CN212560050U - Device for producing glycol diacrylate by using low-concentration ethylene glycol - Google Patents
Device for producing glycol diacrylate by using low-concentration ethylene glycol Download PDFInfo
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- CN212560050U CN212560050U CN202021097584.6U CN202021097584U CN212560050U CN 212560050 U CN212560050 U CN 212560050U CN 202021097584 U CN202021097584 U CN 202021097584U CN 212560050 U CN212560050 U CN 212560050U
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Abstract
The utility model discloses an utilize device of low concentration ethylene glycol production glycol diacrylate, including dehydration tower, fixed bed reactor, catalytic distillation tower, heavy tower, the tower of taking off that connects gradually. The ethylene glycol-containing waste material produced in the production process of ethylene glycol is used as a raw material, and is dehydrated and then reacts with acrylic acid to remove heavy components and light components, so that the ethylene glycol diacrylate is obtained. The utility model takes the waste material generated in the production process of the ethylene glycol as the raw material, the waste material is dangerous waste and can not generate benefit, even the waste material needs to be paid for other companies to be treated, thus causing the waste of the ethylene glycol and bringing about the reduction of economic benefit and the pressure of environmental protection; the utility model discloses changing waste into valuables, the concentration of dipropylene glycol ester is more than or equal to 99.0%, ethylene glycol monoacrylate concentration is less than or equal to 1.0%, water is less than or equal to 0.1%, acrylic acid is less than or equal to 0.2%, has obvious economic benefits and environmental protection advantage.
Description
Technical Field
The utility model relates to a device of production dipropylene glycol ester, concretely relates to utilize device of low concentration ethylene glycol production dipropylene glycol ester, further relate to a device of utilizing low concentration ethylene glycol to produce high concentration dipropylene glycol ester.
Background
Ethylene Glycol Diacrylate (EGDA) belongs to a multifunctional acrylate among special acrylates. Because of containing two C-C bonds, the compound can generate addition reaction and the like with macromolecular chains containing unsaturated bonds, and becomes an ideal nucleating and crosslinking agent of the excellent impact modifier ACR of the polyvinyl chloride. EGDA is also widely used as a crosslinking agent for the preparation of coatings, adhesives and the like, and as a finishing agent, emulsifier, glazing agent and the like for paper, leather, textiles and the like.
At present, the main method for industrially synthesizing EGDA is to use concentrated sulfuric acid as a catalyst and directly esterify acrylic acid and ethylene glycol to synthesize EGDA. Although sulfuric acid has ideal catalytic activity as a catalyst, the sulfuric acid has strong oxidation and dehydration effects, so that side reactions are more, the product composition is complex, the product color is darker, the polymerization phenomenon is serious in the reaction process, troubles are brought to the refining of the product, the sulfuric acid is difficult to recycle, the sulfuric acid can be removed only by alkali washing and water washing of the product, the process is complex, acid-containing wastewater is discharged, and the environment is seriously polluted; sulfuric acid also severely corrodes equipment, and equipment replacement has to be periodically performed although enamel reactors, high-grade stainless steel pipes, and the like are used in industrial production, thereby increasing production costs.
The ethylene glycol produces a byproduct in the production process, namely a waste material containing about 10% of impurities such as 1, 2-butanediol, about 30% of ethylene glycol and the balance of water, and the waste material is treated as hazardous waste. The waste cannot generate benefit, even needs to be treated by other companies at a expense, causes the waste of the ethylene glycol, and brings about the reduction of economic benefit and the pressure of environmental protection.
