe, PL07 is a bulkhead catalytic rectifying tower auxiliary tower return pipe, PL08 is a bulkhead catalytic rectifying tower auxiliary tower top output pipe, PL09 is a first circulation reboiling pipeline, PL10 is a bulkhead catalytic rectifying tower kettle output pipe, PL11 is a product refining tower top gas phase pipe, PL12 is a product refining tower return pipe, PL13 is a product refining tower top output pipe, PL14 is a second circulation reboiling pipeline, and PL15 is a product refining tower kettle output pipe.
Detailed Description
For a better understanding of the present invention, reference will now be made in detail to the present invention, examples of which are illustrated in the accompanying drawings.
The utility model discloses a production facility of next door catalytic distillation production polyformaldehyde dimethyl ether of embodiment, as shown in figure 1, it includes: next door catalytic distillation tower T1 and product refining tower T2, well upper portion in the next door catalytic distillation tower T1 is equipped with a vertical baffle, the upper end of vertical baffle with the interior top of next door catalytic distillation tower T1 is connected, and vertical baffle divides into three region with the inside partition of next door catalytic distillation tower T1: a main tower formed by the middle upper part of the bulkhead catalytic rectifying tower T1 and the left side of the vertical clapboard, an auxiliary tower formed by the middle upper part of the bulkhead catalytic rectifying tower T1 and the right side of the vertical clapboard, and a public stripping section D at the lower part of the bulkhead catalytic rectifying tower T1;
the bottom of the bulkhead catalytic rectifying tower T1 is provided with a bulkhead catalytic rectifying tower extraction outlet corresponding to the public stripping section, the top of the bulkhead catalytic rectifying tower T1 is provided with a main tower top extraction product corresponding to the main tower, and the upper part of the bulkhead catalytic rectifying tower T1 is provided with a methylal feeding hole, a trioxymethylene feeding hole and a main tower reflux opening corresponding to the main tower; an auxiliary tower top outlet is formed in the top of the bulkhead catalytic rectifying tower T1 corresponding to the auxiliary tower, and an auxiliary tower reflux opening is formed in the top of the bulkhead catalytic rectifying tower T1 corresponding to the auxiliary tower; a trioxymethylene feeding pipe PL01 is connected to the trioxymethylene feeding hole;
the top of the product refining tower T2 is provided with a product outlet, and the middle part of the product refining tower T2 is provided with a polyoxymethylene dimethyl ether DMM3-8A crude product feeding hole, wherein a product refining tower reflux hole is formed in the upper part of the product refining tower T2, and a high-boiling discharge hole is formed in the bottom of the product refining tower T2;
a main tower top outlet at the top of the bulkhead catalytic rectifying tower T1 is connected with a bulkhead catalytic rectifying tower main tower condenser E1 through a bulkhead catalytic rectifying tower main tower top gas-phase pipe PL04, and the outlet of the bulkhead catalytic rectifying tower main tower condenser E1The inlet end of the main tower reflux pipe PL05 of the catalytic distillation tower with the separating wall is connected with the main tower reflux inlet, the top outlet of the auxiliary tower at the top of the catalytic distillation tower T1 with the separating wall is connected with the auxiliary tower condenser E2 of the catalytic distillation tower with the separating wall through the gas phase pipe PL06 of the top of the auxiliary tower of the catalytic distillation tower with the separating wall, and the outlet end of the auxiliary tower condenser E2 of the catalytic distillation tower with the separating wall is communicated with the auxiliary tower reflux inlet through the auxiliary tower reflux pipe PL07 of the catalytic distillation tower with the separating wall; the outlet end of the auxiliary tower condenser E2 of the bulkhead catalytic rectifying tower is communicated with a light component feeding pipe PL03 connected to a methylal feeding hole through an auxiliary tower top extraction pipe PL08 of the bulkhead catalytic rectifying tower, and the auxiliary tower top extraction pipe PL08 of the bulkhead catalytic rectifying tower, an auxiliary tower return pipe PL07 of the bulkhead catalytic rectifying tower and the outlet end of the auxiliary tower condenser E2 of the bulkhead catalytic rectifying tower are connected by a three-way joint; a methylal feeding pipe PL02 is connected to the light component feeding pipe PL 03; the extraction port of the bulkhead catalytic rectifying tower is connected with a bulkhead catalytic rectifying tower kettle extraction pipe PL10, and the other end of the bulkhead catalytic rectifying tower kettle extraction pipe PL10 and the polyoxymethylene dimethyl ether DMM3-8The feed inlets of the coarse products are connected;
a product outlet at the top of the product refining tower T2 is connected with a product refining tower condenser E4 through a product refining tower top gas phase pipe PL11, the outlet end of the product refining tower condenser E4 is connected with a product refining tower reflux opening through a product refining tower reflux pipe PL12, the outlet end of the product refining tower condenser E4 is connected with a product refining tower top extraction pipe PL13, and the product refining tower reflux pipe PL12, the product refining tower top extraction pipe PL13 and the outlet end of the product refining tower condenser E4 are connected through a three-way joint; and a high-boiling discharge port at the bottom of the product refining tower T2 is connected with a product refining tower kettle extraction pipe PL 15.
