CN213680472U - Tetrahydrofuran dehydration refining plant - Google Patents
Tetrahydrofuran dehydration refining plant Download PDFInfo
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- CN213680472U CN213680472U CN202021506059.5U CN202021506059U CN213680472U CN 213680472 U CN213680472 U CN 213680472U CN 202021506059 U CN202021506059 U CN 202021506059U CN 213680472 U CN213680472 U CN 213680472U
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Abstract
The invention provides a tetrahydrofuran dehydration refining device, which comprises a membrane separation unit and a rectification unit, wherein: the membrane separation unit comprises a first heat exchange device and a membrane separation assembly; the first heat exchange equipment is provided with a raw material inlet, a raw material outlet, a heat exchange medium inlet and a heat exchange medium outlet; the membrane separation component is provided with a raw material inlet, a retentate outlet and a permeate outlet; a retentate outlet of the membrane separation assembly is connected with a rectification unit; and a material outlet of the rectifying unit is connected with a heat exchange medium inlet of the first heat exchange equipment. The device is used for the isopropanol dehydration process, not only realizes the complete recovery and cyclic utilization of the isopropanol, but also increases the operation flexibility, reduces the energy consumption, and saves the operation cost, the occupied area and the investment cost. The whole device is simple and convenient to operate and stable in operation.
Description
Technical Field
The invention belongs to the field of dehydration and refining processes of mixed organic solvents, and particularly relates to a tetrahydrofuran dehydration and refining device.
Background
Tetrahydrofuran is a heterocyclic organic compound, belongs to ethers, and is a complete hydrogenation product of aromatic compound furan. The liquid is colorless and low-viscosity transparent liquid, has the smell similar to that of diethyl ether, has the characteristics of low toxicity, low boiling point, good fluidity and the like, is an important organic chemical and fine chemical raw material, and is mainly used for producing polytetramethylene ether glycol (PTMEG), polyurethane elastic fibers, elastomers, polyurethane artificial leather and the like. With the rapid increase of domestic demand for polyurethane elastic fibers and elastomers, the demand for tetrahydrofuran will also increase rapidly.
In the mixed solvent system of tetrahydrofuran, one or more solvents form binary azeotropic system or multi-azeotropic system with tetrahydrofuran, so that the purification and refining of the mixed solvent become complicated. The conventional rectification method has high energy consumption and complex process, and a third component is required to be added for an azeotropic system, so that the recovered solvent contains impurities, and the purity and the use quality of the product are influenced.
The membrane separation technology taking the steam permeation dehydration membrane as the core takes the steam partial pressure difference of the removed components as the driving force, shows great advantages in the field of organic solvent dehydration, has simple process route and low energy consumption, does not introduce a third component, and has high product purity. As for a tetrahydrofuran mixed solvent system used in the fine chemical industry, the system is complex and contains certain impurities, an efficient, reliable and energy-saving process needs to be found, and the problems of high energy consumption and low product purity of conventional rectification are solved.
Disclosure of Invention
The invention aims to solve the problems of high energy consumption, low product purity and the like in the purification and refining process of the tetrahydrofuran mixed solvent.
To achieve the object, the present invention firstly provides an apparatus for dehydrating and refining tetrahydrofuran, comprising a membrane separation unit and a rectification unit, wherein: the membrane separation unit comprises a first heat exchange device and a membrane separation assembly; wherein the first heat exchange equipment is provided with a raw material inlet, a raw material outlet, a heat exchange medium inlet and a heat exchange medium outlet; the membrane separation component is provided with a raw material inlet, a retentate outlet and a permeate outlet; a retentate outlet of the membrane separation assembly is connected with a rectification unit; and a material outlet of the rectifying unit is connected with a heat exchange medium inlet of the first heat exchange device.
In another aspect, the present invention provides a method for dehydrating and purifying tetrahydrofuran using the above apparatus for dehydrating and purifying tetrahydrofuran, comprising: conveying the raw materials to heat exchange equipment at a mass flow rate of 2600-3000 kg/h for preheating, and dewatering the raw materials in a membrane separation assembly with an operating pressure of more than 0.2MPa after the raw materials are preheated to 90-130 ℃; continuously separating the dehydrated solvent on the membrane retentate side through a rectification unit to obtain a tetrahydrofuran product; and conveying the finished toluene extracted from the rectification unit to heat exchange equipment to exchange heat with the raw material, and cooling to obtain a toluene product.
