Liquid phase permeable membrane filtration system

Through a multi-layer structure liquid-phase permeable membrane filtration system, the combination of reverse osmosis membrane and nanofiltration membrane is used to solve the problem of incomplete filtration of existing systems, and efficiently remove impurities and microorganisms in solvents, improving product purity and Operational efficiency.

CN222173668UActive Publication Date: 2024-12-17NINGXIA ZHONGHUI CHEM CO LTD
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Patent Information

Application Number
CN202420848880.7
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2024-04-23
Publication Date
2024-12-17
Estimated Expiration
2034-04-23

AI Technical Summary

Technical Problem

The existing liquid-phase permeability membrane filtration system has a single penetration equipment and is not thorough in filtration, which makes the solvent contain a large amount of impurities, which cannot meet the requirements of the USP standard for Class 1, Class 2 and Class 3 residual solvents.

Method used

A liquid-phase permeability membrane filtration system including primary and secondary reverse osmosis hosts and nanofiltration chambers was designed. Using a multi-layer structure of reverse osmosis membrane and nanofiltration membrane, trace amounts of moisture and specific II were removed through the primary reverse osmosis host. Solvents, secondary reverse osmosis host removes formic acid and ether plasma, and nanofiltration membrane removes divalent, trivalent ions and other impurities to improve product purity.

Benefits of technology

The class II residual solvent in the headspace solvent is achieved with a water content of ≤5ppm, a water content of ≤0.03wt%, and a color of ≤10, removing divalent, trivalent ions, Mn≥200 organic matter, microorganisms, colloids, heat sources, viruses, etc. Significantly improves product purity and reduces operating costs and waste generation.

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Abstract

The utility model relates to a chemical industry production technology, and discloses a liquid phase osmosis membrane filtration system, which comprises a raw material tank, a primary reverse osmosis main machine, a secondary reverse osmosis main machine and a nanofiltration box, reverse osmosis membranes are uniformly distributed in the primary reverse osmosis main machine and the secondary reverse osmosis main machine respectively, and nanofiltration membranes with membrane pore diameters of 1-2nm are uniformly distributed in the nanofiltration box; a feeding pipe is mounted on the raw material tank, the raw material tank is connected with the primary reverse osmosis main machine through a first liquid inlet pipe, a first booster pump and a precision filter are arranged on the first liquid inlet pipe, the primary reverse osmosis main machine is connected with an intermediate tank, the intermediate tank is connected with the secondary reverse osmosis main machine through a second liquid inlet pipe, and a second booster pump is arranged on the second liquid inlet pipe; the first-stage reverse osmosis host is connected with a first booster pump, the second-stage reverse osmosis host is connected with a crude product tank, the crude product tank is connected with a nanofiltration box through a third liquid inlet pipe, a third booster pump is arranged on the third liquid inlet pipe, the nanofiltration box is connected with a product tank, and pressure sensors are arranged in inner cavities of the first-stage reverse osmosis host, the second-stage reverse osmosis host and the nanofiltration box.
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Description

Technical Field

[0001] The utility model relates to the technical field of chemical production, and more specifically, particularly to a liquid phase permeation membrane filtering system. Background Art

[0002] Headspace chromatography technology is used in environmental testing, detection of organic residual solvents in drugs, analysis of food, packaging materials, coatings and brewing industry, etc. Commonly used headspace solvents are N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), and N-methylpyrrolidone (NMP). The traditional purification process (acid, alkali, distillation, etc.) cannot meet the PPM level required by the USP standard for Class 1, Class 2, and Class 3 residual solvents in the headspace solvent. The pretreated solvent is dehydrated and small molecular impurities are removed by liquid permeation membrane filtration technology, trace water and specific Class II solvents are removed, and product purity is improved. The effects of the pore size, porosity, membrane thickness, and type of polymer membrane on the filtration speed are studied; the effects of temperature, flow rate, pressure, pH value, etc. on impurity removal efficiency and product purity are investigated to determine the best filtration effect.

[0003] Membrane filtration technology refers to membrane separation technology driven by pressure. It is an advanced means of deep water treatment. Under a certain pressure, when the raw liquid flows through the membrane surface, the many tiny micropores densely distributed on the membrane surface only allow water and small molecules to pass through and become permeate, while the substances in the raw liquid with a volume larger than the micropore diameter of the membrane surface are retained on the liquid inlet side of the membrane and become concentrated liquid, thereby achieving the purpose of separation and concentration of the raw liquid; the existing liquid phase osmosis membrane filtration system has a single osmotic equipment and incomplete filtration, which makes the solvent contain a large amount of impurities. Utility Model Content

[0004] The present application provides a liquid phase osmosis membrane filtration system, which solves the problem that the existing liquid phase osmosis membrane filtration system has a single osmosis device, incomplete filtration, and causes the solvent to contain a large amount of impurities.