Disclosure of Invention
The utility model aims to solve the technical problem that to the not enough of existence among the prior art, and provide a device that utilizes low concentration ethylene glycol to produce high concentration ethylene glycol diacrylate. The utility model discloses use acrylic acid and low concentration ethylene glycol as the raw materials, wherein ethylene glycol content is more than 20% in the low concentration ethylene glycol, especially can be a contain ethylene glycol waste material that produces in the ethylene glycol production process, is a technique that utilizes low concentration ethylene glycol to produce high concentration dipropylene glycol ester.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides an utilize device of low concentration ethylene glycol production high concentration dipropylene glycol ester, including dehydration tower, fixed bed reactor, catalytic distillation tower, heavy tower, the tower of taking off that connects gradually, its characterized in that:
dehydration tower, the top be equipped with gas vent I, the bottom is equipped with discharge gate I, the well upper portion of tower wall one side is equipped with feed inlet I, the upper portion of tower wall opposite side is equipped with backward flow mouth I, wherein: the feed inlet I is connected with a device capable of providing low-concentration ethylene glycol raw material; the exhaust port I is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, one path is connected with the reflux port I, and the other path is connected with a wastewater treatment device; the discharge port I is connected with the fixed bed reactor;
fixed bed reactor, the top is equipped with feed inlet II, the bottom is equipped with discharge gate II, wherein: the feed inlet II is divided into two paths, one path is connected with the discharge outlet I of the dehydration tower, and the other path is connected with a device capable of providing acrylic acid; the discharge port II is connected with a catalytic distillation tower;
catalytic distillation tower, the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the well upper portion of tower wall one side is equipped with feed inlet III, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet III is connected with a discharge outlet II of the fixed bed reactor; the exhaust port II is connected with a condenser II and a reflux tank II, the outlet of the reflux tank II is divided into two paths, one path is connected with the reflux port II, and the other path is connected with an acrylic acid recovery device; the discharge port III is connected with a de-weighting tower;
heavy-duty tower takes off, the top is equipped with gas vent III, the bottom is equipped with discharge gate IV, the upper portion that the middle part of tower wall one side was equipped with feed inlet IV, tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet IV is connected with a discharge outlet III of the catalytic distillation tower; the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, one path is connected with the reflux port III, and the other path is connected with the lightness-removing tower; the discharge port IV is connected with a heavy material storage tank;
the light component removing tower is characterized in that the top of the light component removing tower is provided with an exhaust port IV, the bottom of the light component removing tower is provided with a discharge port V, the middle of one side of the tower wall is provided with a feed port V, and the upper part of the other side of the tower wall is provided with a reflux port IV, wherein: the feed inlet V is connected with a reflux tank III; the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, one path is connected with the reflux port IV, and the other path is connected with a device capable of providing acrylic acid; the discharge port V at the bottom is connected with an ethylene glycol diacrylate product storage tank.
In the technical scheme, the fixed bed reactor is internally filled with a catalyst A; the catalyst A is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst.
In the technical scheme, the catalytic section of the catalytic distillation tower is filled with a catalyst B; the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst; the packing form of the catalyst B is preferably in the form of a module catalyst.
In the technical scheme, the dehydration tower, the fixed bed reactor, the catalytic distillation tower and the heavy component removal tower and the light component removal tower are all equipment in the prior art or commercially available equipment.
The utility model also provides a method for utilizing low concentration ethylene glycol to produce high concentration dipropylene glycol ester, including following step:
(1) and (3) dehydrating: introducing a low-concentration ethylene glycol raw material into a dehydration tower from a feed inlet I for concentration, and removing most of water; the light component is water, the water is discharged from an exhaust port I and condensed by a condenser I to obtain liquid water, the liquid water enters a reflux tank I, one part of materials in the reflux tank I reflows to a dehydration tower through a reflux port I for cyclic utilization, and the other part of the materials is introduced into a wastewater treatment device; the heavy component discharged from a discharge port I at the bottom of the tower is high-concentration ethylene glycol;
