CN211170522U - Device for producing high-concentration ethylene glycol diacetate - Google Patents
Device for producing high-concentration ethylene glycol diacetate Download PDFInfo
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- CN211170522U CN211170522U CN201921538099.5U CN201921538099U CN211170522U CN 211170522 U CN211170522 U CN 211170522U CN 201921538099 U CN201921538099 U CN 201921538099U CN 211170522 U CN211170522 U CN 211170522U
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Abstract
The utility model discloses a device of production high concentration ethylene glycol diacetate, including the pre-heater, fixed bed reactor, monoester catalytic distillation tower, the diester catalytic distillation tower that connect gradually: ethylene glycol and acetic acid react in a fixed bed reactor, and the product enters a monoester catalytic distillation tower; supplementing excessive ethylene glycol into a monoester catalytic distillation tower, carrying out catalytic distillation on materials in the tower, enabling the product to enter a phase separation tank I for phase separation, enabling materials on the upper layer to flow back, enabling materials on the lower layer to be wastewater containing only 0.5% of acetic acid, directly discharging the wastewater into a sewage treatment plant, and enabling the tower bottom product to enter a diester catalytic distillation tower; supplementing excessive acetic acid into the diester catalytic distillation tower, allowing the materials in the tower to undergo catalytic distillation, allowing the product to enter a phase separation tank II for phase separation, allowing the upper layer of materials to flow back, and allowing the lower layer of materials to be a mixture of water, acetic acid and toluene to enter the monoester catalytic distillation tower for cyclic utilization; the ethylene glycol diacetate with high concentration is obtained at the bottom of the diester catalytic distillation tower and is sent out of the device as a product.
Description
Technical Field
The utility model relates to a device of production ethylene glycol diacetate, concretely relates to device of environment-friendly production ethylene glycol diacetate, especially a device of environment-friendly production high concentration ethylene glycol diacetate.
Background
The ethylene glycol diacetate is colorless liquid, has a boiling point of 190.2 ℃, and is an environment-friendly organic solvent which is efficient, safe and nontoxic. The organic ester curing agent is widely used in pharmaceutical industry and casting resin, and also used as a good solvent of various organic resins, particularly nitrocellulose, and a raw material of a leather brightener; the solvent is used as a solvent for nitro spray painting, printing ink, cellulose ester and fluorescent paint in paint coating.
Although the industrial preparation of ethylene glycol diacetate from ethylene glycol and acetic acid by esterification is a general technical route, the currently known industrial devices and patents have the problem of producing waste sulfuric acid or by-product waste water containing more than 5% acetic acid.
The method which is generally adopted in industry is a batch esterification dehydration reaction process by taking sulfuric acid as a catalyst. Sulfuric acid as catalyst has ideal catalytic activity and low cost, but has strong corrosivity and is easy to cause side reactions such as oxidation, carbonization, polymerization, dehydration and the like, products need to be subjected to neutralization treatment, and waste sulfuric acid can cause environmental pollution.
Chinese patents CN 104045554A and CN 109369396A disclose a method for producing ethylene glycol diacetate by using acetic acid and ethylene glycol as raw materials, and the production processes thereof all have the problem of byproduct waste water containing more than 5% of acetic acid, which causes waste of the raw material acetic acid, and the content of the acetic acid in the waste water is high and difficult to treat, thus bringing about economic benefit reduction and environmental protection pressure.
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 of high concentration ethylene glycol diacetate is produced to environment-friendly. The device takes ethylene glycol and acetic acid as raw materials, takes methylbenzene as an entrainer, and the product of the device only contains high-concentration ethylene glycol diacetate and wastewater which can be directly discharged to a sewage treatment plant, so that the device is an environment-friendly technology for producing the high-concentration ethylene glycol diacetate.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
the utility model provides a device of production high concentration ethylene glycol diacetate, includes preheater, fixed bed reactor, monoester catalytic distillation tower, diester catalytic distillation tower that connect gradually:
the preheater be equipped with import and export, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing glycol, and the other path is connected with a device capable of providing acetic acid;
fixed bed reactor, the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
monoester catalytic distillation tower, the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the middle part of tower wall one side is equipped with feed inlet II, well upper portion is equipped with feed inlet III, the middle part of tower wall opposite side is equipped with feed inlet IV, upper portion is equipped with backward flow mouth I, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed inlet III is connected with a device capable of providing glycol; the exhaust port I is connected with a condenser I, and the outlet of the condenser I is connected with a phase separation groove I;
phase separation groove I, be equipped with material inlet I, toluene import I, material leakage fluid dram I and water outlet I, wherein: the material liquid inlet I is connected with an outlet of the condenser I; the toluene inlet I is connected with a device capable of providing toluene; the water outlet I is connected with a sewage treatment system; the material liquid outlet I is divided into two paths, wherein one path is connected with the reflux inlet I of the monoester catalytic distillation tower;
diester catalytic distillation tower, the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet V and feed inlet VI, and feed inlet V's position is higher than the position of feed inlet VI, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet V is connected with a discharge outlet II of the monoester catalytic distillation tower; the feed inlet VI is connected with a device capable of providing acetic acid; the exhaust port II is connected with a condenser II, and the outlet of the condenser II is connected with a phase separation groove II; the discharge port III is connected with a finished product collecting device;
phase separation groove II, be equipped with material inlet II, toluene import II, material leakage fluid dram II and water outlet II, wherein: the material liquid inlet II is connected with an outlet of the condenser II; the toluene inlet II is connected with the other path of the material liquid outlet I of the phase separation groove I; the material liquid outlet II is connected with a reflux outlet II of the diester catalytic distillation tower; the water outlet II is connected with a feed inlet IV of the monoester catalytic distillation tower.
