CN216259552U - Membrane adsorption coupling device for preparing tetrahydrofuran with low water content - Google Patents
Membrane adsorption coupling device for preparing tetrahydrofuran with low water content Download PDFInfo
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- CN216259552U CN216259552U CN202122416989.2U CN202122416989U CN216259552U CN 216259552 U CN216259552 U CN 216259552U CN 202122416989 U CN202122416989 U CN 202122416989U CN 216259552 U CN216259552 U CN 216259552U
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Abstract
The utility model relates to a membrane adsorption coupling device for preparing tetrahydrofuran with low water content. The method comprises the following steps: the preheater is used for heating the tetrahydrofuran mother liquor containing water; the evaporation tank is connected with the preheater and is used for carrying out evaporation treatment on the material obtained in the preheater so as to separate light and heavy components; the membrane component is connected to the top of the evaporation tank and is used for carrying out membrane separation and dehydration on the light component obtained by evaporation treatment; the adsorption tank is connected to the concentration side of the membrane component and is used for deeply dehydrating the dehydrated tetrahydrofuran; the adsorption tank is characterized in that a screen mesh pipe is arranged inside the adsorption tank, the filled adsorbent is arranged outside the screen mesh pipe, and an inner pipeline of the screen mesh pipe is connected with a feed inlet of the adsorption tank. The device has the advantages of low moisture content of finished products, high yield, low investment cost and high production efficiency, and is in line with green economy.
Description
Technical Field
The utility model relates to a membrane adsorption coupling device for preparing low-water-content tetrahydrofuran, in particular to a device for preparing the low-water-content tetrahydrofuran by combining a pervaporation method and adsorption, belonging to the application field of pervaporation membranes.
Background
Tetrahydrofuran is an important organic chemical raw material, and can be used as a solvent in pharmaceutical production, synthesis of polymer materials, manufacture of precision magnetic tapes and electroplating industry. In addition, tetrahydrofuran solution is a reaction solvent for synthesizing medicines (such as chlorhexidines and progesterone). In some synthesis reactions (e.g., grignard reactions, alkylation reactions), the trace amount of water in the solvent can severely affect the yield and purity of the final product. These reactions place high demands on the water content of tetrahydrofuran, and some require even less than 30ppm, so that it is necessary to prepare tetrahydrofuran with a low water content.
At present, the industrial process for preparing tetrahydrofuran with low water content mainly adopts pressure swing rectification, for example, patent CN111170968B introduces that crude tetrahydrofuran is passed through a normal pressure-pressurization two-tower system, and dehydration and drying are fully realized by utilizing the azeotropic composition difference under different pressures. The preparation method has high energy consumption and greater safety risk. If the membrane is treated to be below 30ppm by a membrane dehydration technology, the area of the required membrane is increased by times, the investment cost is quite high, the production efficiency is low, the energy consumption is large, and the market acceptance is low.
SUMMERY OF THE UTILITY MODEL
The utility model aims to provide a membrane adsorption coupling device for preparing tetrahydrofuran with low water content. The utility model discloses a have characteristics easy and simple to handle, equipment area is few, and factor of safety is high, and investment cost is low, and production efficiency is high, and the energy consumption is low, and product moisture is low.
The technical scheme is as follows:
a membrane adsorption coupling device for preparing tetrahydrofuran with low water content comprises:
the preheater is used for heating the tetrahydrofuran mother liquor containing water;
the evaporation tank is connected with the preheater and is used for carrying out evaporation treatment on the material obtained in the preheater so as to separate light and heavy components;
the membrane component is connected to the top of the evaporation tank and is used for carrying out membrane separation and dehydration on the light component obtained by evaporation treatment;
the adsorption tank is connected to the concentration side of the membrane component and is used for deeply dehydrating the dehydrated tetrahydrofuran;
the adsorption tank is characterized in that a screen mesh pipe is arranged inside the adsorption tank, the filled adsorbent is arranged outside the screen mesh pipe, and an inner pipeline of the screen mesh pipe is connected with a feed inlet of the adsorption tank.