(2) esterification reaction: mixing high-concentration ethylene glycol and acrylic acid discharged from a discharge port I of a dehydration tower, introducing the mixture into a fixed bed reactor through a feed port II, and carrying out esterification reaction on the acrylic acid and the ethylene glycol under the catalytic action of a catalyst A in the fixed bed reactor to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port II and a feed port III and then enters a catalytic distillation tower;
(3) catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and separated; after separation, light components are obtained at the top of the tower, the light components are water and acrylic acid, and the light components are discharged from an exhaust port II and condensed by a condenser II to obtain liquid water and acrylic acid which enter a reflux tank II; one part of the material in the reflux tank II is refluxed to the catalytic distillation tower from the reflux port II for recycling, and the other part of the material is introduced into the acrylic acid recovery device; separating to obtain heavy components at the bottom of the tower, wherein the heavy components are dipropylene glycol ester, partial impurities in the ethylene glycol raw material, and a mixture of trace ethylene glycol and trace acrylic acid, and sequentially flow through a discharge hole III and a feed hole IV and then enter a de-weighting tower;
(4) removing weight: heavy components at the bottom of the catalytic distillation tower enter a heavy component removal tower, are separated in the heavy component removal tower, light components are obtained at the top of the tower, are gaseous dipropylene glycol ester and trace acrylic acid, are discharged from an exhaust port III and are condensed into liquid state by a condenser III, and then enter a reflux tank III, one part of materials in the reflux tank III returns to the heavy component removal tower through a reflux port III for recycling, and the other part of materials are sent into a light component removal tower (5) through a feed port V; the heavy substances discharged from a discharge hole IV at the bottom of the tower are part of impurities in the ethylene glycol raw material and are conveyed to a heavy substance storage tank;
(5) light component removal: the material at the top of the heavy component removal tower enters a light component removal tower, is separated in the light component removal tower, and obtains a light component at the top of the tower, wherein the light component is gaseous acrylic acid, is discharged from an exhaust port IV and then is condensed into liquid by a condenser IV and then enters a reflux tank IV, one part of the material in the reflux tank IV returns to the light component removal tower through a reflux port IV for cyclic utilization, and the other part returns to a device capable of providing acrylic acid for cyclic utilization; the material discharged from the discharge hole V at the bottom of the tower is glycol diacrylate and is conveyed into a glycol diacrylate product storage tank.
In the above technical scheme, in the step (1), the low-concentration ethylene glycol raw material is a waste material containing ethylene glycol generated in the production process of ethylene glycol, wherein the concentration of ethylene glycol is not lower than 20%.
In the above technical solution, in the step (1), the operation conditions of the dehydration tower are as follows: the temperature at the top of the tower is 100-110 ℃, and the pressure is 0.10-0.15 Mpaa; the temperature of the tower bottom is 130-140 ℃, and the pressure is 0.15-0.35 Mpaa.
In the technical scheme, in the step (1), the reflux is carried out at a reflux ratio of 0.5-2.
In the above technical solution, in the step (2), the molar ratio of ethylene glycol to acrylic acid is 1: 2-3, preferably 1: 2.2 to 2.6.
In the technical scheme, in the step (2), the space velocity of the fixed bed reactor is 0.5-2 h-1。
In the above technical solution, in the step (2), the catalyst a is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst, such as a KC-104 type catalyst of the chemerin environmental protection technologies ltd.
In the above technical scheme, in the step (2), the esterification reaction conditions are as follows: the temperature is 60-80 ℃, and the pressure is 0.5-1.0 Mpaa; the temperature is preferably 65 to 70 ℃, and the pressure is preferably 0.6 to 0.7 Mpaa.
In the technical scheme, in the step (3), the space velocity of the primary reaction product formed in the fixed bed reactor entering the catalytic distillation tower is 0.5-3h-1。
In the above technical solution, in the step (3), the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst, and the packing form of the catalyst is preferably a modular catalyst form, such as KC-104BD type modular catalyst of the chemerin environmental protection technologies gmbh.
In the above technical scheme, in the step (3), the catalytic distillation reaction is performed under the following reaction conditions: the reaction temperature is 100-120 ℃, and the reaction pressure is 0.10-0.20 Mpaa.
In the above technical solution, in the step (3), the catalytic distillation column has the following operating conditions: the temperature at the top of the tower is 130-150 ℃, and the pressure is 0.10-0.15 Mpaa; the temperature of the tower bottom is 160-180 ℃, and the pressure is 0.15-0.35 Mpaa.
In the technical scheme, in the step (3), the reflux is carried out at a reflux ratio of 0.5-3.
In the above technical scheme, in the step (4), the operation conditions of the heavy component removal tower are as follows: the temperature at the top of the column is 220-240 ℃, the pressure is 0.10-0.15 Mpaa, the temperature at the bottom of the column is 240-260 ℃, and the pressure is 0.25-0.35 Mpaa.