Among the above-mentioned technical scheme, production high concentration ethylene glycol diacetate's device still include heat exchanger I, heat exchanger I is equipped with cold material import A, cold material export A, hot material import A, hot material export A, wherein: the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the hot material outlet A is connected with an inlet of the preheater; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower; the product temperature of the monoester catalytic distillation tower is higher and is equivalent to a hot material, the glycol and the acetic acid are equivalent to a cold material, heat exchange is alternately carried out between cold and hot materials, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is led into the diester catalytic distillation tower through a feed inlet V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product of the glycol and the acetic acid is discharged from a hot material outlet A and is led into a preheater through an inlet.
Among the above-mentioned technical scheme, production high concentration ethylene glycol diacetate's device still include heat exchanger II, heat exchanger II is equipped with cold material import B, cold material export B, hot material import B, hot material export B, wherein: the cold material inlet B is connected with a device capable of providing glycol and acetic acid; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device; the product temperature of the diester catalytic distillation tower is higher and is equivalent to a hot material, the glycol and the acetic acid are equivalent to a cold material, heat exchange is alternately carried out between cold and hot materials, and the temperature of the product of the diester catalytic distillation tower is reduced after heat exchange and is discharged to a finished product collecting device from a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
In the above technical scheme, the device for producing high-concentration ethylene glycol diacetate can simultaneously comprise a heat exchanger I and a heat exchanger II: the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower; the hot material outlet A is connected with the cold material inlet B; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device; the product temperature of the monoester catalytic distillation tower is higher and is equivalent to that of a hot material, the glycol and the acetic acid are equivalent to that of a cold material, cold and hot are alternately subjected to primary heat exchange, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is introduced into the diester catalytic distillation tower from a feed inlet V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product is discharged from a hot material outlet A and is introduced into a heat exchanger II from a cold material inlet B; the product temperature of the diester catalytic distillation tower is higher than that of a hot material, the temperature of the glycol and the acetic acid which are increased after heat exchange is lower than that of a cold material, cold and hot materials are alternately subjected to secondary heat exchange, and the product of the diester catalytic distillation tower is subjected to heat exchange, the temperature is reduced, and the product is discharged to a finished product collecting device through a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
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 catalyst B is filled in the catalytic section of the monoester catalytic distillation tower; the catalyst section of the diester 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.
In the technical scheme, the preheater, the fixed bed reactor, the condenser I and the condenser II, and the phase separation tank I and the phase separation tank II are all equipment existing in the prior art or commercially available equipment; the monoester catalytic distillation tower and the diester catalytic distillation tower are catalytic distillation towers which exist in the prior art or are commercially available and have the function of synthesizing esterified products.
The utility model provides a method for producing high-concentration ethylene glycol diacetate, which comprises the following steps:
(1) esterification reaction: heating raw materials of ethylene glycol and acetic acid by a preheater, introducing the heated raw materials into a fixed bed reactor through a feed inlet I, and carrying out esterification reaction on the acetic 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 I and a feed port II and enters a monoester catalytic distillation tower;
(2) monoester catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a monoester catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the monoester catalytic distillation tower and separated; separating to obtain light components at the top of the tower, wherein the light components are gaseous toluene, water and trace acetic acid, discharging from an exhaust port I, condensing by a condenser I to obtain liquid toluene and water containing the trace acetic acid, allowing the liquid toluene and the water containing the trace acetic acid to enter a phase separation tank I storing the toluene and to be layered in the phase separation tank I, allowing the upper layer to be toluene and the lower layer to be water containing the trace acetic acid, allowing the toluene at the upper layer as an entrainer to return to the monoester catalytic distillation tower from a reflux port I for recycling, introducing the other part to a phase separation tank II, and directly discharging the water containing the trace acetic acid at the lower layer (the content of acetic acid in water is less than 0.5%) into a sewage treatment system for water treatment; after separation, heavy components of the middle-stage reaction product are obtained at the bottom of the tower, the heavy components are a mixture of ethylene glycol monoacetate, ethylene glycol diacetate and ethylene glycol, and the mixture sequentially flows through a discharge hole II and a feed hole V and enters a diester catalytic distillation tower; in the process of carrying out the catalytic distillation reaction, introducing fresh and excessive ethylene glycol from a feed inlet III to prevent acetic acid in the primary product from entering a rectifying section of the monoester catalytic distillation tower;
(3) catalytic distillation of diester: the middle-stage reaction product at the bottom of the monoester catalytic distillation tower enters a diester catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the diester catalytic distillation tower and separated; separating to obtain light components at the tower top, wherein the light components are gaseous methylbenzene, water and acetic acid, and condensing the gaseous methylbenzene, water and acetic acid through a condenser II after being discharged from an exhaust port II to obtain liquid methylbenzene, water and acetic acid; liquid toluene, water and acetic acid are led into a phase separation tank II and layered in the phase separation tank II, the toluene on the upper layer is returned to the diester catalytic distillation tower for recycling from a reflux opening II as an entrainer, and the water and the acetic acid on the lower layer are returned to the monoester catalytic distillation tower for recycling from a feed opening IV; after separation, high-concentration ethylene glycol diacetate is obtained at the bottom of the tower, and flows through a discharge hole III to be sent out of the device to be stored as a product; during the catalytic distillation reaction, fresh, excess acetic acid is introduced at feed VI to ensure complete conversion of ethylene glycol monoacetate to ethylene glycol diacetate in the catalytic distillation section.