[0005] The present application provides a liquid phase osmosis membrane filtration system, including a raw material tank, a reverse osmosis host and a nanofiltration box;

[0006] The reverse osmosis host comprises a primary reverse osmosis host and a secondary reverse osmosis host, wherein the primary reverse osmosis host and the secondary reverse osmosis host are respectively evenly covered with reverse osmosis membranes;

[0007] The nanofiltration box is evenly covered with nanofiltration membranes, and the pore size of the nanofiltration membranes is 1-2 nm;

[0008] A feed pipe is installed on the raw material tank, and the raw material tank is connected to the first-level reverse osmosis main unit through a first liquid inlet pipe, and a first booster pump and a precision filter are arranged on the first liquid inlet pipe. The liquid outlet of the first-level reverse osmosis main unit is connected to an intermediate tank through a pipeline, and the intermediate tank is connected to the second-level reverse osmosis main unit through a second liquid inlet pipe, and a second booster pump is arranged on the second liquid inlet pipe. The liquid outlet of the second-level reverse osmosis main unit is connected to a crude product tank through a pipeline, and the crude product tank is connected to the nanofiltration box through a third liquid inlet pipe, and a third booster pump is arranged on the third liquid inlet pipe. The liquid outlet of the nanofiltration box is connected to a product tank, and pressure sensors are arranged in the inner cavities of the first-level reverse osmosis main unit, the second-level reverse osmosis main unit and the nanofiltration box.

[0009] Preferably, flow meters are installed on the first liquid inlet pipe, the second liquid inlet pipe and the third liquid inlet pipe.

[0010] Preferably, a pH value detector is provided on the nanofiltration box.

[0011] Preferably, temperature sensors are provided in the inner cavities of the primary reverse osmosis main unit, the secondary reverse osmosis main unit and the nanofiltration box.

[0012] Preferably, the primary reverse osmosis main unit, the secondary reverse osmosis main unit and the nanofiltration box are all equipped with waste pipes, and the waste pipes are connected to waste treatment equipment.

[0013] Preferably, the nanofiltration membrane is made of cellulose acetate membrane (CA), polyethersulfone membrane (PES) or polytetrafluoroethylene membrane (PTFE).

[0014] It can be seen from the above technical scheme that the present application provides a liquid phase osmosis membrane filtration system. When in use, the headspace solvent ((N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)) is fed into the raw material tank from the feed pipe, and then the first booster pump on the first liquid inlet pipe pumps the headspace solvent in the raw material tank into the first-stage reverse osmosis main unit. Before entering the first-stage reverse osmosis main unit, the mechanical impurities are first filtered through the precision filter installed on the first liquid inlet pipe. The headspace solvent entering the first-stage reverse osmosis main unit overcomes the natural osmotic pressure and the resistance of the reverse osmosis membrane under the pressure of the first booster pump to allow the solution to pass through The reverse osmosis membrane is evenly distributed. The solution passing through the reverse osmosis membrane enters the intermediate tank from the liquid outlet of the first-stage reverse osmosis host. The second booster pump pumps the solution in the intermediate tank into the second-stage reverse osmosis host for further filtration. The pore size of the reverse osmosis membrane can remove formic acid, ether, acetone and other ions in the headspace solvent. The solution passing through the second-stage reverse osmosis host flows out from the liquid outlet into the crude product tank. The third booster pump pumps the solution in the crude product tank into the nanofiltration box. The pore size of the nanofiltration membrane is 1-2nm, which can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc. in the solution, thereby improving the purity of the product. The solution passing through the nanofiltration box enters the product tank through a pipeline.

[0015] Compared with the prior art, the beneficial effects of the utility model are:

[0016] 1. The utility model utilizes liquid osmosis membrane filtration technology to dehydrate the pretreated solvent, remove small molecular impurities, remove trace water and specific Class II solvents, and the nanofiltration membrane can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc., to improve product purity.