Furthermore, the common stripping section of the bulkhead catalytic distillation column T1 passes through a first circulating reboiling pipeline PL09, a bulkhead catalytic distillation column reboiler E3 is connected to the first circulating reboiling pipeline PL09, and the outlet end of the bulkhead catalytic distillation column reboiler E3 is communicated with the common stripping section of the bulkhead catalytic distillation column T1.
Further, a product refining column reboiler E5 is connected to the outside of the product refining column T2 through a second circulating reboiler line PL14, and an outlet end of the product refining column reboiler E5 is connected to a lower portion of the product refining column T2.
Further, the vertical partition is eccentrically disposed in the divided wall catalytic distillation column T1 such that the cross-sectional area ratio of the auxiliary column to the main column is greater than or equal to 0.32 and less than 1.0.
Further, the column internals of the divided wall catalytic distillation column T1 comprise trays or packing or a combination of trays and packing; the main tower at the upper part of the bulkhead catalytic rectifying tower T1 consists of a rectifying section A positioned above a trioxymethylene feeding hole, a reaction section B positioned between the trioxymethylene feeding hole and a methylal feeding hole and a stripping section C positioned below the methylal feeding hole, wherein the reaction section B is filled with a polymerization ionic liquid catalyst, the reaction section B is provided with 12-24 theoretical plates, the rectifying section A is provided with 8-18 theoretical plates, and the stripping section C is provided with 10-16 theoretical plates; an auxiliary tower at the upper part of the bulkhead catalytic rectifying tower T1 is provided with 18-32 theoretical plates; and a common stripping section D at the lower part of the bulkhead catalytic rectifying tower T1 is provided with 12-38 theoretical plates.
Further, the product refining tower T2 is prepared by adding DMM (dimethyl ether) in polyoxymethylene3-8A product rectifying section above the feed inlet of the crude product and a DMM positioned above the polyoxymethylene dimethyl ether3-8And the product stripping section below the crude product feeding port is formed, the type of the tower internals of the product refining tower T2 is tower plates or fillers, the number of theoretical plates of the product rectifying section is 15-32, and the number of theoretical plates of the product stripping section is 10-24.
Furthermore, the catalyst filled in the reaction section B of the main tower of the bulkhead catalytic distillation tower T1 is a polymerization ionic liquid catalyst,
further, the production method of the production equipment for producing the polyoxymethylene dimethyl ether by the bulkhead catalytic rectification comprises the following specific steps:
step S1: feeding a methylal solution of raw material trioxymethylene into the upper part of a main tower of a bulkhead catalytic rectifying tower T1 from a trioxymethylene feeding pipe PL01 through a trioxymethylene feeding pipe PL01, feeding the raw material methylal into the lower part of the main tower of the bulkhead catalytic rectifying tower T1 from a methylal feeding pipe PL02, and feeding the raw material trioxymethylene and the methylal into a reaction section B of the main tower at the upper part of the bulkhead catalytic rectifying tower T1The polymerization ionic liquid catalyst in the system is catalyzed to carry out consecutive acetal reaction and carry out vapor-liquid mass transfer, the vapor ascending at the top of the main tower realizes phase change through a main tower condenser E1 of the bulkhead catalytic rectifying tower, and all the materials obtained by condensation flow back into the bulkhead catalytic rectifying tower T1; the material descending from the stripping section C of the bulkhead catalytic rectifying tower T1 enters a public stripping section of the bulkhead catalytic rectifying tower T1, the material extracted from the bottom of the public stripping section passes through a bulkhead catalytic rectifying tower reboiler E3, gas-liquid mass transfer exchange is carried out in an auxiliary tower of the bulkhead catalytic rectifying tower T1, the steam ascending from the top of the auxiliary tower realizes phase change through an auxiliary tower condenser E2 of the bulkhead catalytic rectifying tower, and the light component material DMM obtained by condensation1-2One part of the mixture flows back into the catalytic distillation column T1 from the reflux inlet of the auxiliary column, and the other part of the mixture returns into the catalytic distillation column T1 from the methylal feed inlet of the catalytic distillation column T1 for recycling;
step S2: polyoxymethylene dimethyl ether DMM extracted from the bottom of a bulkhead catalytic rectifying tower T13-8The crude product enters a product refining tower T2 through a separation wall catalytic rectifying tower kettle extraction pipe PL10 for rectification, steam rising from the top of the product refining tower T2 realizes phase change through a product refining tower condenser E4, and the material obtained by condensation is polyoxymethylene dimethyl ether DMM3-8One part of the product flows back into the product refining tower from a product refining tower reflux inlet at the upper part of the product refining tower T2, the other part is extracted from a product refining tower top extraction pipe PL13, and high boiling in the product refining tower T2 is discharged from a high boiling discharge outlet at the bottom of the product refining tower through a product refining tower kettle extraction pipe PL 15.