In the technical scheme, in the step (1), the molar ratio of the raw materials, namely the glycol and the acetic acid, entering the preheater is 0.15-0.40: 1, preferably 0.20 to 0.30: 1.
in the technical scheme, in the step (1), the raw materials of ethylene glycol and acetic acid are heated to 60-80 ℃ by a preheater and then introduced into a fixed bed reactor, and the space velocity is 0.5-1 h-1。
In the above technical scheme, in the step (1), the esterification reaction conditions are as follows: the temperature is 60-80 ℃, and the pressure is 0.6-1.2 Mpa; the temperature is preferably 65-70 ℃, and the pressure is preferably 0.7-0.9 MPa.
In the above technical scheme, in the step (1), the catalyst a is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst.
In the above technical scheme, in the step (2), the molar ratio of fresh and excess ethylene glycol introduced into the monoester catalytic distillation column to acetic acid introduced into the preheater in the step (1) is 0.20 to 0.45: 1, preferably 0.35 to 0.40: 1.
in the above technical scheme, in the step (2), the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst.
In the technical scheme, in the step (2), the space velocity of the primary reaction product formed in the fixed bed reactor entering the monoester catalytic distillation tower is 1-3 h-1。
In the above technical scheme, in the step (2), the catalytic distillation reaction is performed under the following reaction conditions: the reaction temperature is 100-120 ℃, and the reaction pressure is 0.15-0.20 Mpa.
In the above technical scheme, in the step (2), the operating conditions of the monoester catalytic distillation column are as follows: the temperature at the top of the tower is 85-95 ℃, and the pressure is 0.10-0.15 Mpa; the temperature of the tower bottom is 160-170 ℃, and the pressure is 0.25-0.35 Mpa.
In the above technical solution, in the step (2), the phase separation tank I has the following operating conditions: the temperature is 40-45 deg.C and the pressure is normal pressure.
In the technical scheme, in the step (2), the reflux ratio of the monoester catalytic distillation tower is 0.5-3. In the above technical scheme, in the step (3), the catalyst B is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst.
In the technical scheme, in the step (3), the middle-stage reaction product at the bottom of the monoester catalytic distillation tower enters the diester catalytic distillation tower at an airspeed of 1-3 h-1。
In the above technical scheme, in the step (3), the catalytic distillation reaction is performed under the following reaction conditions: the reaction temperature is 115-125 ℃, and the reaction pressure is 0.15-0.20 Mpa.
In the above technical scheme, in the step (3), the operating conditions of the diester catalytic distillation tower are as follows: the temperature at the top of the tower is 110-120 ℃, the pressure is 0.10-0.15 Mpa, the temperature at the bottom of the tower is 180-190 ℃, and the pressure is 0.25-0.35 Mpa.
In the technical scheme, in the step (3), the reflux ratio of the diester catalytic distillation tower is 0.5-3.
In the above technical solution, in the step (3), the operating conditions of the phase separation tank II are as follows: the temperature is 40-45 deg.C and the pressure is normal pressure.
In the technical scheme, the molar ratio of the sum of the fresh and excessive acetic acid introduced into the diester catalytic distillation tower in the step (3) and the acetic acid introduced into the preheater in the step (1) to the sum of the fresh and excessive ethylene glycol introduced into the monoester catalytic distillation tower in the step (2) and the ethylene glycol introduced into the preheater in the step (1) is 2.0-2.6: 1, preferably 2.35-2.45: 1.
in the technical scheme, the method comprises a heat exchanger I (9), the temperature of the product of the monoester catalytic distillation tower is higher than that of a hot material, and the temperature of the product of the monoester catalytic distillation tower is alternately changed with cold and hot relative to that of a cold material, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is introduced into the diester catalytic distillation tower from a feeding hole V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product is discharged from a hot material outlet A and is introduced into a preheater from an inlet.