One side of the adsorption tank close to the feed inlet is also provided with a feed distributor, and one end of the screen pipe is connected to the feed distributor.
The number of the screen pipes is more than two.
The adsorption tank is also provided with a discharge port, one side of the interior of the adsorption tank, which is close to the discharge port, is also provided with a discharge concentrator, and the other end of the screen pipe is connected to the discharge concentrator after being sealed by a plugging sheet; the discharging concentrator is also provided with a porous sheet, and the adsorbent is communicated with the discharging port through the porous sheet and the discharging concentrator.
The membrane module is provided with a preferential permeable membrane.
The preferential water permeable membrane is selected from a PVA membrane, an amorphous silica membrane or a molecular sieve membrane.
Further comprising: and the top of the evaporation tank is connected with the inlet of the membrane module through a superheater and is used for heating the material.
Further comprising: and the penetrating fluid condenser is connected to the penetrating side of the membrane module and is used for condensing the penetrating fluid.
Further comprising: and the vacuum unit is connected to the permeation side of the membrane module and is used for applying negative pressure to the permeation side.
Advantageous effects
1. Compared with the traditional preparation process, the method is not limited by the azeotropy of the feed liquid in the dehydration process, does not need to introduce other components, and is efficient, energy-saving and environment-friendly;
2. the feed liquid after adsorption directly exchanges heat with the mother liquid, so that the energy utilization rate of the system is improved, and the heating load of the purification tower is further reduced;
3. the utility model returns the penetrating fluid to the evaporating pot for recycling, thereby reducing the loss of tetrahydrofuran and improving the recovery rate of finished products;
4. the method has the advantages of high automation degree, relatively low investment cost, high production efficiency, and high purity of the obtained tetrahydrofuran finished product, and the water content is less than or equal to 30 ppm.
5. The adsorption process of the utility model effectively distributes the gas at the membrane separation concentrated side into porous materials which are contacted with the adsorbent, thus improving the contact area and increasing the dehydration efficiency.
Drawings
FIG. 1 is a diagram of a membrane adsorption coupling apparatus for the preparation of tetrahydrofuran having a low water content;
FIG. 2 is a structural view of an adsorption tank;
FIG. 3 is an enlarged view of a part of the structure of the discharge port of the canister.
Wherein 1, a preheater; 2. an evaporator tank; 3. a superheater; 4. a membrane module; 5. a permeate condenser; 6. a vacuum unit; 7. an adsorption tank; 8. a feed inlet; 9. a discharge port; 10. a feed distributor; 11. a discharge concentrator; 12. a screen pipe; 13. a plugging sheet; 14. a porous sheet.
Detailed Description
The structure of the coupling device adopted by the utility model is shown in figure 1, and the main structure comprises: a preheater 1 for raising the temperature of a water-containing tetrahydrofuran material in anticipation thereof; the preheater 1 is connected with an evaporation tank 2, the evaporation tank 2 is used for carrying out primary material evaporation separation (for example, when the byproduct mother liquor of the coal-to-ethylene glycol is recovered and purified, the material also contains other high boiling point substances), so that low boiling point substances (such as tetrahydrofuran and water) are distilled out as light components, the evaporation tank 2 is connected with a superheater 3, and the superheater 3 carries out overheating treatment on the light component material obtained from the evaporation tank 2; a permeable molecular sieve membrane is arranged in the membrane component 4 and is connected with the superheater 3, the high-temperature water-containing and tetrahydrofuran material obtained from the superheater 3 enters the permeable molecular sieve membrane for filtration and separation, a penetrating fluid condenser 5 is connected to the permeation side of the membrane component 4 and is used for condensing the water obtained by permeation, and a vacuum unit 6 is connected to the permeation side to make the permeation side have negative pressure; on the retentate side of the membrane module 4, dehydrated tetrahydrofuran is obtained, and the retentate side is further connected to an adsorption tank 7, and the adsorption tank 7 is filled with an adsorbent (e.g., a molecular sieve adsorbent) for removing a trace amount of water in the obtained tetrahydrofuran.