Furthermore, the operation pressure of the bulkhead catalytic rectifying tower T1 is 100-1200 kPa, the top total reflux of the bulkhead catalytic rectifying tower T1 main tower is performed, and the top reflux ratio of the bulkhead catalytic rectifying tower T1 auxiliary tower is 2.2-4.8.
Further, the operating conditions within the product refining column T2 are set to: the operation pressure at the top of the tower is 10-100 kPa, and the reflux ratio at the top of the tower is 0.6-4.5.
Example 1
The bulkhead catalytic rectification tower T1 is a packed tower with the tower diameter of 50mm, the tower body and the packing are both 316L, the packing type is theta ring packing with the specification of phi 3 multiplied by 3, the tower height is 4.5m, the theoretical plate number of the rectification section A is 10, the theoretical plate number of the reaction section B is 14, the catalyst filled in the reaction section B is a polymeric ionic liquid catalyst, the theoretical plate number of the stripping section C is 12, the theoretical plate number of the rectification section E of the auxiliary tower is 28, the theoretical plate number of the public stripping section D is 24, and the cross-sectional area ratio of the auxiliary tower to the main tower is 0.4; the product refining tower T2 is a packed tower with a tower diameter of 40mm, the tower body and the packing are both 316L, the packing type is phi 3 multiplied by 3 specification theta ring packing, the tower height is 3m, the theoretical plate number of the product rectifying section is 20, and the theoretical plate number of the product stripping section is 12.
Feeding a methylal solution of trioxymethylene from the upper part of a bulkhead catalytic rectifying tower T1 at a flow rate of 6g/min, wherein the trioxymethylene content in the solution is 60 percent, and the mass fraction is the same as the following; methylal was fed from the lower portion of the divided wall catalytic distillation column T1 at a flow rate of 5 g/min. Operating conditions of the divided wall catalytic distillation column T1: the pressure at the top of the tower is normal pressure, the temperature at the top of the main tower is 45.3 ℃, the total reflux of the main tower is realized, the temperature at the top of the auxiliary tower is 52.6 ℃, the reflux ratio of the auxiliary tower is 3.0, and the temperature at the bottom of the tower is 130.5 ℃; operating conditions of the product refining column T2: the pressure at the top of the column was 25, the temperature at the top of the column was 92.4 ℃, the temperature at the bottom of the column was 113.5 ℃ and the reflux ratio was 3.8.
Under the conditions, the conversion rate of trioxymethylene in the bulkhead catalytic rectifying tower T1 is 100 percent, and DMM (dimethyl formamide)3-8Selectivity 92.5%, DMM in the top of product refining tower T23-8The total content is 99.1%.
Example 2:
the bulkhead catalytic rectifying tower T1 is a packed tower with a tower diameter of 50mm, the tower body and the packing are both 316L, the packing type is theta ring packing with phi 3 multiplied by 3 specification, the tower height is 4.5m, the theoretical plate number of the rectifying section A is 10, the theoretical plate number of the reaction section B is 14, the catalyst filled in the reaction section B is a polymeric ionic liquid catalyst, the theoretical plate number of the stripping section C is 12, the theoretical plate number of the rectifying section E of the auxiliary tower is 28, the theoretical plate number of the public stripping section D is 24, and the cross-sectional area ratio of the auxiliary tower to the main tower is 0.4. The product refining tower T2 is a packed tower with a tower diameter of 40mm, the tower body and the packing are both 316L, the packing type is phi 3 multiplied by 3 specification theta ring packing, the tower height is 3m, the theoretical plate number of the product rectifying section is 20, and the theoretical plate number of the product stripping section is 12.
