CN212357103U - Tetrahydrofuran-benzene-water mixture separation device - Google Patents
Tetrahydrofuran-benzene-water mixture separation device Download PDFInfo
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- CN212357103U CN212357103U CN201922085411.6U CN201922085411U CN212357103U CN 212357103 U CN212357103 U CN 212357103U CN 201922085411 U CN201922085411 U CN 201922085411U CN 212357103 U CN212357103 U CN 212357103U
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Abstract
The utility model discloses a tetrahydrofuran-benzene-water mixture separator. The method comprises the following steps: the membrane component is provided with a pervaporation membrane and is used for dehydrating the tetrahydrofuran-benzene-water mixture raw material; the preheater, the evaporator and the superheater are connected in sequence; the preheater is connected to a feed pump for feeding the tetrahydrofuran-benzene-water mixture; the superheater is connected with the raw material inlet of the membrane module; the permeation side of the membrane module is connected with a penetrating fluid condenser; the penetrating fluid condenser is connected with the penetrating fluid tank, and the penetrating fluid tank is used for storing penetrating fluid obtained by condensation; the penetrating fluid condenser is provided with a vacuum unit for vacuumizing the penetrating side of the membrane module; the interception side of the membrane component is sequentially connected with a finished product cooler and a dehydration finished product tank; the dehydration finished product tank is connected with the tetrahydrofuran recovery tower, and the top of the tetrahydrofuran recovery tower is connected with the tetrahydrofuran finished product tank through a cooler.
Description
Technical Field
The utility model relates to a device combining permeation gasification membrane dehydration and rectification, in particular to a device for purifying tetrahydrofuran and benzene in a mixture of tetrahydrofuran, benzene and water.
Background
Tetrahydrofuran is an important organic synthetic raw material and is a solvent with excellent performance, is particularly suitable for dissolving PVC, polyvinylidene chloride and butylaniline, is widely used as a solvent for surface coatings, anticorrosive coatings, printing inks, magnetic tapes and film coatings, and is also used as a reaction solvent. Benzene is one of important chemical raw materials, and can be used for preparing dyes, pesticides, plastics, resins, synthetic rubbers, synthetic fibers, synthetic detergents, synthetic medicaments, varnishes and the like.
In the production process of chemical, medicine and pesticide intermediates, tetrahydrofuran and benzene are widely used as solvents, a certain amount of benzene-tetrahydrofuran-water mixed solution is generated in the production process, the mixture of tetrahydrofuran, benzene and water can form 2 binary azeotropes of benzene-water and tetrahydrofuran-water and 1 ternary mixture of tetrahydrofuran-benzene-water, and special rectification is required to be used for separating and obtaining tetrahydrofuran and benzene difficultly. The special rectification process has the problems of complex operation, easy introduction of new impurities and the like. Therefore, it is required to develop a simple separation method.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a method of purification tetrahydrofuran and benzene among tetrahydrofuran, benzene and the water mixture mainly adopts rectification and pervaporation membrane technique, combines traditional handicraft and novel separation technology, adopts pervaporation membrane dehydration technique to replace other dehydration techniques, and the energy consumption is low, is a separation technology of energy-efficient environmental protection with less investment.
A process for the separation of a tetrahydrofuran-benzene-water mixture comprising the steps of:
step 1, removing moisture of a mixture of tetrahydrofuran, benzene and water through a pervaporation dehydration membrane device to obtain a mixture of tetrahydrofuran and benzene;
step 2, enabling the mixture of tetrahydrofuran and benzene obtained in the step 1 to enter a first rectifying tower, obtaining a tetrahydrofuran finished product at the tower top, and obtaining a benzene crude product containing tetrahydrofuran at the tower kettle;
and 3, feeding the benzene crude product containing tetrahydrofuran obtained in the step 2 into a second rectifying tower, obtaining a mixture of tetrahydrofuran and benzene at the tower top, and obtaining a benzene finished product at the tower bottom.
In one embodiment, step 1 is preceded by a superheating of the mixture of tetrahydrofuran, benzene and water to a temperature of 60-85 ℃.
In one embodiment, the temperature of the pervaporation process is 10-20 deg.C superheat, which corresponds to the saturation vapor pressure of the system.
In one embodiment, the pervaporation process employs a molecular sieve membrane, a silica membrane, or a PVA membrane.
In one embodiment, the pressure on the feed side of the pervaporation process is 100-.
In one embodiment, the reflux ratio of the first rectifying tower is 1-5, the operation pressure is 5-300 KPa, and the tower top temperature is 65-90 ℃.
