CN112058094B - Loose nanofiltration membrane and preparation method thereof - Google Patents
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- CN112058094B CN112058094B CN202010944768.XA CN202010944768A CN112058094B CN 112058094 B CN112058094 B CN 112058094B CN 202010944768 A CN202010944768 A CN 202010944768A CN 112058094 B CN112058094 B CN 112058094B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D17/00—Separation of liquids, not provided for elsewhere, e.g. by thermal diffusion
- B01D17/02—Separation of non-miscible liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/30—Cross-linking
Abstract
The invention provides a preparation method of a loose nanofiltration membrane, which comprises the following steps: adding a certain amount of polymer membrane material, polyurea microspheres and pore-forming agent into an organic solvent, heating and stirring to prepare a homogeneous phase solution, and obtaining a membrane casting solution; standing the casting solution in vacuum and defoaming; preparing the defoamed membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for storage; and coating a cross-linking agent on the surface of the base membrane, and cross-linking the base membrane and the cross-linking agent to obtain the nanofiltration membrane material with a loose separation structure on the surface. The invention also provides a loose nanofiltration membrane. The loose nanofiltration membrane prepared by the preparation method provided by the invention has excellent permeability and good separation effect.
Description
Technical Field
The invention relates to the technical field of high polymer materials, in particular to a loose nanofiltration membrane and a preparation method thereof.
Background
Ultrafiltration was one of the earliest membrane separation techniques used for treatment of printing and dyeing wastewater. The ultrafiltration membrane separation technology is usually used for the recovery of useful substances such as dyes, auxiliaries and the like, the recycling of penetrating fluid or the standard discharge of waste water in the treatment of printing and dyeing waste water. However, due to the large pore diameter of the ultrafiltration membrane, the removal effect on soluble substances is not high, the retention capacity on salt is poor, and the removal of small molecular dyes in mixed liquid cannot be completed, so that the single ultrafiltration membrane filtration process cannot meet the treatment requirement and the discharge standard of printing and dyeing wastewater. And the cut molecular weight of the nanofiltration membrane is 200-1000 Da. The molecular weight of the conventional dye molecules is generally between hundreds and thousands, and in addition, the water-soluble dye usually contains polar groups such as carboxyl or sulfonic acid groups and the like, and can be negatively charged in an aqueous solution, so that the rejection rate of the nano-filtration membrane on pollutants in the printing and dyeing wastewater is relatively high.
In the related technology, the surface of the nanofiltration membrane has dense holes, so that the nanofiltration membrane has a good dye removal effect, but also has a certain interception capability on divalent salt and monovalent salt in the mixed solution, so that the separation of the dye and the salt mixed solution cannot be effectively completed.
Therefore, there is a need to provide a novel porous nanofiltration membrane and a preparation method thereof to solve the above problems.
Disclosure of Invention
The invention aims to overcome the technical problems and provide a loose nanofiltration membrane with excellent permeability and good separation effect and a preparation method thereof.
In order to realize the aim, the invention provides a preparation method of a loose nanofiltration membrane, which comprises the following steps:
adding a certain amount of polymer membrane material, polyurea microspheres and pore-forming agent into an organic solvent, heating and stirring to prepare a homogeneous phase solution, and obtaining a membrane casting solution;
standing the casting solution in vacuum and defoaming;
preparing the defoamed membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for storage;
and coating a cross-linking agent on the surface of the base membrane, and cross-linking the base membrane and the cross-linking agent to obtain the nanofiltration membrane material with a loose separation structure on the surface.
Preferably, the polymer membrane material is formed by mixing one or more of polyether sulfone, sulfonated polyether sulfone, polysulfone, sulfonated polysulfone and polyvinylidene fluoride.
Preferably, the pore-foaming agent is polyethylene glycol or polyvinylpyrrolidone.
Preferably, the organic solvent is N, N-dimethylacetamide or N, N-dimethylformamide.
Preferably, the polyurea microspheres are micro-or nano-scale polymer spheres.
Preferably, the mass percentages of the polymer membrane material, the polyurea microspheres, the pore-forming agent and the organic solvent in the membrane casting solution are respectively 15-20%, 1-10%, 2-9% and 60-80%.
Preferably, the cross-linking agent is m-phenylenediamine or glutaraldehyde, and the mass fraction of the cross-linking agent is 2% -15%.