Feeding a methylal solution of trioxymethylene from the upper part of a bulkhead catalytic rectifying tower at a flow rate of 5g/min, wherein the trioxymethylene content in the solution is 40%, and the mass fraction is the same as below; methylal was fed from the lower part of the divided wall catalytic distillation column T1 at a flow rate of 3g/min, and the operating conditions of the divided wall catalytic distillation column T1 were: the pressure at the top of the tower is normal pressure, the temperature at the top of the main tower is 43.6 ℃, the total reflux of the main tower is realized, the temperature at the top of the auxiliary tower is 49.2 ℃, the reflux ratio of the auxiliary tower is 3.5, and the temperature at the bottom of the tower is 132.6 ℃; operating conditions of the product refining column T2: the pressure at the top of the column was 25, the temperature at the top of the column was 96.7 ℃, the temperature at the bottom of the column was 115.7 ℃ and the reflux ratio was 3.5.
Under the conditions, the conversion rate of trioxymethylene in the bulkhead catalytic rectifying tower T1 is 100 percent, and DMM (dimethyl formamide)3-8Selectivity 94.2%, DMM in the top of product refining tower T23-8The total content is 99.4%.
As mentioned above, under the conditions of the process and the equipment, the product after the reaction is well distributed, the utilization rate of the raw material is high, the conversion rate of trioxymethylene is 100 percent, and DMM (dimethyl formamide)3-8The selectivity is over 92 percent.
The above is only the preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (6)
1. The utility model provides a production facility of bulkhead catalytic distillation production polyformaldehyde dimethyl ether which characterized in that, it includes: next door catalytic distillation tower (T1) and product refining tower (T2), well upper portion in next door catalytic distillation tower (T1) is equipped with a vertical baffle, the upper end of vertical baffle with the interior top of next door catalytic distillation tower (T1) is connected, and vertical baffle becomes three region with next door catalytic distillation tower (T1) internal partitioning: a main tower formed by the middle upper part of the bulkhead catalytic rectifying tower (T1) and the left side of the vertical clapboard, an auxiliary tower formed by the middle upper part of the bulkhead catalytic rectifying tower (T1) and the right side of the vertical clapboard, and a public stripping section (D) at the lower part of the bulkhead catalytic rectifying tower (T1);
the bottom of the bulkhead catalytic rectifying tower (T1) is provided with a bulkhead catalytic rectifying tower extraction port corresponding to the public stripping section, the top of the bulkhead catalytic rectifying tower (T1) is provided with a main tower top extraction port corresponding to the main tower, and the upper part of the bulkhead catalytic rectifying tower (T1) is provided with a methylal feeding port, a trioxymethylene feeding port and a main tower return port corresponding to the main tower; the top of the bulkhead catalytic rectifying tower (T1) is provided with an auxiliary tower top extraction port corresponding to the auxiliary tower, and the top of the bulkhead catalytic rectifying tower (T1) is provided with an auxiliary tower return port corresponding to the auxiliary tower; a trioxymethylene feeding pipe (PL01) is connected to the trioxymethylene feeding hole;
the top of the product refining tower (T2) is provided with a product outlet, and the middle of the product refining tower (T2) is provided with a polyoxymethylene dimethyl ether DMM3-8A crude product feeding hole, wherein a product refining tower reflux hole is formed in the upper part of the product refining tower (T2), and a high-boiling discharge hole is formed in the bottom of the product refining tower (T2);
a main tower top outlet at the top of the bulkhead catalytic rectifying tower (T1) is connected with a bulkhead catalytic rectifying tower main tower condenser (E1) through a bulkhead catalytic rectifying tower main tower top gas-phase pipe (PL04), the outlet end of the bulkhead catalytic rectifying tower main tower condenser (E1) is connected with a main tower return port through a bulkhead catalytic rectifying tower main tower return pipe (PL05), an auxiliary tower top outlet at the top of the bulkhead catalytic rectifying tower (T1) is connected with a bulkhead catalytic rectifying tower auxiliary tower condenser (E2) through a bulkhead catalytic rectifying tower auxiliary tower top gas-phase pipe (PL06), and the outlet end of the bulkhead catalytic rectifying tower auxiliary tower condenser (E2) is communicated with an auxiliary tower return pipe (PL07) through a bulkhead catalytic rectifying tower return pipe; the outlet end of the auxiliary tower condenser (E2) of the bulkhead catalytic rectifying tower is communicated with a light component feeding pipe (PL03) connected to a methylal feeding hole through an auxiliary tower top extraction pipe (PL08) of the bulkhead catalytic rectifying tower, and the outlet ends of the auxiliary tower top extraction pipe (PL08), the auxiliary tower reflux pipe (PL07) of the bulkhead catalytic rectifying tower and the auxiliary tower condenser (E2) of the bulkhead catalytic rectifying tower are connected by a three-way joint; a methylal feeding pipe (PL02) is connected to the light component feeding pipe (PL 03); the extraction port of the bulkhead catalytic rectifying tower is connected with a bulkhead catalytic rectifying tower kettle extraction pipe (PL10), and the other end of the bulkhead catalytic rectifying tower kettle extraction pipe (PL10) and the polyoxymethylene dimethyl ether DMM3-8The feed inlets of the coarse products are connected;
a product outlet at the top of the product refining tower (T2) is connected with a product refining tower condenser (E4) through a product refining tower top gas phase pipe (PL11), the outlet end of the product refining tower condenser (E4) is connected with a product refining tower reflux inlet through a product refining tower reflux pipe (PL12), the outlet end of the product refining tower condenser (E4) is connected with a product refining tower top extraction pipe (PL13), and the outlet ends of the product refining tower reflux pipe (PL12), the product refining tower top extraction pipe (PL13) and the product refining tower condenser (E4) are connected through a three-way joint; a high-boiling discharge port at the bottom of the product refining tower (T2) is connected with a product refining tower kettle extraction pipe (PL 15).