In the technical scheme, in the step (4), the reflux is carried out at a reflux ratio of 0.3-2.
In the above technical solution, in the step (5), the operation conditions of the light component removal tower are as follows: the temperature at the top of the column is 130-150 ℃, the pressure is 0.10-0.15 Mpaa, the temperature at the bottom of the column is 160-180 ℃, and the pressure is 0.25-0.35 Mpaa.
In the technical scheme, in the step (5), the reflux ratio is 0.5-3.
The utility model discloses technical scheme's advantage lies in:
(1) the utility model discloses a raw materials ethylene glycol can be for the waste material that produces in the ethylene glycol production process, and this waste material is useless for the danger, and this kind of waste material can not produce the benefit, needs to go out to take even and please other company to handle, causes the waste of ethylene glycol, brings economic benefits decline and environmental protection pressure, so the utility model discloses obvious economic benefits and environmental protection advantage have.
(2) The utility model discloses a raw materials ethylene glycol does not have high expectations to the concentration of ethylene glycol, and the ethylene glycol concentration is not less than 20% can.
(3) The utility model discloses a product quality is excellent: the concentration of the dipropylene glycol ester is more than or equal to 99.0 percent, the concentration of the ethylene glycol monoacrylate is less than or equal to 1.0 percent, the concentration of the water is less than or equal to 0.1 percent, and the concentration of the acrylic acid is less than or equal to 0.2 percent.
Drawings
FIG. 1: the utility model discloses the overall structure schematic diagram of the device;
wherein: 1 is a dehydration tower, 2 is a fixed bed reactor, 3 is a catalytic distillation tower, 4 is a heavy component removal tower, and 5 is a light component removal tower.
Detailed Description
The following detailed description of the embodiments of the present invention, but the present invention is not limited to the following description:
the utility model provides an utilize device of low concentration ethylene glycol production high concentration dipropylene glycol ester, including dehydration tower 1, fixed bed reactor 2, catalytic distillation tower 3, heavy tower 4 of taking off that connects gradually, take off light tower 5, as shown in fig. 1:
heavy-duty tower 4, the top is equipped with gas vent III, the bottom is equipped with discharge gate IV, the upper portion that the middle part of tower wall one side was equipped with feed inlet IV, tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet IV is connected with a discharge outlet III of the catalytic distillation tower 3; the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, one path is connected with the reflux port III, and the other path is connected with the lightness-removing tower 5; the discharge port IV is connected with a heavy material storage tank;
the light component removing tower 5 is provided with an exhaust port IV at the top and a discharge port V at the bottom, a feed inlet V is arranged at the middle part of one side of the tower wall, and a reflux port IV is arranged at the upper part of the other side of the tower wall, wherein: the feed inlet V is connected with a reflux tank III; the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, one path is connected with the reflux port IV, and the other path is connected with a device capable of providing acrylic acid; the discharge port V at the bottom is connected with an ethylene glycol diacrylate product storage tank.
In the utility model, the fixed bed reactor 2 is internally filled with a catalyst A; the catalyst A is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst.
In the utility model, the catalytic distillation tower 3 is filled with a catalyst B in the catalytic section; the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cation resin catalyst; the packing form of the catalyst B is preferably a module catalyst form.
The utility model discloses in, dehydration tower, fixed bed reactor, catalytic distillation tower, take off heavy-duty tower, take off light tower and be the equipment or the equipment of selling that prior art exists.
