CN113617117A - Dehydration equipment and process for comprehensively recovering liquid phase membrane from organic solvent - Google Patents
Dehydration equipment and process for comprehensively recovering liquid phase membrane from organic solvent Download PDFInfo
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- CN113617117A CN113617117A CN202110822903.8A CN202110822903A CN113617117A CN 113617117 A CN113617117 A CN 113617117A CN 202110822903 A CN202110822903 A CN 202110822903A CN 113617117 A CN113617117 A CN 113617117A
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- organic solvent
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- 239000012528 membrane Substances 0.000 title claims abstract description 73
- 239000003960 organic solvent Substances 0.000 title claims abstract description 45
- 239000007791 liquid phase Substances 0.000 title claims abstract description 39
- 230000018044 dehydration Effects 0.000 title claims abstract description 36
- 238000006297 dehydration reaction Methods 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 20
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000002994 raw material Substances 0.000 claims abstract description 24
- 239000012530 fluid Substances 0.000 claims abstract description 22
- 230000000149 penetrating effect Effects 0.000 claims abstract description 22
- 238000011084 recovery Methods 0.000 claims abstract description 13
- 239000006096 absorbing agent Substances 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 10
- 239000012071 phase Substances 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims description 55
- 208000005156 Dehydration Diseases 0.000 claims description 31
- 239000007788 liquid Substances 0.000 claims description 18
- 239000012466 permeate Substances 0.000 claims description 12
- 238000002309 gasification Methods 0.000 claims description 10
- 238000000926 separation method Methods 0.000 claims description 8
- 239000002808 molecular sieve Substances 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 5
- 238000005485 electric heating Methods 0.000 claims description 3
- 230000003749 cleanliness Effects 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 38
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000005373 pervaporation Methods 0.000 description 2
- 150000001298 alcohols Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 150000002170 ethers Chemical class 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D36/00—Filter circuits or combinations of filters with other separating devices
- B01D36/003—Filters in combination with devices for the removal of liquids
Abstract
The invention provides a dehydration device and a dehydration process for an organic solvent comprehensive recovery liquid phase membrane, which comprises a feed pump, a precision filter, a preheater, a heater, a membrane assembly, a finished product condenser, a back pressure valve, an activated carbon adsorber, a finished product tank, a penetrating fluid condenser, a penetrating fluid tank, a vacuum unit, a tail gas condenser and a tail gas condensate tank; the feed pump, the precision filter, the preheater, the heater, the membrane module, the finished product condenser, the back pressure valve, the activated carbon absorber and the finished product tank are sequentially connected through pipelines. Compared with a gas phase dehydration mode, the invention adopts a liquid phase dehydration mode, and can save more than 80 percent of heat source for heating the raw material and more than 80 percent of circulating water for cooling the product; the invention is completely operated under the condition of liquid phase, and has higher safety; the pipeline of the invention is provided with the activated carbon absorber, which can improve the purity and cleanliness of the product; the outlet of the vacuum unit is provided with the cooling recovery device, so that the organic matter emission is reduced, and the environment is protected.
Description
Technical Field
The invention belongs to the technical field of pharmaceutical chemical equipment, and particularly relates to a liquid phase membrane dehydration device for comprehensively recovering an organic solvent.
Background
In the existing dehydration and recovery process of the organic solvent of the pervaporation membrane, a large amount of heat sources are needed to gasify the organic solvent and water together to complete dehydration, and then circulating water is used to liquefy and cool the finished product to normal temperature.
Patent document CN201710476235.1 provides a pervaporation membrane organic solvent dehydration device, which gasifies organic solvent raw materials and water together, but a large amount of heat sources are required in the gasification process, the energy consumption is large, and the concentration of organic matters in the tail gas emission also does not meet the requirement of environmental protection.
Disclosure of Invention
The invention aims to provide the dehydration equipment for the comprehensive recovery of the liquid phase membrane of the organic solvent, which can perform dehydration under the liquid phase condition, aiming at the defects of the prior art.