In the technical scheme, the method further comprises a heat exchanger II (10), the temperature of the product of the diester catalytic distillation tower is higher than that of a hot material, the cold and hot materials of the glycol and the acetic acid are alternately subjected to heat exchange relative to a cold material, and the temperature of the product of the diester catalytic distillation tower is reduced after the heat exchange, and the product is discharged to a finished product collecting device from a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
In the above technical solution, the method may include both the heat exchanger I (9) and the heat exchanger II (10): the temperature of the product of the monoester catalytic distillation tower is higher than that of a hot material, and the glycol and the acetic acid are opposite to that of a cold material, cold and hot heat exchange is alternately carried out for the first time, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is introduced into the diester catalytic distillation tower from a feed inlet V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product is discharged from a hot material outlet A and is introduced into a heat exchanger II from a cold material inlet B; the product temperature of the diester catalytic distillation tower is higher than that of a hot material, the temperature of the glycol and the acetic acid which are increased after heat exchange is lower than that of a cold material, cold and hot materials are alternately subjected to secondary heat exchange, and the product of the diester catalytic distillation tower is subjected to heat exchange, the temperature is reduced, and the product is discharged to a finished product collecting device through a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
The utility model discloses technical scheme's advantage lies in:
(1) the product of the utility model is only two, one product is high-concentration ethylene glycol diacetate which is a required product; the other product is waste water, the content of acetic acid in the waste water is very low and is less than 0.5 percent, and the acetic acid can be directly discharged into a sewage treatment plant without producing other pollution sources, so the utility model has the obvious advantage of environmental protection.
(2) The utility model discloses a product quality is excellent: the concentration of the ethylene glycol diacetate is more than or equal to 99.5 percent, the concentration of the ethylene glycol monoacetate is less than or equal to 0.2 percent, the concentration of the water is less than or equal to 0.1 percent, and the concentration of the acetic acid is less than or equal to 0.2 percent.
Drawings
FIG. 1 is a schematic view of the overall structure of the device of the present invention;
FIG. 2 is a schematic structural view of the apparatus of the present invention including a heat exchanger I and a heat exchanger II;
wherein: 1 is a preheater, 2 is a fixed bed reactor, 3 is a monoester catalytic distillation tower, 4 is a diester catalytic distillation tower, 5 is a condenser I, 6 is a phase splitting tank I, 7 is a condenser II, 8 is a phase splitting tank II, 9 is a heat exchanger I, and 10 is a heat exchanger II.
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 a production high concentration ethylene glycol diacetate's device, includes preheater 1, fixed bed reactor 2, monoester catalytic distillation tower 3, diester catalytic distillation tower 4 that connect gradually, as shown in figure 1:
preheater 1, be equipped with import and export, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing glycol, and the other path is connected with a device capable of providing acetic acid;
fixed bed reactor 2, the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
monoester catalytic distillation tower 3, the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the middle part of tower wall one side is equipped with feed inlet II, well upper portion is equipped with feed inlet III, the middle part of tower wall opposite side is equipped with feed inlet IV, upper portion is equipped with backward flow mouth I, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed inlet III is connected with a device capable of providing glycol; the exhaust port I is connected with a condenser I5, and the outlet of the condenser I is connected with a phase separation groove I6;
phase separation groove I6, be equipped with material inlet I, toluene import I, material leakage fluid dram I and water outlet I, wherein: the material liquid inlet I is connected with an outlet of the condenser I; the toluene inlet I is connected with a device capable of providing toluene; the water outlet I is connected with a sewage treatment system; the material liquid outlet I is divided into two paths, wherein one path is connected with the reflux inlet I of the monoester catalytic distillation tower;
diester catalytic distillation tower 4, the top is equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet V and feed inlet VI, and feed inlet V's position is higher than the position of feed inlet VI, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet V is connected with a discharge outlet II of the monoester catalytic distillation tower; the feed inlet VI is connected with a device capable of providing acetic acid; the exhaust port II is connected with a condenser II 7, and the outlet of the condenser II is connected with a phase separation groove II 8; the discharge port III is connected with a finished product collecting device;
phase separation groove II 8, be equipped with material inlet II, toluene import II, material leakage fluid dram II and water outlet II, wherein: the material liquid inlet II is connected with an outlet of the condenser II; the toluene inlet II is connected with the other path of the material liquid outlet I of the phase separation groove I; the material liquid outlet II is connected with a reflux outlet II of the diester catalytic distillation tower; the water outlet II is connected with a feed inlet IV of the monoester catalytic distillation tower;
the fixed bed reactor is internally filled with a catalyst A, and the catalyst A is a solid acid catalyst, preferably a macroporous sulfonic acid cationic resin catalyst;
the catalyst section of the monoester catalytic distillation tower is filled with a catalyst B, and the catalyst section of the diester 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 device in the utility model, still include heat exchanger I9, as shown in FIG. 2: heat exchanger I is equipped with cold material import A, cold material export A, hot material import A, hot material export A, wherein: the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the hot material outlet A is connected with an inlet of the preheater; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower; the product temperature of the monoester catalytic distillation tower is higher and is equivalent to a hot material, the glycol and the acetic acid are equivalent to a cold material, heat exchange is alternately carried out between cold and hot materials, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is led into the diester catalytic distillation tower through a feed inlet V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product of the glycol and the acetic acid is discharged from a hot material outlet A and is led into a preheater through an inlet.