The utility model provides a method for producing high-concentration dipropylene glycol ester by using low-concentration ethylene glycol, which comprises the following steps:
(1) and (3) dehydrating: introducing a low-concentration ethylene glycol raw material into a dehydrating tower 1 from a feed inlet I for concentration, and removing most of water; the light component is water, the water is discharged from an exhaust port I and condensed by a condenser I to obtain liquid water, the liquid water enters a reflux tank I, one part of materials in the reflux tank I reflows to a dehydration tower through a reflux port I for cyclic utilization, and the other part of the materials is introduced into a wastewater treatment device; the heavy component discharged from a discharge port I at the bottom of the tower is high-concentration ethylene glycol;
(2) esterification reaction: mixing high-concentration ethylene glycol and acrylic acid discharged from a discharge port I of a dehydration tower, introducing the mixture into a fixed bed reactor 2 through a feed port II, and carrying out esterification reaction on the acrylic acid and the ethylene glycol under the catalytic action of a catalyst A in the fixed bed reactor to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port II and a feed port III and then enters a catalytic distillation tower 3;
(3) catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and separated; after separation, light components are obtained at the top of the tower, the light components are water and acrylic acid, and the light components are discharged from an exhaust port II and condensed by a condenser II to obtain liquid water and acrylic acid which enter a reflux tank II; one part of the material in the reflux tank II is refluxed to the catalytic distillation tower from the reflux port II for recycling, and the other part of the material is introduced into the acrylic acid recovery device; separating to obtain heavy components at the bottom of the tower, wherein the heavy components are dipropylene glycol ester, partial impurities in the ethylene glycol raw material, and a mixture of trace ethylene glycol and trace acrylic acid, and sequentially flow through a discharge hole III and a feed hole IV and then enter a de-weighting tower;
(4) removing weight: heavy components at the bottom of the catalytic distillation tower enter a heavy component removal tower 4, are separated in the heavy component removal tower, light components are obtained at the top of the tower, are gaseous dipropylene glycol ester and trace acrylic acid, are discharged from an exhaust port III and are condensed into liquid through a condenser III, and then enter a reflux tank III, one part of materials in the reflux tank III returns to the heavy component removal tower through a reflux port III for recycling, and the other part of materials are sent into a light component removal tower 5 through a feed port V; the heavy substances discharged from a discharge hole IV at the bottom of the tower are part of impurities in the ethylene glycol raw material and are conveyed to a heavy substance storage tank;
(5) light component removal: the material at the top of the heavy component removal tower enters a light component removal tower, is separated in the light component removal tower, and obtains a light component at the top of the tower, wherein the light component is gaseous acrylic acid, is discharged from an exhaust port IV and then is condensed into liquid by a condenser IV and then enters a reflux tank IV, one part of the material in the reflux tank IV returns to the light component removal tower through a reflux port IV for cyclic utilization, and the other part returns to a device capable of providing acrylic acid for cyclic utilization; the material discharged from the discharge hole V at the bottom of the tower is glycol diacrylate and is conveyed into a glycol diacrylate product storage tank.
The invention is elucidated below in connection with specific embodiments:
example 1:
a method for producing high-concentration dipropylene glycol ester by using low-concentration ethylene glycol specifically comprises the following steps:
(1) and (3) dehydrating: introducing a low-concentration ethylene glycol raw material into a dehydration tower from a feed inlet I for concentration, and removing most of water; the light component is water, and the water is discharged from an exhaust port I and condensed by a condenser I to obtain liquid water which enters a reflux tank I; one part of the materials in the reflux tank I returns to the dehydration tower 1 through a reflux port I for cyclic utilization, and the other part is connected with a wastewater treatment device; the heavy substances discharged from a discharge port I at the bottom of the tower are high-concentration ethylene glycol.
The ethylene glycol raw material is waste generated in the production process of ethylene glycol, wherein the concentration of the ethylene glycol is 30 percent, the concentration of heavy substances which do not participate in the reaction is 10 percent, and the balance is water;
the top operation conditions of the dehydrating tower are as follows: the temperature is 105-110 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 135-140 ℃, and the pressure is 0.25-0.30 Mpaa;
the reflux ratio of the dehydration tower is 1.5.
(2) Esterification reaction: mixing high-concentration ethylene glycol and acrylic acid (the molar ratio is 1: 2.4) discharged from a discharge port I at the bottom of the dehydration tower, and introducing the mixture into a fixed bed reactor from a feed port II at the airspeed of 0.8h-1Carrying out esterification reaction on acrylic acid and ethylene glycol under the catalysis of a catalyst A in a fixed bed reactor at 65-70 ℃ and 0.7-0.8 Mpa to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port II and a feed port III and enters a catalytic distillation tower;
the catalyst A is a macroporous sulfonic acid cation resin catalyst and adopts a KC-104 type catalyst produced by Kery environmental protection science and technology Limited.