Wherein, the structure in the adsorption tank 7 includes: a feed inlet 8 and a discharge outlet 9, which are respectively located at two ends of the adsorption tank 7 and are used for feeding the dehydrated tetrahydrofuran obtained in the membrane module 4, a feed distributor 10 is arranged in the adsorption tank 7 at a position close to the feed inlet 8 and is used for redistributing the feed into a plurality of strands of materials, the feed distributor 10 is further connected with a plurality of screen pipes 12, the screen pipes 12 penetrate into the adsorption tank 7, one ends of the screen pipes 12 in the pipes are communicated with the feed inlet 8 through the feed distributor 10, a space formed outside the screen pipes 12 is used for filling an adsorbent, and the screen pipes 12 are of a screen structure and are used for preventing the adsorbent from entering the inside of the screen pipes 12; at the other end of the screen pipe 12 is a plugging sheet 13 for preventing the feed gas from directly flowing out from the end of the screen pipe 12; in addition, a discharge concentrator 11 is further provided inside the adsorption tank 7 on the side facing the discharge port 9, the other end of the screen pipe 12 is fixed to the discharge concentrator 11, and a porous sheet 14 having a porous structure on the surface and used for preventing the adsorbent from seeping out is further provided on the discharge concentrator 11, and the porous sheet 14 is connected to the discharge port 9 through the discharge concentrator 11. In the operation process, tetrahydrofuran concentrated gas firstly enters from the feed inlet 8, and can be divided into a plurality of strands of materials to enter the screen pipe 12 after being redistributed by the feed distributor 10, and the feed gas can be rapidly dispersed and then contacted with the adsorbent because the adsorbent filled outside the screen pipe 12, so that the contact area and the adsorption rate are improved; since the bottom of the screen pipe 12 is blocked by the blocking piece 13, the concentrated tetrahydrofuran cannot be directly removed from the screen pipe 12, but all the concentrated tetrahydrofuran must finally enter into contact with the adsorbent, since the bottom of the discharging concentrator 11 is also provided with the porous piece 14, the porous piece 14 ensures that the adsorbent cannot pass through and the tetrahydrofuran adsorbed with water can pass through, and finally, the plurality of strands of tetrahydrofuran gas are concentrated by the discharging concentrator 11 and discharged from the discharging port 9.
The method for preparing the tetrahydrofuran with low water content comprises the following specific steps: firstly, purging the whole device by using inert gas to isolate the outside air; heating and vaporizing the water-containing tetrahydrofuran, wherein the water content of the tetrahydrofuran before entering the membrane can be controlled to be 1-20%; heating tetrahydrofuran steam to 95-115 ℃ through a superheater before membrane feeding, wherein the water content of the tetrahydrofuran steam after membrane primary dehydration is 0.05-0.1 wt.%; after membrane dehydration, tetrahydrofuran directly enters an adsorption tank without condensation to carry out secondary dehydration, and a dehydrated finished product and mother liquor are condensed after heat exchange to obtain a final product. Wherein the gauge pressure of the feed liquid side of the membrane module is 0-0.3 MPa; the permeation side is connected with a vacuum system, and the absolute pressure of the permeation side is 150-2000 Pa; the pervaporation membrane is made of a preferential water permeable membrane, such as a NaA molecular sieve membrane, a PVA membrane and a hollow fiber membrane; the penetrating fluid of the pervaporation membrane returns to the evaporation tank in the step 1 after being condensed. The temperature range of the adsorption tank is 80-100 ℃, and the pressure is 0-0.3 MPa. The temperature range of the evaporation tank is 105-120 ℃, the operation pressure is 0-0.3MPa, and the feeding temperature is 60-80 ℃.