The invention adopts the dehydration membrane with selective permeability to preferentially separate the water from the mixed solvent, breaks away the existence of an azeotropic system caused by the existence of the water, simplifies the subsequent separation process of the mixed solvent, and solves the dehydration problem which can not be avoided by the conventional rectification. In addition, the tetrahydrofuran and the toluene are separated in a two-stage rectification energy efficiency coupling mode, the latent heat of the steam of the second separation tower is fully utilized, the energy integration is realized, the energy consumption is reduced, the consumption of the primary steam is reduced, and the number of equipment is reduced. The material extracted from the second separation tower bottom liquid heats the raw material entering the membrane separation, and part of heat energy is recovered.
Drawings
FIG. 1 is a schematic flow diagram of a tetrahydrofuran dehydration purification apparatus of the present invention, wherein:
1. a first heat exchange device; 2. a membrane separation module; 3. a first separation column; 4. a second separation column; 5. a second heat exchange device; 6. a third heat exchange device; 7. a fourth heat exchange device; 8. a fifth heat exchange device; 9. a permeate processing module.
Detailed Description
The following detailed description of the invention refers to the accompanying drawings.
The tetrahydrofuran dehydration refining device comprises a membrane separation unit and a rectification unit. The tetrahydrofuran raw material to be treated enters a membrane separation unit after being preheated, and the membrane separation process is carried out. Water molecules penetrate through the molecular sieve membrane to form a permeate, and the permeate is discharged out of the system through the membrane separation unit. The toluene and tetrahydrofuran with larger molecular size are intercepted by the molecular sieve membrane and enter a rectification unit, and the toluene and tetrahydrofuran products are separated. And in the system design, heat exchange is formed between the product and the raw materials so as to recycle the heat source of the product to realize the heating of the raw materials.
In a specific embodiment, the membrane separation unit comprises a first heat exchange device 1, a membrane separation module 2 and a permeate treatment module 9; the permeate outlet of the membrane separation module 2 is connected with a permeate treatment module 9.
In the specific embodiment, the rectification unit comprises a first separation tower 3, a second heat exchange device 5, a third heat exchange device 6, a second separation tower 4, a fourth heat exchange device 7 and a fifth heat exchange device 8; wherein the first heat exchange device 1 is provided with a raw material inlet, a raw material outlet, a heat exchange medium inlet and a heat exchange medium outlet; the membrane separation component 2 is provided with a raw material inlet, a retentate outlet and a permeate outlet; the retentate outlet of the membrane separation module 2 is connected with a rectification unit; a material outlet of the rectification unit is connected with a heat exchange medium inlet of the first heat exchange device 1; the second heat exchange device 5 is also connected with the first heat exchange device 1; said third heat exchange means 6 is further connected to the overhead vapor outlet of the second separation column 4; said fifth heat exchange device 8 is also connected to the third heat exchange device 6.
In the above tetrahydrofuran dehydration purification apparatus of the present invention:
the first heat exchange device 1 provides a place for heat exchange of the water-containing toluene tetrahydrofuran raw material and the finished toluene, the toluene from the tower bottom of the second separation tower 4 enters the first heat exchange device 1 as a heat exchange medium, heat is exchanged to the mixed raw material of the water-containing toluene tetrahydrofuran and the water-containing tetrahydrofuran steam from the tower top of the first separation tower 3, and the temperature and the pressure of the mixed raw material entering the membrane separation assembly 2 are improved. According to the process requirements, the first heat exchange device 1 can be selected from, but not limited to, a fixed tube-plate type tube-and-tube heat exchanger, a floating head type tube-and-tube heat exchanger, a U-shaped tube-and-tube heat exchanger, a spiral plate type heat exchanger, a spiral tube wound heat exchanger and a plate type heat exchanger.
The membrane separation unit is used for realizing the high-efficiency separation of isopropanol and water. For this purpose, the membrane separation unit is preferably an inorganic molecular sieve membrane separation unit, consisting of n (n is a positive integer) molecular sieve membrane modules 2. The membrane assembly can be a single tube pass or a plurality of tube passes, and the area of the single membrane assembly can be controlled between 5 square meters and 300 square meters. The number n of membrane modules arranged in each set is determined according to the separation purpose; when n is greater than 1, the membrane modules can be connected in series or in parallel according to the material condition, the separation target and the like. On the other hand, from the component structure, the present invention can adopt, but is not limited to, specific forms such as a thermostatic membrane component or a baffle-type membrane component. In the embodiment of the present invention, the molecular sieve membrane module may be specifically exemplified by, but not limited to, a plate-type, tubular-type, hollow fiber-type or spiral plate-type molecular sieve membrane module, preferably a tubular-type molecular sieve membrane module. Suitable types of molecular sieves include LTA, SOD, FAU, MOR, FER, MFI, PHI, BEA, CHA, ERI, and mixed crystal molecular sieve membranes thereof, preferably type A molecular sieve membranes.