(3) Catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and under the operating conditions of 100-110 ℃ and 0.10-0.15 Mpaa in a reaction section, and is separated; after separation, light components are obtained at the top of the tower, wherein the light components comprise water (about 20% by mass) and acrylic acid (about 80% by mass), are discharged from an exhaust port II and are condensed into liquid through a condenser II to enter a reflux tank II; one part of the materials in the reflux tank II returns to the catalytic distillation tower from the reflux port II for recycling, and the other part of the materials is connected with an acrylic acid recovery device; separating to obtain a final reaction product at the bottom of the tower, wherein the final reaction product is a mixture of dipropylene glycol ester, part of impurities in the raw material glycol, a small amount of acrylic acid and a trace amount of glycol, and sequentially flows through a discharge hole III and a feed hole IV to enter a de-weighting tower 4; in the course of carrying out the catalytic distillation reaction.
The catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC-104BD module catalyst produced by Kary environmental protection science and technology Limited;
the top operation conditions of the catalytic distillation tower are as follows: the temperature is 130-135 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 160-165 ℃, and the pressure is 0.20-0.25 Mpaa;
the reflux ratio of the catalytic distillation tower is 1.
(4) Removing weight: the final-stage reaction product at the bottom of the catalytic distillation tower enters a heavy component removal tower, after separation in the heavy component removal tower, light components are obtained at the top of the tower, the light components are gaseous dipropylene glycol ester and a small amount of acrylic acid, the light components are discharged from an exhaust port III and condensed into liquid through a condenser III to enter a reflux tank III, one part of materials in the reflux tank III returns to the heavy component removal tower through a reflux port III for cyclic utilization, and the other part of materials are sent into the light component removal tower through a feed port V; the heavy substances discharged from the discharge port IV at the bottom of the tower are part of impurities in the raw material glycol, and about 5 percent of glycol diacrylate and glycol.
The tower top operation conditions of the de-heavy tower are as follows: the temperature is 220-225 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 240-245 ℃, and the pressure is 0.25-0.30 Mpaa;
the reflux ratio of the de-heavy tower is 0.6.
(5) Light component removal: the material at the top of the heavy component removal tower enters a light component removal tower, after separation in the light component removal tower, light components are obtained at the top of the light component removal tower, the light components are gaseous acrylic acid and trace dipropylene glycol ester, the light components are discharged from an exhaust port IV and condensed into liquid by a condenser IV to enter a reflux tank IV, one part of the material in the reflux tank IV returns to the light component removal tower through a reflux port IV for recycling, and the other part of the material is connected with an acrylic acid raw material tank; the material discharged from the discharge port V at the bottom of the tower is ethylene glycol diacrylate, and the rest is a small amount of ethylene glycol diacrylate, trace ethylene glycol and acrylic acid, and is sent into a product storage tank through the discharge port V.
The tower top operation conditions of the light component removal tower are as follows: the temperature is 130-135 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 160-165 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the lightness-removing column is 1.5.
In the product of this example, the concentration of dipropylene glycol ester was 99.2%, the concentration of ethylene glycol monoacrylate was 0.55%, the concentration of water was 0.09%, and the concentration of acrylic acid was 0.11%.
Example 2:
a method for producing high-concentration dipropylene glycol ester by using low-concentration ethylene glycol specifically comprises the following steps:
(1) and (3) dehydrating: introducing a low-concentration ethylene glycol raw material into a dehydration tower from a feed inlet I for concentration, and removing most of water; the light component is water, and the water is discharged from an exhaust port I and condensed by a condenser I to obtain liquid water which enters a reflux tank I; one part of the materials in the reflux tank I returns to the dehydration tower through the reflux port I for cyclic utilization, and the other part is connected with a wastewater treatment device; the heavy substances discharged from a discharge port I at the bottom of the tower are high-concentration ethylene glycol.
The ethylene glycol raw material is waste material generated in the production process of ethylene glycol, wherein the concentration of the ethylene glycol is 50%, the concentration of heavy substances which do not participate in the reaction is 10%, and the balance is water.