In one embodiment, the reflux ratio of the second rectifying tower is 3-10, the operation pressure is 5-300 KPa, and the tower top temperature is 74-100 ℃.
An apparatus for separating a tetrahydrofuran-benzene-water mixture comprising:
the membrane component is provided with a pervaporation membrane and is used for dehydrating the tetrahydrofuran-benzene-water mixture raw material;
the preheater, the evaporator and the superheater are connected in sequence; the preheater is connected to a feed pump for feeding the tetrahydrofuran-benzene-water mixture; the superheater is connected with the raw material inlet of the membrane module;
the permeation side of the membrane module is connected with a penetrating fluid condenser; the penetrating fluid condenser is connected with the penetrating fluid tank, and the penetrating fluid tank is used for storing penetrating fluid obtained by condensation;
the penetrating fluid condenser is provided with a vacuum unit for vacuumizing the penetrating side of the membrane module;
the interception side of the membrane component is sequentially connected with a finished product cooler and a dehydration finished product tank;
the dehydration finished product tank is connected with the tetrahydrofuran recovery tower, and the top of the tetrahydrofuran recovery tower is connected with the tetrahydrofuran finished product tank through a cooler; the tower bottom of the tetrahydrofuran recovery tower is connected with a tower kettle liquid tank through a cooler;
the tower kettle liquid tank is connected with the benzene recovery tower, and the tower top of the benzene recovery tower is connected with the mixture tank through a cooler; the bottom of the benzene recovery tower is connected with a benzene finished product tank through a cooler.
In one embodiment, the pervaporation membrane is a molecular sieve membrane, a silica membrane or a PVA membrane.
In one embodiment, the membrane module is formed by connecting a plurality of modules in series or in parallel; and when the components are connected in series, a heat compensator is also arranged between the upper and lower two-stage components and used for heating the raw materials.
In one embodiment, a reboiler is further provided at the bottom of the tetrahydrofuran recovery column for heating the residue.
In one embodiment, a condenser is further arranged at the top of the tetrahydrofuran recovery tower or the benzene recovery tower, and is used for condensing steam at the top of the tower and refluxing the steam into the tower.
In one embodiment, the column bottoms tank is connected to the benzene recovery column by a column feed pump.
In one embodiment, the dehydration product tank is connected to the tetrahydrofuran recovery column by a column feed pump.
Advantageous effects
The utility model discloses a multiple azeotropic system in tetrahydrofuran, benzene and the water mixture has been broken to infiltration gasification membrane dehydration technique, can directly adopt conventional rectification method can realize the separation of system, replaces extraction rectification, differential pressure rectification to divide water, and the energy consumption is low, simplifies recovery process.
In the process of the utility model, the purpose of the pervaporation process is to remove water in the ternary mixed system, break the existing various azeotropic compositions and prepare for the subsequent rectification separation; the purpose of the first stage of rectification is to successfully separate tetrahydrofuran as a light component preferentially, and to obtain a benzene crude product containing tetrahydrofuran as a component with higher purity; the second stage of rectification aims at rectifying the bottom liquid of the first stage of rectification tower again, benzene with higher purity can be obtained from the bottom of the tower under the adopted process conditions, the light composition contains benzene and tetrahydrofuran at the same time, and the part of light components can be returned to the previous working procedure for rectification and recycling again.
Drawings
Fig. 1 is a process flow diagram of the present invention. Wherein, 1 is a membrane component, 2 is a preheater, 3 is an evaporator, 4 is a superheater, 5 is a feed pump, 6 is a penetrating fluid condenser, 7 is a penetrating fluid tank, 8 is a vacuum unit, 9 is a finished product cooler, 10 is a dehydration finished product tank, 11 is a tetrahydrofuran recovery tower, 12 is a tetrahydrofuran finished product tank, 13 is a tower kettle fluid tank, 14 is a benzene recovery tower, 15 is a mixture tank, 16 is a benzene finished product tank, 17 is a heat compensator, and 18 is a reboiler.