In order to solve the technical problems, the invention adopts the following technical scheme:
a liquid phase membrane dehydration device for comprehensively recovering organic solvent comprises a feed pump, a precision filter, a preheater, a heater, a membrane assembly, a finished product condenser, a back pressure valve, an activated carbon adsorber, a finished product tank, a penetrating fluid condenser, a penetrating fluid tank, a vacuum unit, a tail gas condenser and a tail gas condensate tank; the feed pump, the precision filter, the preheater, the heater, the membrane module, the finished product condenser, the back pressure valve, the activated carbon absorber and the finished product tank are sequentially connected through pipelines; and the permeation side of the membrane component, the penetrating fluid condenser, the penetrating fluid tank, the vacuum unit, the tail gas condenser and the tail gas condensate tank are sequentially connected through pipelines.
The permeation gasification membrane in the membrane module is at least one stage.
The number of the permeable gasification membranes has two or more than two stages, and the single group of the permeable gasification membranes with the number of the two or more than two stages is used in series or the multiple groups are mixed in parallel for use.
The heater may use steam or thermal oil or electric heating as a heat source.
A process for comprehensively recovering liquid-phase membrane dehydration equipment by using an organic solvent comprises the following steps:
the method comprises the following steps: feeding a water-containing 10wt.% organic solvent raw material into a feed pump;
step two: the raw materials enter a preheater from an outlet of a feed pump through a precision filter, and enter the heater after being preheated by a shell pass of the preheater;
step three: the preheated raw materials are heated in a heater and then enter a membrane module for dehydration treatment;
step four: the heated raw material passes through the interception side surface of a molecular sieve membrane in the membrane component, water molecules penetrate through the membrane and enter the permeation side, organic solvent molecules are discharged from an outlet of the interception side of the membrane component, and the water content of the organic solvent can be reduced to be below 200 PPM;
step five: enabling a product containing water to 200PPM discharged from an outlet at the interception side to enter the top end of a preheater, performing heat exchange with a thrown normal-temperature raw material through a tube pass of the preheater, cooling the product to be close to the normal temperature, and then enabling the product to enter a finished product condenser from the bottom end of the preheater;
step six: a back pressure valve and an activated carbon absorber are sequentially arranged between the finished product condenser and the finished product tank, the activated carbon absorber removes and decolours the impurities to obtain an anhydrous organic solvent product, and the anhydrous organic solvent product is stored in the finished product tank.
When gas-phase water molecules on the permeation side of the membrane module pass through the penetrating fluid condenser, the temperature is reduced and the gas-phase water molecules are cooled to a low-temperature liquid phase; and (4) after the cooled penetrating fluid enters a penetrating fluid tank to perform gas-liquid separation, storing and discharging the liquid phase in the penetrating fluid tank.
The vacuum unit pumps out the non-condensable gas and organic molecules in the permeation liquid tank, conveys the non-condensable gas and the organic molecules to a tail gas condenser to be cooled to a normal-temperature liquid state, conveys the non-condensable gas and the organic molecules to a tail gas condensate tank to be subjected to gas-liquid separation, stores and recycles the liquid phase in the tail gas condensate tank, and discharges and treats a small amount of non-condensable gas.
And step five, cooling to normal temperature by circulating water.
Compared with the prior art, the invention has the beneficial effects that:
(1) compared with a gas phase dehydration mode, the invention adopts a liquid phase dehydration mode, and can save more than 80 percent of heat source for heating the raw material and more than 80 percent of circulating water for cooling the product;
(2) the invention is completely operated under the condition of liquid phase, and has higher safety;
(3) the pipeline of the invention is provided with the activated carbon absorber, which can improve the purity and cleanliness of the product;
(4) the outlet of the vacuum unit is provided with the cooling recovery device, so that the organic matter emission is reduced, and the environment is protected;
(5) the equipment structure is simpler after liquid-phase feeding, the safety requirement and the processing difficulty are reduced, so that the processing period of the equipment is shortened, and the manufacturing cost of the equipment is saved.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
Wherein, 1-a feed pump; 2-a precision filter; 3-a preheater; 4-a heater; 5-a membrane module; 6-finished product condenser; 7-back pressure valve; 8-activated carbon adsorber; 9-finished product tank; 10-permeate condenser; 11-a permeate tank; 12-a vacuum unit; 13-tail gas condenser; 14-tail gas condensate tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict.