2. The production equipment for producing polyoxymethylene dimethyl ethers by bulkhead catalytic distillation according to claim 1, wherein the common stripping section of the bulkhead catalytic distillation column (T1) is connected to a bulkhead catalytic distillation column reboiler (E3) through a first circulating reboiler line (PL09) connected to the first circulating reboiler line (PL09), and an outlet end of the bulkhead catalytic distillation column reboiler (E3) is connected to the common stripping section of the bulkhead catalytic distillation column (T1).
3. The production equipment for producing polyoxymethylene dimethyl ethers by bulkhead catalytic distillation as claimed in claim 1, wherein a product rectifying column reboiler (E5) is connected to the outside of said product rectifying column (T2) through a second circulating reboiler piping (PL14), and an outlet end of said product rectifying column reboiler (E5) is connected to a lower portion of said product rectifying column (T2).
4. The production apparatus for polyoxymethylene dimethyl ethers by bulkhead catalytic distillation according to claim 1, wherein said vertical partition is eccentrically disposed in said bulkhead catalytic distillation column (T1) such that the ratio of the cross-sectional area of said sub-column to the main column is 0.32 or more and less than 1.0.
5. The production apparatus for polyoxymethylene dimethyl ethers by bulkhead catalytic distillation according to claim 1, wherein the type of column internals of the bulkhead catalytic distillation column (T1) comprises trays or packing or a combination of trays and packing; the main tower at the upper part of the bulkhead catalytic rectifying tower (T1) consists of a rectifying section (A) positioned above a trioxymethylene feeding hole, a reaction section (B) positioned between the trioxymethylene feeding hole and a methylal feeding hole and a stripping section (C) positioned below the methylal feeding hole, wherein the reaction section (B) is filled with a polymeric ion liquid catalyst, the reaction section (B) is provided with 12-24 theoretical plates, the rectifying section (A) is provided with 8-18 theoretical plates, and the stripping section (C) is provided with 10-16 theoretical plates; an auxiliary tower at the upper part of the bulkhead catalytic rectifying tower (T1) is provided with 18-32 theoretical plates; and a common stripping section (D) at the lower part of the bulkhead catalytic rectifying tower (T1) is provided with 12-38 theoretical plates.
6. The production equipment for producing polyoxymethylene dimethyl ethers by bulkhead catalytic distillation as claimed in claim 1, wherein the product refining column (T2) is made of DMM located in polyoxymethylene dimethyl ethers3-8A product rectifying section above the feed inlet of the crude product and a DMM positioned above the polyoxymethylene dimethyl ether3-8The product stripping section below the crude product feed inlet is composed of tower plates or fillers as column internals of a product refining column (T2), the number of theoretical plates of the product rectifying section is 15-32, and the number of theoretical plates of the product stripping section is 10-24.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114805057A (en) * | 2022-06-10 | 2022-07-29 | 福建技术师范学院 | Production method for producing butyric anhydride by bulkhead reaction and rectification |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114805057A (en) * | 2022-06-10 | 2022-07-29 | 福建技术师范学院 | Production method for producing butyric anhydride by bulkhead reaction and rectification |
| CN114805057B (en) * | 2022-06-10 | 2024-02-02 | 福建技术师范学院 | Production method for producing butyric anhydride by partition wall reaction and rectification |
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