The invention also discloses a loose nanofiltration membrane prepared by the preparation method.
Compared with the related technology, in the loose nanofiltration membrane and the preparation method thereof provided by the invention, a separation layer with a loose structure is formed on the surface of the membrane through the cross-linking reaction between long-chain polymer monomers; after the base membrane is formed, a loose nanofiltration membrane with a loose separation structure on the surface is obtained on the surface of the base membrane through the cross-linking reaction of the isophthalaldehyde and the polyurea microspheres. The polyurea microspheres and the base membrane are blended to enhance the binding capacity between the separation layer and the support layer, so that the prepared nanofiltration membrane can achieve the effects of good interception effect, excellent permeability and high-efficiency pollution resistance in the process of micromolecule separation by dye desalination, and the loose surface characteristics of the structure of the separation layer endow the nanofiltration membrane with better and more specific performance, so that the separation membrane can be used for separation processes such as oil-water separation, protein and drug purification.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all 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.
The invention provides a preparation method of a loose nanofiltration membrane, which comprises the following steps:
s1: adding a certain amount of polymer membrane material, polyurea microspheres and pore-forming agent into an organic solvent, heating and stirring to prepare a homogeneous phase solution, and obtaining a membrane casting solution.
The polymer membrane material is one or a mixture of polyether sulfone, sulfonated polyether sulfone, polysulfone, sulfonated polysulfone and polyvinylidene fluoride; the pore-foaming agent is polyethylene glycol or polyvinylpyrrolidone; the organic solvent is N, N-dimethylacetamide or N, N-dimethylformamide; the polyurea microspheres are micron-sized or nano-sized polymer spheres.
The mass percentages of the polymer membrane material, the polyurea microspheres, the pore-forming agent and the organic solvent in the membrane casting solution are respectively 15-20%, 1-10%, 2-9% and 60-80%.
The pore-foaming agent can adjust the hydrophilicity of the polymer membrane material and the viscosity of the membrane casting solution, thereby influencing the performances of the porosity, the pure water flux and the like of the formed membrane.
S2: and standing the casting solution in vacuum and defoaming.
S3: preparing the defoamed membrane casting solution into a basement membrane by a phase inversion method, and placing the basement membrane in deionized water for storage.
S4: and coating a cross-linking agent on the surface of the base membrane, and cross-linking the base membrane and the cross-linking agent to obtain the nanofiltration membrane material with a loose separation structure on the surface.
The cross-linking agent is m-phenylenediamine or glutaraldehyde, and the mass fraction of the cross-linking agent is 2% -15%. Preferably, the cross-linking agent is isophthalaldehyde.
In the preparation method provided by the invention, the polyurea microspheres, the polymer membrane material and the pore-forming agent are mixed in advance, then the cross-linking reaction is carried out on the polyurea microspheres and the cross-linking agent with high reaction activity, and the nanofiltration membrane with a loose separation structure can be obtained through one-step reaction.
The polymer membrane material is long-chain polymer monomers, and a cross-linking reaction among the long-chain polymer monomers is favorable for forming a separation layer with a loose structure on the surface of the membrane; after the base membrane is formed, a loose nanofiltration membrane with a loose separation structure on the surface is obtained on the surface of the base membrane through the cross-linking reaction of the isophthalaldehyde and the polyurea microspheres. The polyurea microspheres and the base membrane are blended to enhance the binding capacity between the separation layer and the support layer, so that the prepared nanofiltration membrane can achieve the effects of good interception effect, excellent permeability and high-efficiency pollution resistance in the process of micromolecule separation by dye desalination, and the loose surface characteristics of the structure of the separation layer endow the nanofiltration membrane with better and more specific performance, so that the separation membrane can be used for separation processes such as oil-water separation, protein and drug purification.
The invention also provides a loose nanofiltration membrane prepared by the preparation method.
Example one
The embodiment provides a preparation method of a loose nanofiltration membrane, which comprises the following specific steps:
(1) preparing a casting solution: adding 20g of polyether sulfone, 5g of polyurea microspheres and 5g of polyethylene glycol-800 into 70ml of N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: and (3) preparing an m-phenylenediamine ethanol solution with the mass fraction of 5%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for one hour to obtain the loose nanofiltration membrane A.