The present invention is further illustrated by the following examples, which are not to be construed as limiting the invention.
A liquid phase membrane dehydration device for comprehensively recovering organic solvent comprises a feed pump 1, a precision filter 2, a preheater 3, a heater 4, a membrane component 5, a finished product condenser 6, a back pressure valve 7, an active carbon adsorber 8, a finished product tank 9, a penetrating fluid condenser 10, a penetrating fluid tank 11, a vacuum unit 12, a tail gas condenser 13 and a tail gas condensate tank 14; the device comprises a feed pump 1, a precision filter 2, a preheater 3, a heater 4, a membrane component 5, a finished product condenser 6, a back pressure valve 7, an activated carbon adsorber 8 and a finished product tank 9 which are sequentially connected through pipelines; the permeation side of the membrane module 5, a penetrating fluid condenser 10, a penetrating fluid tank 11, a vacuum unit 12, a tail gas condenser 13 and a tail gas condensate tank 14 are sequentially connected through pipelines.
The permeation gasification membrane in the membrane module 5 is at least one stage; when the permeable gasification membrane is in two or more stages, the permeable gasification membrane can be combined and used in a multi-stage single-group series connection mode, and can also be combined and used in a multi-stage series multi-group parallel connection mode.
The heater 4 may use steam or thermal oil or electric heating as a heat source.
A process for comprehensively recovering liquid-phase membrane dehydration equipment by using an organic solvent comprises the following steps:
the method comprises the following steps: feeding an organic solvent raw material containing 10wt.% of water into a feed pump 1;
step two: the raw materials enter a preheater 3 from the outlet of a feed pump 1 through a precision filter 2, and enter a heater 4 after being preheated by the shell pass of the preheater 3;
step three: the preheated raw materials are heated in a heater 4 and then enter a membrane module 5 for dehydration treatment;
step four: the heated raw material passes through the interception side surface of the molecular sieve membrane in the membrane component 5, water molecules penetrate through the membrane and enter the permeation side, organic solvent molecules are discharged from an outlet at the interception side of the membrane component 5, and the water content of the organic solvent can be reduced to be below 200 PPM;
step five: the method comprises the following steps that (1) products containing water and 200PPM discharged from an outlet at the interception side enter the top end of a preheater 3, are subjected to heat exchange with a thrown normal-temperature raw material through a tube pass of the preheater 3, are cooled to be close to normal-temperature products, and then enter a finished product condenser 6 from the bottom end of the preheater 3;
step six: a back pressure valve 7 and an activated carbon absorber 8 are sequentially arranged between the finished product condenser 6 and the finished product tank 9, the activated carbon absorber 8 removes impurities and decolors the finished product to obtain an anhydrous organic solvent product, and the anhydrous organic solvent product is stored in the finished product tank 9.
When gas-phase water molecules on the permeation side of the membrane module 5 pass through the penetrating fluid condenser 10, the temperature is reduced and the gas-phase water molecules are cooled to a low-temperature liquid phase; the cooled permeate enters the permeate tank 11 for gas-liquid separation, and the liquid phase is stored and discharged in the permeate tank 11.
The vacuum unit 12 pumps out the non-condensable gas and organic molecules in the permeate liquid tank 11, conveys the non-condensable gas and the organic molecules to the tail gas condenser 13 to be cooled to a normal-temperature liquid state, conveys the non-condensable gas and the organic molecules to the tail gas condensate tank 14 to be subjected to gas-liquid separation, stores and recycles the liquid phase in the tail gas condensate tank 14, and discharges and processes a small amount of non-condensable gas.