The top operation conditions of the dehydrating tower are as follows: the temperature is 105-110 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 135-140 ℃, and the pressure is 0.25-0.30 Mpaa;
the reflux ratio of the dehydration tower is 1.3.
(2) Esterification reaction: mixing high-concentration ethylene glycol and acrylic acid (the molar ratio is 1: 2.6) discharged from a discharge port I at the bottom of the dehydration tower, and introducing the mixture into a fixed bed reactor from a feed port II at the airspeed of 0.8h-1Carrying out esterification reaction on acrylic acid and ethylene glycol under the catalysis of a catalyst A in a fixed bed reactor at 65-70 ℃ and 0.7-0.8 Mpa to obtain a primary reaction product; the primary reaction product sequentially flows through a discharge port II and a feed port III and enters a catalytic distillation tower;
the catalyst A is a macroporous sulfonic acid cation resin catalyst and adopts a KC-104 type catalyst produced by Kary environmental protection science and technology Limited.
(3) Catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the catalytic distillation tower and under the operating conditions of 100-110 ℃ and 0.10-0.15 Mpaa in a reaction section, and is separated; after separation, light components are obtained at the top of the tower, wherein the light components comprise water (the mass percent is about 13%) and acrylic acid (the mass percent is about 87%), and are discharged from an exhaust port II and condensed into liquid through a condenser II to enter a reflux tank II; one part of the materials in the reflux tank II returns to the catalytic distillation tower from the reflux port II for recycling, and the other part of the materials is connected with an acrylic acid recovery device; separating to obtain a final reaction product at the bottom of the tower, wherein the final reaction product is a mixture of dipropylene glycol ester, part of impurities in the raw material glycol, a small amount of acrylic acid and a trace amount of glycol, and sequentially flows through a discharge hole III and a feed hole IV to enter a de-weighting tower; in the course of carrying out the catalytic distillation reaction.
The catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC-104BD module catalyst produced by Kary environmental protection science and technology with limited shares;
the top operation conditions of the catalytic distillation tower are as follows: the temperature is 130-135 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 160-165 ℃, and the pressure is 0.20-0.25 Mpaa;
the reflux ratio of the catalytic distillation tower is 1.
(4) Removing weight: the final-stage reaction product at the bottom of the catalytic distillation tower enters a heavy component removal tower, after separation in the heavy component removal tower, light components are obtained at the top of the tower, the light components are gaseous dipropylene glycol ester and a small amount of acrylic acid, the light components are discharged from an exhaust port III and condensed into liquid through a condenser III to enter a reflux tank III, one part of materials in the reflux tank III returns to the heavy component removal tower through a reflux port III for cyclic utilization, and the other part of materials are sent into the light component removal tower through a feed port V; the heavy substances discharged from the discharge port IV at the bottom of the tower are part of impurities in the raw material glycol, and about 5 percent of glycol diacrylate and glycol.
The tower top operation conditions of the de-heavy tower are as follows: the temperature is 220-225 ℃, the pressure is 0.10-0.15 Mpaa, and the operation conditions at the bottom of the tower are as follows: the temperature is 240-245 ℃, and the pressure is 0.25-0.30 Mpaa;
the reflux ratio of the de-heavy tower is 0.6.
(5) Light component removal: the material at the top of the heavy component removal tower enters a light component removal tower, after separation in the light component removal tower, light components are obtained at the top of the light component removal tower, the light components are gaseous acrylic acid and trace dipropylene glycol ester, the light components are discharged from an exhaust port IV and condensed into liquid by a condenser IV to enter a reflux tank IV, one part of the material in the reflux tank IV returns to the light component removal tower through a reflux port IV for recycling, and the other part of the material is connected with an acrylic acid raw material tank; the material discharged from the discharge port V at the bottom of the tower is ethylene glycol diacrylate, and the rest is a small amount of ethylene glycol diacrylate, trace ethylene glycol and acrylic acid, and is sent into a product storage tank through the discharge port V.
The tower top operation conditions of the light component removal tower are as follows: the temperature is 130-135 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 160-165 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the lightness-removing column is 1.5.