The first separation tower 3 is used for realizing the rectification and removal of the tetrahydrofuran azeotropic component, the normal-pressure azeotrope of tetrahydrofuran and water is extracted from the tower top, and the mixed material of toluene and tetrahydrofuran is extracted from the tower bottom. The first separation column 3 may be selected from, but not limited to, a tray column, a packed column.
The second separation tower 4 is used for realizing the rectification separation of tetrahydrofuran and toluene, tetrahydrofuran steam is extracted from the tower top, and toluene materials are extracted from the tower bottom. The second separation column 4 may be selected from, but not limited to, a tray column, a packed column.
The second heat exchange means 5 receives the overhead vapour from the first separation column 3 and condenses it to produce reflux. The second heat exchange device 5 can be selected from, but is not limited to, a fixed tube-plate type tube-and-tube heat exchanger, a floating head type tube-and-tube heat exchanger, a U-shaped tube-and-tube heat exchanger, a spiral plate type heat exchanger, a spiral tube wound heat exchanger, and a plate type heat exchanger.
The third heat exchange device 6 provides a heat exchange place for the toluene-tetrahydrofuran mixture and the tetrahydrofuran vapor, wherein the tetrahydrofuran vapor from the top of the second separation tower 4 enters the third heat exchange device 6 as a heat exchange medium to exchange heat with the toluene-tetrahydrofuran mixture, and the toluene-tetrahydrofuran mixture is heated and then enters the second separation tower 4. According to the process requirement, the third heat exchange device 6 can be selected from, but not limited to, a fixed tube-plate type tube-and-tube heat exchanger, a floating head type tube-and-tube heat exchanger, a U-shaped tube-and-tube heat exchanger, a spiral plate type heat exchanger, a spiral tube wound heat exchanger and a plate type heat exchanger.
The fourth heat exchange device 7 receives the tower bottom material from the second separation tower 4, and the tower bottom material is refluxed by condensation. The fourth heat exchange device 7 can be selected from, but not limited to, a fixed tube-plate type tube-and-tube heat exchanger, a floating head type tube-and-tube heat exchanger, a U-shaped tube-and-tube heat exchanger, a spiral plate type heat exchanger, a spiral tube wound heat exchanger, and a plate type heat exchanger.
Said fifth heat exchange means 8 receives the tetrahydrofuran vapors and condenses them further to obtain the product tetrahydrofuran. The fifth heat exchange device can be selected from, but is not limited to, a fixed tube-plate type tube heat exchanger, a floating head type tube heat exchanger, a U-shaped tube heat exchanger, a spiral plate type heat exchanger, a spiral tube wound heat exchanger and a plate type heat exchanger.
The permeate processing module 9 is used for receiving the permeate from the membrane separation module 2 and further processing the permeate to directly discharge the permeate. The permeate processing component can be selected from but not limited to a vacuum unit and a vacuum unit with steam condensation recovery.
In the structural description of the above-mentioned device, the components that can be determined by those skilled in the art through the prior art in this field are not described, and these components can be exemplified but not limited to: piping for connecting the various devices, a feed tank for storing and/or supplying the tetrahydrofuran feedstock, a product tank for receiving/processing the tetrahydrofuran product, etc. In addition, in combination with the above description, those skilled in the art can determine the most appropriate device selection and type according to the design requirements and requirements under the guidance of the prior art, and it is needless to describe this.