The device in the utility model, still include heat exchanger II 10, as shown in fig. 2: heat exchanger II is equipped with cold material import B, cold material export B, hot material import B, hot material export B, wherein: the cold material inlet B is connected with a device capable of providing glycol and acetic acid; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device; the product temperature of the diester catalytic distillation tower is higher and is equivalent to a hot material, the glycol and the acetic acid are equivalent to a cold material, heat exchange is alternately carried out between cold and hot materials, and the temperature of the product of the diester catalytic distillation tower is reduced after heat exchange and is discharged to a finished product collecting device from a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
The device in the utility model can include heat exchanger I9 and heat exchanger II 10 simultaneously, as shown in FIG. 2: the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower; the hot material outlet A is connected with the cold material inlet B; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device; the product temperature of the monoester catalytic distillation tower is higher and is equivalent to that of a hot material, the glycol and the acetic acid are equivalent to that of a cold material, cold and hot are alternately subjected to primary heat exchange, the temperature of the product of the monoester catalytic distillation tower is reduced after heat exchange, the product is discharged from a cold material outlet A and is introduced into the diester catalytic distillation tower from a feed inlet V, and the temperature of the product of the monoester catalytic distillation tower is increased after heat exchange, the product is discharged from a hot material outlet A and is introduced into a heat exchanger II from a cold material inlet B; the product temperature of the diester catalytic distillation tower is higher than that of a hot material, the temperature of the glycol and the acetic acid which are increased after heat exchange is lower than that of a cold material, cold and hot materials are alternately subjected to secondary heat exchange, and the product of the diester catalytic distillation tower is subjected to heat exchange, the temperature is reduced, and the product is discharged to a finished product collecting device through a cold material outlet B; the temperature rise of the glycol and the acetic acid after heat exchange is discharged from a hot material outlet B and is introduced into the preheater through an inlet.
In the utility model, the preheater, the fixed bed reactor, the condenser I and the condenser II, the phase splitting groove I and the phase splitting groove II are all the equipment existing in the prior art or the commercially available equipment; the monoester catalytic distillation tower and the diester catalytic distillation tower are catalytic distillation towers which exist in the prior art or are commercially available and have the function of synthesizing esterified products.
The utility model provides a method for circularly producing high-concentration ethylene glycol diacetate, which comprises the following steps:
(1) esterification reaction: heating raw materials of ethylene glycol and acetic acid by a preheater, introducing the heated raw materials into a fixed bed reactor through a feed inlet I, and carrying out esterification reaction on the acetic 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 I and a feed port II and enters a monoester catalytic distillation tower;
(2) monoester catalytic distillation reaction: the primary reaction product formed in the fixed bed reactor enters a monoester catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the monoester catalytic distillation tower and separated; separating to obtain light components at the top of the tower, wherein the light components are gaseous toluene, water and trace acetic acid, discharging from an exhaust port I, condensing by a condenser I to obtain liquid toluene and water containing the trace acetic acid, allowing the liquid toluene and the water containing the trace acetic acid to enter a phase separation tank I storing the toluene and to be layered in the phase separation tank I, allowing the upper layer to be toluene and the lower layer to be water containing the trace acetic acid, allowing the toluene at the upper layer as an entrainer to return to the monoester catalytic distillation tower from a reflux port I for recycling, introducing the other part to a phase separation tank II, and directly discharging the water containing the trace acetic acid at the lower layer (the content of acetic acid in water is less than 0.5%) into a sewage treatment system for water treatment; after separation, heavy components of the middle-stage reaction product are obtained at the bottom of the tower, the heavy components are a mixture of ethylene glycol monoacetate, ethylene glycol diacetate and ethylene glycol, and the mixture sequentially flows through a discharge hole II and a feed hole V and enters a diester catalytic distillation tower; in the process of carrying out the catalytic distillation reaction, introducing fresh and excessive ethylene glycol from a feed inlet III to prevent acetic acid in the primary product from entering a rectifying section of the monoester catalytic distillation tower;
(3) catalytic distillation of diester: the middle-stage reaction product at the bottom of the monoester catalytic distillation tower enters a diester catalytic distillation tower, and is subjected to catalytic distillation reaction under the catalytic action of a catalyst B in the diester catalytic distillation tower and separated; separating to obtain light components at the tower top, wherein the light components are gaseous methylbenzene, water and acetic acid, and condensing the gaseous methylbenzene, water and acetic acid through a condenser II after being discharged from an exhaust port II to obtain liquid methylbenzene, water and acetic acid; liquid toluene, water and acetic acid are led into a phase separation tank II and layered in the phase separation tank II, the toluene on the upper layer is returned to the diester catalytic distillation tower for recycling from a reflux opening II as an entrainer, and the water and the acetic acid on the lower layer are returned to the monoester catalytic distillation tower for recycling from a feed opening IV; after separation, high-concentration ethylene glycol diacetate is obtained at the bottom of the tower, and flows through a discharge hole III to be sent out of the device to be stored as a product; during the catalytic distillation reaction, fresh, excess acetic acid is introduced at feed VI to ensure complete conversion of ethylene glycol monoacetate to ethylene glycol diacetate in the catalytic distillation section.