Detailed Description
As shown in fig. 1, a separation apparatus of a tetrahydrofuran-benzene-water mixture includes: a membrane module 1, in which a pervaporation membrane is installed, for dehydrating a tetrahydrofuran-benzene-water mixture raw material; and a preheater 2, an evaporator 3 and a superheater 4 which are connected in sequence; the preheater 2 is connected to a feed pump 5, the feed pump 5 being used to feed the tetrahydrofuran-benzene-water mixture; the superheater 4 is connected with the raw material inlet of the membrane module 1; the penetrating fluid condenser 6 is connected with the penetrating fluid side of the membrane module 1; the penetrating fluid condenser 6 is connected with a penetrating fluid tank 7, and the penetrating fluid tank 7 is used for storing penetrating fluid obtained by condensation; a vacuum unit 8 is arranged on the penetrating fluid condenser 6 and is used for vacuumizing the penetrating side of the membrane module 1; the interception side of the membrane module 1 is sequentially connected with a finished product cooler 9 and a dehydration finished product tank 10; the dehydration finished product tank 10 is connected with a tetrahydrofuran recovery tower 11, and the top of the tetrahydrofuran recovery tower 11 is connected with a tetrahydrofuran finished product tank 12 through a cooler; the tower bottom of the tetrahydrofuran recovery tower 11 is connected with a tower kettle liquid tank 13 through a cooler; the tower kettle liquid tank 13 is connected with a benzene recovery tower 14, and the top of the benzene recovery tower 14 is connected with a mixture tank 15 through a cooler; the bottom of the benzene recovery column 14 is connected to a finished benzene tank 16 via a cooler. The pervaporation membrane is a molecular sieve membrane, a silica membrane or a PVA membrane. The membrane module 1 is formed by connecting a plurality of modules in series or in parallel; when the modules are connected in series, a heat compensator 17 is provided between the upper and lower modules for heating the raw material. A reboiler 18 is further arranged at the bottom of the tetrahydrofuran recovery tower 11 and is used for heating the kettle liquid. A condenser is further arranged at the top of the tetrahydrofuran recovery tower 11 or the benzene recovery tower 14 for condensing steam at the top of the tower and refluxing the steam to the tower. The tower kettle liquid tank 13 is connected with the benzene recovery tower 14 through a tower feeding pump. The dehydration finished product tank 10 is connected with the tetrahydrofuran recovery tower 11 through a tower feeding pump.
In a typical embodiment, a process for purifying tetrahydrofuran and benzene from a mixture of tetrahydrofuran, benzene, and water comprises the steps of:
(1) removing water from the mixture of tetrahydrofuran, benzene and water by a pervaporation dehydration membrane device to obtain a high-purity mixture of tetrahydrofuran and benzene;
(2) feeding the mixture of tetrahydrofuran and benzene obtained in the step (1) into a tetrahydrofuran recovery tower, obtaining a tetrahydrofuran finished product at the tower top, and obtaining a benzene crude product containing tetrahydrofuran at the tower kettle;
(3) and (3) feeding the crude benzene product obtained in the step (2) into a benzene recovery tower, obtaining a mixture of tetrahydrofuran and benzene at the tower top, and obtaining a finished benzene product at the tower bottom.
In the process, dehydration is carried out by using a pervaporation membrane technology, and then separation of tetrahydrofuran and benzene is carried out by using 2 rectifying towers.
In the process, the pervaporation dehydration membrane device comprises a preheater, an evaporator, a superheater, membrane modules, a penetrating fluid condenser, a vacuum pump, a delivery pump and the like, wherein the membrane modules are connected in series or in parallel according to different processes, the feeding operation pressure is 100-600kPa, and the operation temperature is 10-20 ℃ of superheat corresponding to the saturated vapor pressure of the system.
In the above process, the pervaporation dehydration membrane comprises an inorganic membrane and an organic membrane, mainly a molecular sieve membrane, a silicon dioxide membrane and a PVA membrane.
In the process, the tetrahydrofuran product is obtained at the top of the rectifying tower in the step (2), the reflux ratio is 1-5, the operation pressure is 5-300 KPa, and the temperature at the top of the rectifying tower is 65-90 ℃.
In the above process, the feed to the benzene recovery column in the step (3) is from the bottom liquid of the tetrahydrofuran distillation column in the step (2).
In the process, the benzene finished product is obtained in the tower kettle of the benzene recovery tower in the step (3), the reflux ratio is 3-10, the operation pressure is 5-300 KPa, and the tower top temperature is 74-100 ℃.
In the following examples, the mass ratios of the tetrahydrofuran-benzene-water mixture used were: 79%, 14% and 7%.