And step five, cooling to normal temperature by circulating water.
When the organic solvent comprehensive recovery liquid phase membrane dehydration equipment is in operation, a feeding pump 1 is used for pumping an organic solvent containing 10wt.% of water into a system, and particle impurities in pipelines or raw materials are removed through a precision filter 2, so that the damage of the particles in the pipelines and the raw materials to a molecular sieve membrane in a membrane component 5 is prevented; and the preheated raw material enters a heater 4 after being preheated by the shell pass of a preheater 3, the preheated raw material is heated to the temperature required by the process and then enters a membrane component 5 for dehydration, the material passes through the interception side surface of a molecular sieve membrane, water molecules enter the permeation side through the membrane, organic solvent molecules are discharged from the interception side outlet of the membrane component 5, and the water content of the organic solvent can be reduced to below 200PPM at the moment.
The product at the process temperature enters a tube side of a preheater 3 to exchange heat with the normal-temperature raw material, and the heat carried by the product is fully recovered; the product cooled to the temperature close to the normal temperature enters a finished product condenser 6, and is cooled to the normal temperature through circulating water; a back pressure valve 7 is arranged at the outlet of the finished product condenser 6, and the back pressure valve 7 is used for maintaining the stable process pressure of the molecular sieve membrane dehydration system; an activated carbon adsorber 8 is arranged on a pipeline between the backpressure valve 7 and the finished product tank 9, so that final impurity removal and decoloration are carried out on the product, and higher purity and cleanliness are achieved; finally, the anhydrous organic solvent product enters a finished product tank 9 for storage and use.
The outlet of the permeation side of the membrane component 5 is connected with a permeation liquid condenser 10, a permeation liquid tank 11 and a vacuum unit 12, the vacuum unit 12 is used for maintaining the vacuum state of the permeation side of the molecular sieve membrane dehydration system, and water molecules permeating from the interception side are pumped out of the membrane dehydration system; the gas phase water molecules on the permeation side are cooled to a low temperature liquid phase when passing through the penetrating fluid condenser 10; the cooled permeate enters the permeate tank 11 for gas-liquid separation, and the liquid phase is stored and discharged in the permeate tank 11.
A small amount of non-condensable gas and organic molecules are discharged through the vacuum unit 12; a tail gas condenser 13 is arranged at the outlet of the vacuum unit 12, and most organic solvent molecules in the tail gas under the normal pressure state are cooled to be in a normal-temperature liquid state; after the cooled tail gas enters the tail gas condensate tank 14 for gas-liquid separation, the liquid phase is stored and recycled in the tail gas condensate tank 14, and a small amount of non-condensable gas is discharged and treated. The tail gas condenser 13 and the tail gas condensate tank 14 arranged at the tail gas outlet of the vacuum unit 12 effectively cool and collect the organic solvent in the vacuum system, improve the comprehensive yield of the product, further reduce the concentration of organic matters in the waste gas and reduce the environmental protection pressure. Compared with the original gas phase dehydration mode, the liquid phase dehydration mode of the invention can save more than 80 percent of heat source for heating the raw material and more than 80 percent of circulating water for cooling the product
The equipment structure is simpler after liquid-phase feeding, the safety requirement and the processing difficulty are reduced, so that the processing period of the equipment is shortened, and the manufacturing cost of the equipment is saved.
The dehydration process of the liquid phase membrane for comprehensively recovering the organic solvent is suitable for various organic solvent systems, such as: alcohols, ethers, ketones, esters, hydrocarbons, acetonitrile, THF, DMF, and the like.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and detail may be made therein without departing from the spirit and scope of the invention.