The invention is elucidated below in connection with specific embodiments:
example 1:
an environment-friendly method for producing high-concentration ethylene glycol diacetate specifically comprises the following steps:
(1) esterification reaction: ethylene glycol and acetic acid (molar ratio is 0.25: 1) are heated by a preheater to 65-70 ℃, and then are introduced into the fixed bed reactor from a feed inlet I, and the space velocity is 0.8h-1Carrying out esterification reaction on acetic 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 I and a feed port II and enters a monoester catalytic distillation tower;
the catalyst A is a macroporous sulfonic acid cation resin catalyst, and adopts a KC156 type ethylene glycol diacetate catalyst of Kery environmental protection science and technology Limited company.
(2) Catalytic distillation of monoester: reaction product of fixed bed reactor (space velocity of 2 h)-1) After entering a monoester catalytic distillation tower, reacting and separating under the action of a catalyst B in the catalytic distillation tower at 100-110 ℃ and under the condition of 0.15-0.20 Mpa; the materials at the tower top are gaseous entrainer toluene, water and trace acetic acid, the materials are discharged from an exhaust port I and then condensed by a condenser I to obtain liquid toluene and water containing trace acetic acid, the toluene and the water containing trace acetic acid are layered in a phase separation tank I, the toluene at the upper layer is taken as the entrainer and divided into two paths, one path returns to the tower from a reflux port I, the other path flows to a phase separation tank II to supplement the toluene for the phase separation tank II, and the water containing trace acetic acid (the content is less than 0.5%) at the lower layer of the phase separation tank I is sent to a decontamination water treatment plant for treatment; the material at the bottom of the tower is mainly a mixture of ethylene glycol diacetate, ethylene glycol monoacetate and ethylene glycol, and sequentially flows through a discharge port II and a feed port V and enters a diester catalytic distillation tower; ethylene glycol was fed into the monoester catalytic distillation column at feed port III, and the molar ratio of ethylene glycol fed to acetic acid in step (1) was 0.35: 1. Is fed from a feed inlet IVThe lower layer of liquid water in the phase separation tank II, acetic acid and a small amount of toluene.
The catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC156-BD type ethylene glycol diacetate module catalyst of Kerril environmental protection science and technology Limited company;
the top operation conditions of the catalytic distillation column 10 are as follows: the temperature is 85-90 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 165-170 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the monoester catalytic distillation tower is 1.
The phase separation tank I has the following operating conditions: the temperature is 40-45 deg.C and the pressure is normal pressure.
(3) Catalytic distillation of diester: the reaction product at the bottom of the monoester catalytic distillation tower (space velocity of 2 h)-1) After entering a diester catalytic distillation tower through a feed inlet V, reacting and separating under the action of a catalyst B in the catalytic distillation tower at the temperature of 115-120 ℃ and under the pressure of 0.15-0.20 Mpa; the materials at the tower top are gaseous entrainer toluene, acetic acid and water, the gaseous entrainer toluene, acetic acid and water are obtained by condensing through a condenser II after being discharged from an exhaust port II, the toluene, the acetic acid and the water are layered in a phase separation tank II, the toluene serving as the entrainer returns to the tower from a reflux port II at the upper layer, and the water and the acetic acid at the lower layer of the phase separation tank II are sent to a monoester catalytic distillation tower for recycling; the material at the bottom of the tower is high-concentration ethylene glycol diacetate and flows through a discharge hole III to be taken as a product to be discharged out of the device; supplementing acetic acid into the diester catalytic distillation tower from a feed port VI, wherein the molar ratio of the total of the supplemented acetic acid and the acetic acid in the step (1) to the total of ethylene glycol in the step (1) and the step (2) is 2.4: 1;
the catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC156-BD type ethylene glycol diacetate module catalyst of Kerril environmental protection science and technology Limited company;
the top operation conditions of the diester catalytic distillation tower are as follows: the temperature is 110-115 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operating conditions are as follows: the temperature is 180-185 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the diester catalytic distillation tower is 1.