In another aspect, the present invention provides a method for dehydrating and purifying tetrahydrofuran, the method using the apparatus of the present invention, comprising the steps of:
(1) mixing a raw material containing 3-15 wt% of water, 5-20 wt% of toluene and 70-80 wt% of tetrahydrofuran with a material extracted from the top of the first separation tower 3, conveying the mixture to heat exchange equipment at a mass flow rate of 2700-3300 kg/h for preheating, and preheating to 110 +/-2 ℃, wherein a heat source used for preheating is finished toluene from a separation unit; the preheated raw material enters a membrane separation component 2 for dehydration, and the operating pressure is 0.2-0.4 MPa; the permeate is directly discharged after passing through the permeate treatment component 9;
(2) the dehydrated retentate enters a first separation tower 3 for separation, after heat exchange is carried out on steam extracted from the top of the first separation tower 3 through a second heat exchange device 3, part of the steam flows back to the first separation tower 3 to continue to participate in the reaction, and part of the steam is conveyed to a raw material inlet of a first heat exchange device 1 to participate in the reaction; the first separation tower 3 is operated under normal pressure, the temperature of the top of the tower is 60-66 ℃, the temperature of the bottom of the tower is 70-80 ℃, and the reflux ratio of the top of the tower is 1.1 +/-0.2;
(3) materials extracted from the bottom of the first separation tower 3 are conveyed to the second separation tower 4 to be continuously separated, steam extracted from the top of the second separation tower 4 is conveyed to the third heat exchange equipment 6 to provide a heat source, part of the materials after heat exchange returns to the top of the second separation tower 4 to continuously participate in the reaction, and part of the materials pass through the fifth heat exchange equipment 8 to extract finished product tetrahydrofuran; the second separation tower 4 adopts the pressurization operation, the absolute pressure of the operation pressure is 0.2-0.6MPa, the temperature at the top of the tower is 100-;
(4) and materials extracted from the tower bottom of the second separation tower 4 are subjected to heat exchange by the fourth heat exchange equipment 7 and then flow back to the second separation tower 4 to continuously participate in the reaction, and finished toluene is conveyed from the tower bottom to the first heat exchange equipment 1 to provide a heat source and then is condensed and extracted.
The contents and effects of the present invention will be further described with reference to the following examples, but the present invention should not be construed as being limited to the contents in any form. In this example, a tetrahydrofuran dehydration purification apparatus as illustrated in fig. 1 was used in the method, and the selection of each apparatus in the apparatus is as follows:
the first heat exchange device 1 is a fixed tube-plate type tubular heat exchanger.
The membrane separation component 2 is a tubular molecular sieve membrane component; the molecular sieve membrane is an A-type molecular sieve membrane.
The first separation tower 3 is a packed tower.
The second separation tower 4 is a packed tower.
The second heat exchange device 5 is a fixed tube-plate type tubular heat exchanger.
The third heat exchange device 6 is a fixed tube-plate type tubular heat exchanger.
The fourth heat exchange device 7 is a fixed tube-plate type tubular heat exchanger.
And the fifth heat exchange device 8 adopts a fixed tube-plate type tubular heat exchanger.
The permeate treatment component 9 adopts a vacuum unit with steam condensation and recovery.
The method for dehydrating and refining the tetrahydrofuran by using the equipment comprises the following steps:
(1) raw materials from the fine chemical reaction and the refining process comprise 6 wt% of water, 17 wt% of toluene and 77% of tetrahydrofuran, and azeotrope of tetrahydrofuran water extracted from the top of a packed tower 3 is mixed and conveyed to a fixed tube plate type tubular heat exchanger 1 at a mass flow rate of 2980kg/h for preheating, wherein the preheating is carried out to 110 ℃, and a heat source used for preheating is finished product toluene from a separation unit; the preheated raw material enters a tubular molecular sieve membrane component 2 for dehydration, and the operating pressure is 0.3 MPa; the permeate containing less than 1 wt% of mixed solvent is directly discharged after passing through a vacuum unit 9 with steam condensation recovery;
(2) the dehydrated retentate toluene tetrahydrofuran contains 0.5 wt% of water and enters a packed tower 3 for separation, tetrahydrofuran water azeotrope containing 6 wt% of water and 94 wt% of tetrahydrofuran extracted from the top of the packed tower 3 is condensed by a fixed tube plate type tubular heat exchanger 3, then the condensed tetrahydrofuran water azeotrope returns to the packed tower 3 to continuously participate in reaction, and part of the condensed tetrahydrofuran water azeotrope is conveyed to a raw material inlet of the fixed tube plate type tubular heat exchanger 1 to participate in reaction; the packed tower 3 is operated under normal pressure, the temperature of the top of the tower is 63 ℃, the temperature of the bottom of the tower is 75 ℃, and the reflux ratio of the top of the tower is 1.1;
(3) materials extracted from the bottom of the packed tower 3 are conveyed to the packed tower 4 to be continuously separated, steam extracted from the top of the packed tower 4 is conveyed to the fixed tube plate type tubular heat exchanger 6 to provide a heat source, part of the materials after heat exchange returns to the top of the packed tower 4 to continuously participate in the reaction, and part of the materials pass through the fixed tube plate type tubular heat exchanger 8 to extract finished tetrahydrofuran; the packed tower 4 adopts pressurization operation, the absolute pressure of the operation pressure is 0.3MPa, the temperature of the tower top is 105 ℃, the temperature of the tower kettle is 155 ℃, and the reflux ratio of the tower top is 0.5;
(4) materials extracted from the tower bottom of the packed tower 4 are subjected to heat exchange through the fixed tube plate type tubular heat exchanger 7 and then flow back to the packed tower 4 to continue to participate in the reaction, and finished toluene is conveyed from the tower bottom to the fixed tube plate type tubular heat exchanger 1 to provide a heat source and then is extracted through condensation.