Example 1
The adopted process is shown in figure 1, feed liquid enters a preheater through a membrane feed pump, the temperature is up to 75 ℃, the top temperature of an evaporator is 110 ℃, the feed liquid is superheated to 120 ℃ through a superheater, the feed liquid enters a NaA molecular sieve membrane separation unit in the form of superheated steam after reaching a certain temperature, and the membrane separation unit comprises 6 membrane separation units with the thickness of 10m2The membrane modules are connected in series, and the operating pressure is 0.3 MPa. The water and a small amount of organic matters in the raw materials permeate to the downstream side of the membrane from the upstream side of the membrane through the membrane module, the mixture of tetrahydrofuran and benzene with the water content of 0.1wt.% is obtained in the last stage of the upstream side of the membrane, and the mixture is collected in a dehydration finished product tank through a preheater and a finished product cooler. The downstream side of the membrane adopts a vacuum pumping and condensing mode to form the vapor partial pressure difference of components on the upstream side and the downstream side of the membrane. The penetrating fluid steam enters the penetrating fluid condenser under the suction of the vacuum unit, and the condensed penetrating fluid is discharged through the penetrating fluid pump.
The mixture of tetrahydrofuran and benzene in the dehydration finished product tank comprises the following components: benzene: water is about 85.0: 14.9: 0.1, the reaction product enters the middle part of a tetrahydrofuran recovery tower through a tower feeding pump, and the theoretical plate number is 40. The tetrahydrofuran recovery tower is operated continuously at normal pressure, and the reboiler heats and vaporizes the feed liquid. The operation pressure is 1KPa, the top temperature of the rectifying tower is 66 ℃, and the reflux ratio is 2. After the total reflux stabilizing operation, tetrahydrofuran finished product steam with the benzene content less than or equal to 0.2wt.% is extracted from the tower top, and the tetrahydrofuran finished product steam is partially refluxed to the top of the tower after passing through a condenser and a cooler and is partially extracted into a tetrahydrofuran finished product tank. And (3) allowing the benzene crude product containing 15wt.% of tetrahydrofuran at the tower bottom to pass through a cooler and then enter a tower kettle liquid tank.
The crude benzene in the liquid tank of the tower kettle is conveyed to the middle part of the benzene recovery tower by a feeding pump of the benzene recovery tower. The benzene recovery tower is operated continuously at normal pressure, and the reboiler heats and vaporizes the feed liquid. The operation pressure is 2KPa, the tower top temperature of the rectifying tower is 75 ℃, and the reflux ratio is 6. After the total reflux stabilizing operation, tetrahydrofuran/benzene vapor with the benzene content of 50wt.% is extracted from the top of the benzene recovery tower, and after the tetrahydrofuran/benzene vapor is condensed by a benzene recovery condenser and a cooler, part of the tetrahydrofuran/benzene vapor flows back to the top of the benzene recovery tower, and part of the tetrahydrofuran/benzene vapor is extracted into a mixture tank. And a benzene finished product with the benzene content of more than or equal to 99.5 percent is obtained at the bottom of the benzene recovery tower and is cooled and then is sent to a benzene finished product tank.
Example 2
The adopted process is shown in figure 1, the temperature of feed liquid enters a preheater through a membrane feed pump and then reaches 75 ℃, the temperature of the top of an evaporator is 100 ℃, the feed liquid is superheated to 110 ℃ through a superheater and then enters a NaA molecular sieve membrane separation unit in the form of superheated steam after reaching a certain temperature, and the membrane separation unit comprises 4 membrane separation units with the diameter of 10m2The membrane modules are connected in series, and the operating pressure is 0.2 MPa. The water and a small amount of organic matters in the raw materials permeate to the downstream side of the membrane from the upstream side of the membrane through the membrane module, the mixture of tetrahydrofuran and benzene with the water content of 0.15wt.% is obtained in the last stage of the upstream side of the membrane, and the mixture is collected in a dehydration finished product tank through a preheater and a finished product cooler. The downstream side of the membrane adopts a vacuum pumping and condensing mode to form the vapor partial pressure difference of components on the upstream side and the downstream side of the membrane. The penetrating fluid steam enters the penetrating fluid condenser under the suction of the vacuum unit, and the condensed penetrating fluid is discharged through the penetrating fluid pump.
The mixture of tetrahydrofuran and benzene in the dehydration finished product tank comprises the following components: benzene: water was about 84.96: 14.89: 0.15, the reaction product enters the middle part of a tetrahydrofuran recovery tower through a tower feeding pump, and the theoretical plate number is 40. The tetrahydrofuran recovery tower is operated continuously at normal pressure, and the reboiler heats and vaporizes the feed liquid. The operation pressure is 20KPa, the top temperature of the rectifying tower is 70 ℃, and the reflux ratio is 3. After the total reflux stabilizing operation, tetrahydrofuran finished product steam with the benzene content less than or equal to 0.2wt.% is extracted from the tower top, and the tetrahydrofuran finished product steam is partially refluxed to the top of the tower after passing through a condenser and a cooler and is partially extracted into a tetrahydrofuran finished product tank. And (3) allowing the benzene crude product containing 15wt.% of tetrahydrofuran at the tower bottom to pass through a cooler and then enter a tower kettle liquid tank.