The operating conditions of the phase separation tank II are as follows: the temperature is 40-45 deg.C and the pressure is normal pressure.
In the product of this example, the concentration of ethylene glycol diacetate was 99.6%, the concentration of ethylene glycol monoacetate was 0.16%, the concentration of water was 0.09%, and the concentration of acetic acid was 0.15%.
Example 2:
an environment-friendly method for producing high-concentration ethylene glycol diacetate specifically comprises the following steps:
(1) esterification reaction: ethylene glycol) and acetic acid (molar ratio 0.25: 1) sequentially flows through a heat exchanger I, a heat exchanger I and a preheater, is heated by the preheater to 65-70 ℃, and then is introduced into the fixed bed reactor from a feed inlet I, and the airspeed is 0.8h-1Carrying out esterification reaction on acetic 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 reaction product; the reaction product sequentially flows through a discharge port I and a feed port II and enters a monoester catalytic distillation tower;
the catalyst A is a macroporous sulfonic acid cation resin catalyst, and adopts a KC156 type ethylene glycol diacetate catalyst of Kery environmental protection science and technology Limited company.
(2) Catalytic distillation of monoester: reaction product of fixed bed reactor (space velocity of 2 h)-1) After entering a monoester catalytic distillation tower, reacting and separating under the action of a catalyst B in the catalytic distillation tower at 100-110 ℃ and under the condition of 0.15-0.20 Mpa; the materials at the tower top are gaseous entrainer toluene, water and trace acetic acid, the materials are discharged from an exhaust port I and then condensed by a condenser I to obtain liquid toluene and water containing trace acetic acid, the toluene and the water containing trace acetic acid are layered in a phase separation tank I, the toluene at the upper layer is taken as the entrainer and divided into two paths, one path returns to the tower from a reflux port I, the other path is used for supplementing toluene for a phase separation tank II, and the water containing trace acetic acid (the content of acetic acid is less than 0.5%) at the lower layer of the phase separation tank I is sent to a decontamination water treatment plant; the material at the bottom of the tower is mainly a mixture of ethylene glycol diacetate, ethylene glycol monoacetate and ethylene glycol, and the mixture sequentially flows through a discharge port II, a heat exchanger I and a feed port V and then enters a diester catalytic distillation tower; make up from feed inlet III to monoester catalytic distillation towerEthylene glycol was charged, and the molar ratio of supplemental ethylene glycol to acetic acid in step (1) was 0.35: 1. The lower layer liquid water, acetic acid and a small amount of toluene are fed into the phase separation tank II from a feed inlet IV.
The catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC156-BD type ethylene glycol diacetate module catalyst of Kerril environmental protection science and technology Limited company;
the top operation conditions of the catalytic distillation column 10 are as follows: the temperature is 85-90 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operation conditions are as follows: the temperature is 165-170 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the monoester catalytic distillation tower is 1.
The phase separation tank I has the following operating conditions: the temperature is 40-45 deg.C and the pressure is normal pressure.
(3) Catalytic distillation of diester: the reaction product at the bottom of the monoester catalytic distillation tower (space velocity of 2 h)-1) After entering a diester catalytic distillation tower through a feed inlet V, reacting and separating under the action of a catalyst B in the catalytic distillation tower at the temperature of 115-120 ℃ and under the pressure of 0.15-0.20 Mpa; the materials at the tower top are gaseous entrainer toluene, acetic acid and water, the gaseous entrainer toluene, acetic acid and water are obtained by condensing through a condenser II after being discharged from an exhaust port II, the toluene, the acetic acid and the water are layered in a phase separation tank II, the toluene serving as the entrainer returns to the tower from a reflux port II at the upper layer, and the water and the acetic acid at the lower layer of the phase separation tank II are sent to a monoester catalytic distillation tower for recycling; the material at the bottom of the tower is high-concentration ethylene glycol diacetate and flows through a discharge port III and a heat exchanger II to be taken as a product to be sent out of the device; supplementing acetic acid into the diester catalytic distillation tower from a feed port VI, wherein the molar ratio of the total of the supplemented acetic acid and the acetic acid in the step (1) to the total of ethylene glycol in the step (1) and the step (2) is 2.4: 1;
the catalyst B is a macroporous sulfonic acid cation resin catalyst and adopts a KC156-BD type ethylene glycol diacetate module catalyst of Kerril environmental protection science and technology Limited company;
the top operation conditions of the diester catalytic distillation tower 20 are as follows: the temperature is 110-115 ℃, the pressure is 0.10-0.15 Mpa, and the tower bottom operating conditions are as follows: the temperature is 180-185 ℃, and the pressure is 0.25-0.30 Mpa;
the reflux ratio of the diester catalytic distillation tower is 1.
The operating conditions of the phase separation tank II are as follows: the temperature is 40-45 deg.C and the pressure is normal pressure.