Example 1
By using the membrane adsorption coupling device for preparing tetrahydrofuran with low water content as shown in figure 1, the following steps are adopted: firstly, purging the device by using high-purity nitrogen to isolate the outside air; then the water-containing tetrahydrofuran mother liquor is heated to 65 ℃ by a preheater 1 and then enters an evaporation tank 2 for heating and vaporization; heating the vaporized tetrahydrofuran feed liquid to 107 ℃ through a superheater 3, and then feeding the tetrahydrofuran feed liquid into a membrane module 4 for primary dehydration; threshing deviceAfter the water content reaches 0.078%, the tetrahydrofuran steam directly enters the adsorption tank 7 for secondary adsorption and dehydration, and finally a tetrahydrofuran finished product containing 27ppm of water is obtained. Wherein the temperature of the evaporation tank is kept at 114 ℃ and the operation pressure is 0.18 MPa. The membrane module 4 adopts a NaA molecular sieve membrane, the operating pressure of the feed liquid side of the membrane module is 0.2MPa gauge pressure, the absolute pressure of the permeation side is 798Pa under the suction of the vacuum unit 6, and the removed permeation liquid is condensed by the permeation liquid condenser 5 and then returns to the evaporation tank 2 for recovery. The permeate vapor was passed through a permeate condenser to obtain a permeate having a water content of about 96.7 wt.%, and the pervaporation membrane operated at an average flux of 1.31kg/m2H. The adsorption tank 7 adopts a granular 4A molecular sieve, the operation temperature is 88 ℃, and the pressure is 0.14 MPa.
Example 2
By using the membrane adsorption coupling device for preparing tetrahydrofuran with low water content as shown in figure 1, the following steps are adopted: firstly, purging the device by using high-purity nitrogen to isolate the outside air; then the water-containing tetrahydrofuran mother liquor is heated to 62 ℃ by a preheater 1 and then enters an evaporation tank 2 for heating and vaporization; heating the vaporized tetrahydrofuran feed liquid to 107 ℃ through a superheater 3, and then feeding the tetrahydrofuran feed liquid into a membrane module 4 for primary dehydration; after the dehydration is carried out to 0.066%, the tetrahydrofuran steam directly enters an adsorption tank 7 for secondary adsorption dehydration, and finally a tetrahydrofuran finished product containing 24ppm of water is obtained. Wherein the temperature of the evaporation tank is kept at 107 ℃ and the operating pressure is 0.13 MPa. The membrane module 4 adopts a NaA molecular sieve membrane, the operating pressure of the feed liquid side of the membrane module is 0.17MPa gauge pressure, the absolute pressure of the permeation side is 909Pa under the suction of the vacuum unit 6, and the removed permeation liquid is condensed by the permeation liquid condenser 5 and then returns to the evaporation tank 2 for recovery. The permeate vapor was passed through a permeate condenser to obtain a permeate having a water content of about 98.2 wt.%, with the pervaporation membrane operating at an average flux of 1.25kg/m2H. The adsorption tank 7 is made of activated alumina, the operation temperature is 92 ℃, and the pressure is 0.15 MPa.
Example 3
By using the membrane adsorption coupling device for preparing tetrahydrofuran with low water content as shown in figure 1, the following steps are adopted: firstly, purging the device by using high-purity nitrogen to isolate the outside air; then the water-containing tetrahydrofuran mother liquor is heated to 68 ℃ by a preheater 1 and then enters an evaporation tank 2 for heating and vaporization; after vaporizationThe tetrahydrofuran feed liquid is heated to 107 ℃ by a superheater 3 and then enters a membrane module 4 for primary dehydration; after the dehydration is carried out to 0.053%, the tetrahydrofuran steam directly enters an adsorption tank 7 for secondary adsorption dehydration, and finally a tetrahydrofuran finished product containing 21ppm of water is obtained. Wherein the temperature of the evaporation tank is kept at 119 ℃, and the operating pressure is 0.19 MPa. The membrane module 4 adopts a NaA molecular sieve membrane, the operating pressure of the feed liquid side of the membrane module is 0.24MPa gauge pressure, the absolute pressure of the permeation side is 798Pa under the suction of the vacuum unit 6, and the removed permeation liquid is condensed by the permeation liquid condenser 5 and then returns to the evaporation tank 2 for recovery. The permeate vapor was passed through a permeate condenser to obtain a permeate having a water content of about 94.3 wt.%, and the pervaporation membrane operated at an average flux of 1.55kg/m2H. The adsorption tank 7 adopts a granular 4A molecular sieve, the operation temperature is 95 ℃, and the pressure is 0.17 MPa.