[0017] 2. The utility model removes formic acid, ether, acetone and other ions in the headspace solvent (N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)) by the pore size of the reverse osmosis membrane, so as to achieve the headspace solvent Class II residual solvent ≤5ppm, and has both decolorization and water removal effects, so that the chromaticity (Pt-Co) ≤10 and the water content ≤0.03wt%.

[0018] 3. The utility model does not generate any waste, has a long working life and low operating costs.

[0019] In summary, the pore size of the reverse osmosis membrane in a liquid osmosis membrane filtration system removes formic acid, ether, acetone and other ions in the headspace solvent ((N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)), and achieves a headspace solvent Class II residual solvent ≤5ppm, and has both decolorization and water removal effects, making the chromaticity (Pt-Co) ≤10 and the water content ≤0.03wt%. The nanofiltration membrane can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc., to improve product purity. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] In order to more clearly illustrate the technical solution of the present invention, the following briefly introduces the drawings required for use in the embodiments. Obviously, for ordinary technicians in this field, other drawings can be obtained based on these drawings without inventiveness.

[0021] Figure 1 A schematic diagram of a liquid phase permeation membrane filtration system provided by the utility model;

[0022] Figure 2 This is a schematic diagram of a nanofiltration box in a liquid phase permeation membrane filtration system provided by the utility model.

[0023] The reference numerals in the specific implementation manner are as follows:

[0024] 1. Raw material tank; 2. Feed pipe; 3. Precision filter; 4. First-stage reverse osmosis main unit; 5. First liquid inlet pipe; 6. Intermediate tank; 7. Second-stage reverse osmosis main unit; 8. Second liquid inlet pipe; 9. Crude product tank; 10. First booster pump; 11. Second booster pump; 12. Third booster pump; 13. Nanofiltration box; 14. Nanofiltration membrane; 15. Third liquid inlet pipe; 16. Product tank; 17. Temperature sensor; 18. Flow meter; 19. Pressure sensor; 20. PH value detector; 21. Waste pipe; 22. Waste treatment equipment. DETAILED DESCRIPTION

[0025] In order to enable those skilled in the art to better understand the technical solutions in the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings.

[0026] See also Figure 1-2, a liquid phase osmosis membrane filtration system. In order to solve the problem that the existing liquid phase osmosis membrane filtration system has a single osmosis device and incomplete filtration, resulting in a large amount of impurities in the solvent, the application proposes a reverse osmosis membrane pore size in the liquid phase osmosis membrane filtration system to remove formic acid, ether, acetone and other ions in the headspace solvent ((N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)), to achieve the headspace solvent Class II residual solvent ≤5ppm, and has both decolorization and water removal effects, so that the chromaticity (Pt-Co) ≤10 and the water content ≤0.03wt%. The nanofiltration membrane can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc., to improve product purity.

[0027] Specifically, a liquid phase osmosis membrane filtration system includes a raw material tank 1, a reverse osmosis host and a nanofiltration box 13; the reverse osmosis host includes a first-level reverse osmosis host 4 and a second-level reverse osmosis host 7, the pretreated solvent is dehydrated, small molecular impurities are removed, trace water and specific Class II solvents are removed, the first-level reverse osmosis host 4 and the second-level reverse osmosis host 7 are evenly covered with reverse osmosis membranes, and the formic acid, ether, acetone and other ions in the headspace solvent ((N, N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N, N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)) are removed through the pore size of the reverse osmosis membrane, so that the headspace solvent Class II residual solvent is ≤5ppm, and it has both decolorization and water removal effects; the nanofiltration box 13 is evenly covered with nanofiltration membranes 14, and the nanofiltration membranes 14 are cellulose acetate filter membranes (CA), polyethersulfone filter membranes The nanofiltration membrane 14 is made of PES or PTFE, and the pore size of the nanofiltration membrane 14 is 1-2nm. The nanofiltration membrane can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc., to improve the purity of the product. A temperature sensor 17 is provided in the inner cavity of the first-stage reverse osmosis host 4, the second-stage reverse osmosis host 7 and the nanofiltration box 13 to control the temperature in the first-stage reverse osmosis host 4, the second-stage reverse osmosis host 7 and the nanofiltration box 13 at 30-50°C. A pressure sensor 19 is provided in the inner cavity of the first-stage reverse osmosis host 4, the second-stage reverse osmosis host 7 and the nanofiltration box 13 to control the pressure in the first-stage reverse osmosis host 4, the second-stage reverse osmosis host 7 and the nanofiltration box 13 at 1-40bar (100-4000kpa). During the operation, the pressure drop range is controlled at 1-5bar (100-500kpa).