Claims (8)
1. The utility model provides an organic solvent is synthesized and is retrieved liquid phase membrane dewatering equipment which characterized in that: comprises a feed pump (1), a precision filter (2), a preheater (3), a heater (4), a membrane component (5), a finished product condenser (6), a back pressure valve (7), an activated carbon absorber (8), a finished product tank (9), a penetrating fluid condenser (10), a penetrating fluid tank (11), a vacuum unit (12), a tail gas condenser (13) and a tail gas condensate tank (14); the feed pump (1), the precision filter (2), the preheater (3), the heater (4), the membrane module (5), the finished product condenser (6), the back pressure valve (7), the activated carbon absorber (8) and the finished product tank (9) are sequentially connected through pipelines; the permeate side of the membrane component (5), the permeate condenser (10), the permeate liquid tank (11), the vacuum unit (12), the tail gas condenser (13) and the tail gas condensate tank (14) are sequentially connected through pipelines.
2. The organic solvent comprehensive recovery liquid phase membrane dehydration device according to claim 1, characterized in that: the permeation gasification membrane in the membrane module (5) is at least one stage.
3. The organic solvent comprehensive recovery liquid phase membrane dehydration device according to claim 2, characterized in that: the number of the permeable gasification membranes has two or more than two stages, and the single group of the permeable gasification membranes with the number of the two or more than two stages is used in series or the multiple groups are mixed in parallel for use.
4. The organic solvent comprehensive recovery liquid phase membrane dehydration device according to claim 1, characterized in that: the heater (4) can use steam or heat conduction oil or electric heating as a heat source.
5. A process for the integrated recovery of liquid phase membrane dehydration equipment using an organic solvent according to claim 1, characterized by comprising the steps of:
the method comprises the following steps: feeding a raw material containing 10wt.% of water of an organic solvent into a feed pump (1);
step two: the raw materials enter a preheater (3) from an outlet of a feed pump (1) through a precision filter (2), and enter a heater (4) after being preheated by a shell pass of the preheater (3);
step three: the preheated raw materials are heated in a heater 4 and then enter a membrane module (5) for dehydration treatment;
step four: the heated raw material passes through the interception side surface of the molecular sieve membrane in the membrane component (5), water molecules penetrate through the membrane and enter the permeation side, organic solvent molecules are discharged from an outlet at the interception side of the membrane component (5), and the water content of the organic solvent can be reduced to be below 200 PPM;
step five: enabling a product containing water to 200PPM discharged from an outlet at the interception side to enter the top end of a preheater (3), performing heat exchange with a thrown normal-temperature raw material through a tube side of the preheater (3), cooling to a product close to the normal temperature, and then entering a finished product condenser (6) from the bottom end of the preheater (3);
step six: a back pressure valve (7) and an activated carbon absorber (8) are sequentially arranged between the finished product condenser (6) and the finished product tank (9), the activated carbon absorber (8) removes impurities and decolors the finished product to obtain an anhydrous organic solvent product, and the anhydrous organic solvent product is stored in the finished product tank (9).
6. The integrated recovery liquid-phase membrane dehydration process of organic solvent according to claim 5, characterized in that: when gas-phase water molecules on the permeation side of the membrane module (5) pass through the penetrating fluid condenser (10), the temperature is reduced and the gas-phase water molecules are cooled to a low-temperature liquid phase; the cooled penetrating fluid enters a penetrating fluid tank (11) for gas-liquid separation, and then the liquid phase is stored and discharged in the penetrating fluid tank (11).
7. The integrated recovery liquid-phase membrane dehydration process of organic solvent according to claim 6, characterized in that: the vacuum unit (12) pumps out the non-condensable gas and organic molecules in the permeation liquid tank (11), conveys the non-condensable gas and the organic molecules to a tail gas condenser (13) to be cooled to a normal-temperature liquid state, conveys the non-condensable gas and the organic molecules to a tail gas condensate tank (14) to be subjected to gas-liquid separation, stores and recycles the liquid phase in the tail gas condensate tank (14), and discharges and processes a small amount of non-condensable gas.
8. The integrated recovery liquid-phase membrane dehydration process of organic solvent according to claim 5, characterized in that: and step five, cooling to normal temperature by circulating water.
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Application publication date: 20211109 |