According to the method, the fixed tube plate type shell-and-tube heat exchanger 7 at the tower bottom of the packed tower 4 needs to be input for primary steam heat supply, all other heat supply is used for energy recycling, and the amount of steam consumed for treating one ton of water-containing mixed solvent raw material is 1.1-1.2 tons. Compared with the traditional pure rectification process, the energy-saving benefit can reach more than 30-40%.
Claims (7)
1. Tetrahydrofuran dehydration refining plant, its characterized in that includes membrane separation unit and rectification unit, wherein: the membrane separation unit comprises a first heat exchange device (1) and a membrane separation assembly (2);
the first heat exchange device (1) is provided with a raw material inlet, a raw material outlet, a heat exchange medium inlet and a heat exchange medium outlet; the membrane separation component (2) is provided with a raw material inlet, a retentate outlet and a permeate outlet;
the retentate outlet of the membrane separation module (2) is connected with a rectification unit; and a material outlet of the rectifying unit is connected with a heat exchange medium inlet of the first heat exchange device (1).
2. The tetrahydrofuran dehydration refining apparatus according to claim 1, characterized in that said permeate outlet of said membrane separation module (2) is connected to a permeate treatment module (9).
3. The apparatus according to claim 1, wherein the rectification unit comprises a primary rectification module and a secondary rectification module.
4. The tetrahydrofuran dehydration refining plant according to claim 3, characterized in that said primary rectification module comprises a first separation column (3), a second heat exchange device (5) and a third heat exchange device (6), and said secondary rectification module comprises a second separation column (4), a fourth heat exchange device (7) and a fifth heat exchange device (8).
5. The apparatus for dehydrating and refining tetrahydrofuran according to claim 4, wherein said second heat exchange means (5) is further connected to said first heat exchange means (1), and said third heat exchange means (6) is further connected to an overhead vapor outlet of said second separation column (4).
6. The apparatus for dehydrating and refining tetrahydrofuran according to claim 4, wherein said fifth heat exchange means (8) is further connected to a third heat exchange means (6).
7. The apparatus for dehydrating and purifying tetrahydrofuran according to claim 1, wherein: the device comprises a membrane separation unit and a rectification unit, wherein the membrane separation unit comprises a first heat exchange device (1), a membrane separation assembly (2) and a permeate treatment assembly (9); the rectification unit comprises a first separation tower (3), a second heat exchange device (5), a third heat exchange device (6), a second separation tower (4), a fourth heat exchange device (7) and a fifth heat exchange device (8);
wherein the first heat exchange device (1) is provided with a raw material inlet, a raw material outlet, a heat exchange medium inlet and a heat exchange medium outlet; the membrane separation component (2) is provided with a raw material inlet, a retentate outlet and a permeate outlet;
the retentate outlet of the membrane separation module (2) is connected with a rectification unit; a material outlet of the rectification unit is connected with a heat exchange medium inlet of the first heat exchange device (1); the second heat exchange device (5) is also connected with the first heat exchange device (1); the third heat exchange device (6) is also connected with the top steam outlet of the second separation tower (4); the fifth heat exchange device (8) is also connected with the third heat exchange device (6).
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115677625A (en) * | 2022-11-03 | 2023-02-03 | 杰特(宁夏)科技有限公司 | Novel process for producing tetrahydrofuran by using BDO byproduct waste liquid |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115677625A (en) * | 2022-11-03 | 2023-02-03 | 杰特(宁夏)科技有限公司 | Novel process for producing tetrahydrofuran by using BDO byproduct waste liquid |
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