[0028] A feed pipe 2 is installed on the raw material tank 1, and the raw material tank 1 is connected to the primary reverse osmosis main unit 4 through a first liquid inlet pipe 5. The first liquid inlet pipe 5 is provided with a first booster pump 10 and a precision filter 3. The liquid outlet of the primary reverse osmosis main unit 4 is connected to an intermediate tank 6 through a pipeline, and the headspace solvent ((N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)) is fed into the raw material tank 1 from the feed pipe 2, and then the first booster pump 10 on the first liquid inlet pipe 5 pumps the headspace solvent in the raw material tank 1 into the primary reverse osmosis main unit 4. Before entering the primary reverse osmosis main unit 4, mechanical impurities are first filtered through the precision filter 3 installed on the first liquid inlet pipe 5. The headspace solvent entering the primary reverse osmosis main unit 4 overcomes the natural osmotic pressure and the resistance of the reverse osmosis membrane under the pressure of the first booster pump 10, so that the solution passes through the evenly distributed reverse osmosis membrane, and the solution passing through the reverse osmosis membrane is discharged from the primary reverse osmosis main unit 4. The liquid outlet enters the intermediate tank 6; the intermediate tank 6 is connected to the secondary reverse osmosis host 7 through a second liquid inlet pipe 8, and the second liquid inlet pipe 8 is provided with a second booster pump 11. The liquid outlet of the secondary reverse osmosis host 7 is connected to the crude product tank 9 through a pipeline. The second booster pump 11 pumps the solution in the intermediate tank 6 into the secondary reverse osmosis host 7 for further filtration. The pore size of the reverse osmosis membrane can remove formic acid, ether, acetone and other ions in the headspace solvent. The solution of the secondary reverse osmosis host 7 flows out from the liquid outlet and enters The crude product tank 9 is connected to the nanofiltration box 13 through the third liquid inlet pipe 15. The nanofiltration box 13 is provided with a pH detector 20. The pH of the solution entering the nanofiltration box 13 is between 5 and 8. The third liquid inlet pipe 15 is provided with a third booster pump 12. The first liquid inlet pipe 5, the second liquid inlet pipe 8 and the third liquid inlet pipe 15 are all equipped with flow meters 18. The flow meters 18 installed on the first liquid inlet pipe 5, the second liquid inlet pipe 8 and the third liquid inlet pipe 15 are used to control the flow rate of the solution at 1-5m 3 / h, the liquid outlet of the nanofiltration box 13 is connected to the product tank 16, and the third booster pump 12 pumps the solution in the crude product tank 9 into the nanofiltration box 13 through the third liquid inlet pipe 15. The pore size of the nanofiltration membrane 14 is 1-2nm, which can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc. in the solution, thereby improving the purity of the product, and the solution passing through the nanofiltration box 13 enters the product tank 16 through a pipeline.

[0029] In some embodiments, the primary reverse osmosis main unit 4, the secondary reverse osmosis main unit 7 and the nanofiltration box 13 are all equipped with a waste pipe 21, and the waste pipe 21 is connected to the waste treatment equipment 22. The waste filtered out from the primary reverse osmosis main unit 4, the secondary reverse osmosis main unit 7 and the nanofiltration box 13 enters the waste treatment equipment 22 from the waste pipe 21 for treatment, recycling and reuse.

[0030] It can be seen from the above technical scheme that a liquid phase osmosis membrane filtration system, when in use, feeds the headspace solvent ((N,N-dimethylformamide (DMF), dimethyl sulfoxide (DMSO), N,N-dimethylacetamide (DMAC), N-methylpyrrolidone (NMP)) from the feed pipe 2 into the raw material tank 1, and then the first booster pump 10 on the first liquid inlet pipe 5 pumps the headspace solvent in the raw material tank 1 into the primary reverse osmosis mainframe 4, and before entering the primary reverse osmosis mainframe 4, the mechanical impurities are filtered through the precision filter 3 installed on the first liquid inlet pipe 5, and the headspace solvent entering the primary reverse osmosis mainframe 4 overcomes the natural osmotic pressure and the resistance of the reverse osmosis membrane under the pressure of the first booster pump 10 so that the solution passes through the uniformly distributed reverse osmosis membrane, The solution passing through the reverse osmosis membrane enters the intermediate tank 6 from the liquid outlet of the first-stage reverse osmosis host 4, and the second booster pump 11 pumps the solution in the intermediate tank 6 into the second-stage reverse osmosis host 7 for further filtration. The pore size of the reverse osmosis membrane can remove formic acid, ether, acetone and other ions in the headspace solvent. The solution passing through the second-stage reverse osmosis host 7 flows out from the liquid outlet into the crude product tank 9, and the third booster pump 12 pumps the solution in the crude product tank 9 into the nanofiltration box 13 through the third liquid inlet pipe 15. The pore size of the nanofiltration membrane 14 is 1-2nm, which can remove divalent and trivalent ions, organic matter with Mn≥200, as well as microorganisms, colloids, heat sources, viruses, etc. in the solution, thereby improving the purity of the product. The solution passing through the nanofiltration box 13 enters the product tank 16 through a pipeline.