In this example, the concentration of ethylene glycol diacetate was 99.6%, the concentration of ethylene glycol monoacetate was 0.16%, the concentration of water was 0.09%, and the concentration of acetic acid was 0.15%. Because the heat exchange is carried out twice, 5-10% of the total energy consumption can be saved.
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 (6)
1. The utility model provides a device of production high concentration ethylene glycol diacetate, includes preheater (1), fixed bed reactor (2), monoester catalytic distillation tower (3), diester catalytic distillation tower (4) that connect gradually, its characterized in that:
the preheater (1) is provided with an inlet and an outlet, wherein: the inlet is divided into two paths, one path is connected with a device capable of providing glycol, and the other path is connected with a device capable of providing acetic acid;
fixed bed reactor (2), the top is equipped with feed inlet I, the bottom is equipped with discharge gate I, wherein: the feed inlet I is connected with the outlet of the preheater;
monoester catalytic distillation tower (3), the top is equipped with gas vent I, the bottom is equipped with discharge gate II, the middle part of tower wall one side is equipped with feed inlet II, well upper portion is equipped with feed inlet III, the middle part of tower wall opposite side is equipped with feed inlet IV, upper portion is equipped with backward flow mouth I, wherein: the feed inlet II is connected with a discharge outlet I of the fixed bed reactor; the feed inlet III is connected with a device capable of providing glycol; the exhaust port I is connected with a condenser I (5), and the outlet of the condenser I is connected with a phase separation groove I (6);
phase separation groove I (6), be equipped with material inlet I, toluene import I, material leakage fluid dram I and water outlet I, wherein: the material liquid inlet I is connected with an outlet of the condenser I; the toluene inlet I is connected with a device capable of providing toluene; the water outlet I is connected with a sewage treatment system; the material liquid outlet I is divided into two paths, wherein one path is connected with the reflux inlet I of the monoester catalytic distillation tower;
diester catalytic distillation tower (4), the top be equipped with gas vent II, the bottom is equipped with discharge gate III, the middle part of tower wall one side is equipped with feed inlet V and feed inlet VI, and feed inlet V's position is higher than the position of feed inlet VI, the upper portion of tower wall opposite side is equipped with backward flow mouth II, wherein: the feed inlet V is connected with a discharge outlet II of the monoester catalytic distillation tower; the feed inlet VI is connected with a device capable of providing acetic acid; the exhaust port II is connected with a condenser II (7), and the outlet of the condenser II is connected with a phase separation groove II (8); the discharge port III is connected with a finished product collecting device;
phase separation groove II (8), be equipped with material inlet II, toluene import II, material leakage fluid dram II and water outlet II, wherein: the material liquid inlet II is connected with an outlet of the condenser II; the toluene inlet II is connected with the other path of the material liquid outlet I of the phase separation groove I; the material liquid outlet II is connected with a reflux outlet II of the diester catalytic distillation tower; the water outlet II is connected with a feed inlet IV of the monoester catalytic distillation tower.
2. The apparatus for producing ethylene glycol diacetate at high concentration according to claim 1, wherein: the device of production high concentration ethylene glycol diacetate still include heat exchanger I (9), heat exchanger I is equipped with cold material import A, cold material export A, hot material import A, hot material export A, wherein: the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the hot material outlet A is connected with an inlet of the preheater; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower.
3. The apparatus for producing ethylene glycol diacetate at high concentration according to claim 1, wherein: the device of production high concentration ethylene glycol diacetate still include heat exchanger II (10), heat exchanger II is equipped with cold material import B, cold material export B, hot material import B, hot material export B, wherein: the cold material inlet B is connected with a device capable of providing glycol and acetic acid; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device.
4. The apparatus for producing ethylene glycol diacetate at high concentration according to claim 1, wherein: the device for producing the high-concentration ethylene glycol diacetate simultaneously comprises a heat exchanger I (9) and a heat exchanger II (10): the cold material inlet A is connected with a device capable of providing glycol and acetic acid; the hot material inlet A is connected with a discharge hole II of the monoester catalytic distillation tower; the cold material outlet A is connected with a feed inlet V of the diester catalytic distillation tower; the hot material outlet A is connected with the cold material inlet B; the hot material inlet B is connected with a discharge hole III of the diester catalytic distillation tower; the hot material outlet B is connected with an inlet of the preheater; the cold material outlet B is connected with a finished product collecting device.
5. The apparatus for producing ethylene glycol diacetate at high concentration according to claim 1, wherein: the fixed bed reactor is internally filled with a catalyst A; the catalyst A is a solid acid catalyst.
6. The apparatus for producing ethylene glycol diacetate at high concentration according to claim 1, wherein: the catalyst section of the monoester catalytic distillation tower is filled with a catalyst B; the catalyst section of the diester catalytic distillation tower is filled with a catalyst B; the catalyst B is a solid acid catalyst.
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