Claims (9)
1. A membrane adsorption coupling device for preparing tetrahydrofuran with low water content is characterized by comprising:
the preheater (1) is used for heating the tetrahydrofuran mother liquor containing water;
the evaporation tank (2) is connected with the preheater (1) and is used for carrying out evaporation treatment on the material obtained in the preheater (1) so as to separate light and heavy components;
the membrane component (4) is connected to the top of the evaporation tank (2) and is used for carrying out membrane separation and dehydration on the light component obtained by evaporation treatment;
the adsorption tank (7) is connected to the concentration side of the membrane module (4) and is used for deeply dehydrating the dehydrated tetrahydrofuran;
the adsorption tank is characterized in that a screen mesh pipe (12) is arranged inside the adsorption tank (7), the outside of the screen mesh pipe (12) is filled with an adsorbent, and an internal pipeline of the screen mesh pipe (12) is connected with a feed port (8) of the adsorption tank (7).
2. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 1, wherein a feed distributor (10) is further disposed on one side of the adsorption tank (7) close to the feed inlet (8), and one end of the screen pipe (12) is connected to the feed distributor (10).
3. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 2, wherein the number of the screen pipes (12) is more than two.
4. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 3, wherein the adsorption tank (7) is further provided with a discharge port (9), one side of the interior of the adsorption tank (7) close to the discharge port (9) is further provided with a discharge concentrator (11), and the other end of the screen pipe (12) is connected to the discharge concentrator (11) after being sealed by a plugging sheet (13); the discharging concentrator (11) is also provided with a porous sheet (14), and the adsorbent is communicated with the discharging port (9) through the porous sheet (14) and the discharging concentrator (11).
5. The membrane adsorptive coupling device for preparing tetrahydrofuran with low water content according to claim 1, wherein said membrane module (4) is installed with a membrane with preferential water permeability.
6. The membrane adsorptive coupling device for preparing low water content tetrahydrofuran according to claim 5, wherein said preferentially water permeable membrane is selected from the group consisting of a PVA membrane, an amorphous silica membrane and a molecular sieve membrane.
7. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 1, further comprising: the top of the evaporation tank (2) is connected with the inlet of the membrane module (4) through the superheater (3) and is used for heating materials.
8. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 1, further comprising: and the penetrating fluid condenser (5) is connected to the penetrating side of the membrane module (4) and is used for condensing the penetrating fluid.
9. The membrane adsorption coupling device for preparing tetrahydrofuran with low water content according to claim 1, further comprising: and the vacuum unit (6) is connected to the permeation side of the membrane module (4) and is used for applying negative pressure to the permeation side.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117658260A (en) * | 2023-12-04 | 2024-03-08 | 重庆中润新材料股份有限公司 | Tetrahydrofuran waste liquid recovery system and method |
| CN118084273A (en) * | 2024-04-23 | 2024-05-28 | 河南氢力能源有限公司 | Integrated sewage treatment equipment and method for 2-methyl furan production |
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2021
- 2021-10-08 CN CN202122416989.2U patent/CN216259552U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117658260A (en) * | 2023-12-04 | 2024-03-08 | 重庆中润新材料股份有限公司 | Tetrahydrofuran waste liquid recovery system and method |
| CN118084273A (en) * | 2024-04-23 | 2024-05-28 | 河南氢力能源有限公司 | Integrated sewage treatment equipment and method for 2-methyl furan production |
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