[0031] Those skilled in the art will readily come up with other embodiments of the present invention after considering the specification and practicing the application disclosed herein. The present invention is intended to cover any variation, use or adaptation of the present invention, which follows the general principles of the present invention and includes common knowledge or customary technical means in the art disclosed by the present invention. The specification and examples are to be regarded as exemplary only, and the true scope of the present invention is indicated by the claims.

[0032] It should be understood that the present invention is not limited to the precise structure described above and shown in the drawings, and various modifications and changes can be made without departing from its scope. The above-described embodiments of the present invention do not constitute a limitation on the scope of protection of the present invention.

Claims

1. A liquid phase permeation membrane filtration system, characterized in that: It comprises a raw material tank (1), a reverse osmosis main unit and a nanofiltration box (13); The reverse osmosis main unit comprises a primary reverse osmosis main unit (4) and a secondary reverse osmosis main unit (7), wherein the primary reverse osmosis main unit (4) and the secondary reverse osmosis main unit (7) are respectively evenly filled with reverse osmosis membranes; The nanofiltration box (13) is evenly filled with nanofiltration membranes (14), and the pore diameter of the nanofiltration membranes (14) is 1-2 nm; The raw material tank (1) is provided with a feed pipe (2), the raw material tank (1) is connected to the primary reverse osmosis main unit (4) via a first liquid inlet pipe (5), the first liquid inlet pipe (5) is provided with a first booster pump (10) and a precision filter (3), the liquid outlet of the primary reverse osmosis main unit (4) is connected to an intermediate tank (6) via a pipeline, the intermediate tank (6) is connected to the secondary reverse osmosis main unit (7) via a second liquid inlet pipe (8), the second liquid inlet pipe (8) is provided with a second booster pump (10) and a precision filter (3), The invention relates to a nanofiltration tank (13) and a reverse osmosis main unit (4). The secondary reverse osmosis main unit (7) has a liquid outlet connected to a crude product tank (9) via a pipeline, the crude product tank (9) is connected to the nanofiltration tank (13) via a third liquid inlet pipe (15), the third liquid inlet pipe (15) is provided with a third booster pump (12), the liquid outlet of the nanofiltration tank (13) is connected to a product tank (16), and pressure sensors (19) are provided in the inner cavities of the primary reverse osmosis main unit (4), the secondary reverse osmosis main unit (7) and the nanofiltration tank (13).

2. A liquid phase permeation membrane filtration system according to claim 1, characterized in that: A flow meter (18) is installed on each of the first liquid inlet pipe (5), the second liquid inlet pipe (8) and the third liquid inlet pipe (15).

3. A liquid phase permeation membrane filtration system according to claim 1, characterized in that: The nanofiltration box (13) is provided with a pH value detector (20).

4. A liquid phase permeation membrane filtration system according to claim 1, characterized in that: Temperature sensors (17) are provided in the inner cavities of the primary reverse osmosis main unit (4), the secondary reverse osmosis main unit (7) and the nanofiltration box (13).

5. A liquid phase permeation membrane filtration system according to claim 4, characterized in that: The primary reverse osmosis main unit (4), the secondary reverse osmosis main unit (7) and the nanofiltration box (13) are all equipped with a waste pipe (21), and the waste pipe (21) is connected to a waste treatment device (22).

6. The liquid phase permeation membrane filtration system according to claim 1, characterized in that: The nanofiltration membrane (14) is made of cellulose acetate filter membrane (CA), polyethersulfone filter membrane (PES) or polytetrafluoroethylene filter membrane (PTFE).