The crude benzene in the liquid tank of the tower kettle is conveyed to the middle part of the benzene recovery tower by a feeding pump of the benzene recovery tower. The benzene recovery tower is operated continuously at normal pressure, and the reboiler heats and vaporizes the feed liquid. The operation pressure is 1KPa, the top temperature of the rectifying tower is 70 ℃, and the reflux ratio is 10. After the total reflux stabilizing operation, tetrahydrofuran/benzene vapor with the benzene content of 50wt.% is extracted from the top of the benzene recovery tower, and after the tetrahydrofuran/benzene vapor is condensed by a benzene recovery condenser and a cooler, part of the tetrahydrofuran/benzene vapor flows back to the top of the benzene recovery tower, and part of the tetrahydrofuran/benzene vapor is extracted into a mixture tank. And a benzene finished product with the benzene content of more than or equal to 99.8 percent is obtained at the bottom of the benzene recovery tower and is cooled and then is sent to a benzene finished product tank.
Comparative experiment
If the tetrahydrofuran-benzene-water mixture is directly rectified without pervaporation separation and dehydration as described above, if the rectification process in example 1 is used, the mixture of tetrahydrofuran 77.7%, benzene 15.2%, and water 7.1% can be obtained from the top of the column due to the existence of 2 binary azeotropes of benzene-water, tetrahydrofuran-water, and 1 ternary azeotrope of tetrahydrofuran-benzene-water, and the separation cannot be achieved.
Claims (7)
1. An apparatus for separating a tetrahydrofuran-benzene-water mixture, comprising:
a membrane module (1) in which a pervaporation membrane is installed for dehydrating a tetrahydrofuran-benzene-water mixture raw material;
the preheater (2), the evaporator (3) and the superheater (4) are connected in sequence; the preheater (2) is connected to a feed pump (5), the feed pump (5) being used to feed the tetrahydrofuran-benzene-water mixture; the superheater (4) is connected with a raw material inlet of the membrane module (1);
the permeation side of the membrane module (1) is connected with a penetrating fluid condenser (6); the penetrating fluid condenser (6) is connected with the penetrating fluid tank (7), and the penetrating fluid tank (7) is used for storing penetrating fluid obtained by condensation;
a vacuum unit (8) is arranged on the penetrating fluid condenser (6) and is used for vacuumizing the penetrating side of the membrane module (1);
the interception side of the membrane module (1) is sequentially connected with a finished product cooler (9) and a dehydration finished product tank (10);
the dehydration finished product tank (10) is connected with a tetrahydrofuran recovery tower (11), and the top of the tetrahydrofuran recovery tower (11) is connected with a tetrahydrofuran finished product tank (12) through a cooler; the bottom of the tetrahydrofuran recovery tower (11) is connected with a tower kettle liquid tank (13) through a cooler;
the tower kettle liquid tank (13) is connected to a benzene recovery tower (14), and the top of the benzene recovery tower (14) is connected to a mixture tank (15) through a cooler; the bottom of the benzene recovery column (14) is connected to a benzene product tank (16) through a cooler.
2. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1 wherein the pervaporation membrane is a molecular sieve membrane, a silica membrane or a PVA membrane.
3. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1, wherein the membrane module (1) is formed by connecting a plurality of modules in series or in parallel; when the modules are connected in series, a heat compensator (17) is arranged between the upper and lower modules for heating the raw materials.
4. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1, wherein a reboiler (18) is further provided at the bottom of the tetrahydrofuran recovery column (11) for heat-treating the bottoms.
5. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1, wherein a condenser is further provided at the top of the tetrahydrofuran recovery column (11) or the benzene recovery column (14) for condensing the vapor at the top of the column and refluxing the condensed vapor into the column.
6. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1, wherein the column bottom tank (13) is connected to the benzene recovery column (14) by a column feed pump.
7. The apparatus for separating a tetrahydrofuran-benzene-water mixture according to claim 1 wherein the dehydration product tank (10) is connected to the tetrahydrofuran recovery column (11) by a column feed pump.
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| CN201922085411.6U CN212357103U (en) | 2019-11-28 | 2019-11-28 | Tetrahydrofuran-benzene-water mixture separation device |
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| CN201922085411.6U CN212357103U (en) | 2019-11-28 | 2019-11-28 | Tetrahydrofuran-benzene-water mixture separation device |
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