In the product of this example, the concentration of dipropylene glycol ester was 99.4%, the concentration of ethylene glycol monoacrylate was 0.49%, the concentration of water was 0.04%, and the concentration of acrylic acid was 0.05%.
The above examples are merely illustrative of the technical concept and technical features of the present invention, and thus the scope of the present invention is not limited thereto. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (7)
1. The utility model provides an utilize device of low concentration ethylene glycol production glycol diacrylate, includes dehydration tower (1), fixed bed reactor (2), catalytic distillation tower (3), heavy tower (4), light tower (5) of taking off that connect gradually, its characterized in that:
dehydration tower (1), the top is equipped with gas vent I, the bottom is equipped with discharge gate I, the well upper portion of tower wall one side is equipped with feed inlet I, the upper portion of tower wall opposite side is equipped with backward flow mouth I, wherein: the feed inlet I is connected with a device capable of providing low-concentration ethylene glycol raw material; the exhaust port I is connected with a condenser I and a reflux tank I, the outlet of the reflux tank I is divided into two paths, one path is connected with the reflux port I, and the other path is connected with a wastewater treatment device; the discharge port I is connected with the fixed bed reactor (2);
fixed bed reactor (2), the top is equipped with feed inlet II, the bottom is equipped with discharge gate II, wherein: the feed inlet II is divided into two paths, one path is connected with the discharge outlet I of the dehydration tower (1), and the other path is connected with a device capable of providing acrylic acid; the discharge port II is connected with the catalytic distillation tower (3);
catalytic distillation tower (3), the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the well upper portion of tower wall one side is equipped with feed inlet III, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet III is connected with the discharge outlet II of the fixed bed reactor (2); the exhaust port II is connected with a condenser II and a reflux tank II, the outlet of the reflux tank II is divided into two paths, one path is connected with the reflux port II, and the other path is connected with an acrylic acid recovery device; the discharge port III is connected with the de-weighting tower (4);
heavy tower (4) takes off, the top is equipped with gas vent III, the bottom is equipped with discharge gate IV, the upper portion that the middle part of tower wall one side was equipped with feed inlet IV, tower wall opposite side is equipped with backward flow mouth III, wherein: the feed inlet IV is connected with a discharge outlet III of the catalytic distillation tower (3); the exhaust port III is connected with a condenser III and a reflux tank III, the outlet of the reflux tank III is divided into two paths, one path is connected with the reflux port III, and the other path is connected with the lightness-removing tower (5); the discharge port IV is connected with a heavy material storage tank;
take off light tower (5), the top is equipped with gas vent IV, the bottom is equipped with discharge gate V, the middle part of tower wall one side is equipped with feed inlet V, the upper portion of tower wall opposite side is equipped with backward flow mouth IV, wherein: the feed inlet V is connected with a reflux tank III; the exhaust port IV is connected with a condenser IV and a reflux tank IV, the outlet of the reflux tank IV is divided into two paths, one path is connected with the reflux port IV, and the other path is connected with a device capable of providing acrylic acid; the discharge port V at the bottom is connected with an ethylene glycol diacrylate product storage tank.
2. The apparatus of claim 1, wherein: the fixed bed reactor (2) is internally filled with a catalyst A.
3. The apparatus of claim 2, wherein: the catalyst A is a solid acid catalyst.
4. The apparatus of claim 3, wherein: the catalyst A is a macroporous sulfonic acid cation resin catalyst.
5. The apparatus of claim 1, wherein: the catalytic distillation tower (3) is filled with a catalyst B in the catalytic section.
6. The apparatus of claim 5, wherein: the catalyst B is a solid acid catalyst.
7. The apparatus of claim 6, wherein: the catalyst B is a macroporous sulfonic acid cation resin catalyst.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021097584.6U CN212560050U (en) | 2020-06-15 | 2020-06-15 | Device for producing glycol diacrylate by using low-concentration ethylene glycol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021097584.6U CN212560050U (en) | 2020-06-15 | 2020-06-15 | Device for producing glycol diacrylate by using low-concentration ethylene glycol |
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