Example two
The embodiment provides a preparation method of a loose nanofiltration membrane, which comprises the following specific steps:
(1) preparing a casting solution: adding 17g of polysulfone, 3g of polyurea microspheres and 5g of polyvinylpyrrolidone into 75mLN, N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: and (3) preparing an m-phenylenediamine ethanol solution with the mass fraction of 10%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for 45 minutes to obtain the loose nanofiltration membrane B.
EXAMPLE III
The embodiment provides a preparation method of a loose nanofiltration membrane, which comprises the following specific steps:
(1) preparing a casting solution: adding 20g of polyvinylidene fluoride, 3g of polyurea microspheres and 5g of polyvinylpyrrolidone into 72mLN, N-dimethylacetamide organic solution, heating to 80 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: and (3) preparing an m-phenylenediamine ethanol solution with the mass fraction of 3%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for 1.5 hours to obtain the loose nanofiltration membrane C.
Example four
The embodiment provides a preparation method of a loose nanofiltration membrane, which comprises the following specific steps:
(1) preparing a casting solution: adding 17g of polysulfone, 2g of polyurea microspheres and 5g of polyethylene glycol-1000 into 76mLN, N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: and (3) preparing an m-phenylenediamine ethanol solution with the mass fraction of 15%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for 30 minutes to obtain the loose nanofiltration membrane D.
The loose nanofiltration membranes A-D obtained in the above examples were subjected to interception experiments and water contact angle tests of different solutions, and the corresponding properties were measured as shown in the following table:
the experiment proves that the prepared loose nanofiltration membrane has higher separation effect on micromolecular dye and multivalent salt, and the loose nanofiltration membrane has excellent permeability and separation efficiency.
Compared with the related technology, in the loose nanofiltration membrane and the preparation method thereof provided by the invention, a separation layer with a loose structure is formed on the surface of the membrane through the cross-linking reaction between long-chain polymer monomers; after the base membrane is formed, a loose nanofiltration membrane with a loose separation structure on the surface is obtained on the surface of the base membrane through the cross-linking reaction of the isophthalaldehyde and the polyurea microspheres. The polyurea microspheres and the base membrane are blended to enhance the binding capacity between the separation layer and the support layer, so that the prepared nanofiltration membrane can achieve the effects of good interception effect, excellent permeability and high-efficiency pollution resistance in the process of micromolecule separation by dye desalination, and the loose surface characteristics of the structure of the separation layer endow the nanofiltration membrane with better and more specific performance, so that the separation membrane can be used for separation processes such as oil-water separation, protein and drug purification.
While the foregoing is directed to embodiments of the present invention, it will be understood by those skilled in the art that various changes may be made without departing from the spirit and scope of the invention.
Claims (4)
1. The preparation method of the loose nanofiltration membrane is characterized by comprising the following steps:
(1) preparing a casting solution: adding 20g of polyether sulfone, 5g of polyurea microspheres and 5g of polyethylene glycol-800 into 70mL of N, N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: and (3) preparing an m-phenylenediamine ethanol solution with the mass fraction of 5%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for one hour to obtain the loose nanofiltration membrane.
2. The preparation method of the loose nanofiltration membrane is characterized by comprising the following steps:
(1) preparing a casting solution: adding 17g of polysulfone, 3g of polyurea microspheres and 5g of polyvinylpyrrolidone into 75mL of N, N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: preparing a m-phenylenediamine ethanol solution with the mass fraction of 10%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for 45 minutes to obtain the loose nanofiltration membrane.
3. The preparation method of the loose nanofiltration membrane is characterized by comprising the following steps:
(1) preparing a casting solution: adding 20g of polyvinylidene fluoride, 3g of polyurea microspheres and 5g of polyvinylpyrrolidone into 72mL of N, N-dimethylacetamide organic solution, heating to 80 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: preparing an m-phenylenediamine ethanol solution with the mass fraction of 3%, coating the m-phenylenediamine ethanol solution on the surface of the base membrane, and crosslinking for 1.5 hours to obtain the loose nanofiltration membrane.
4. The preparation method of the loose nanofiltration membrane is characterized by comprising the following steps:
(1) preparing a casting solution: adding 17g of polysulfone, 2g of polyurea microspheres and 5g of polyethylene glycol-1000 into 76mL of N, N-dimethylacetamide organic solution, heating to 70 ℃, and stirring to be homogeneous;
(2) and (3) vacuum standing defoaming: vacuumizing the casting solution in a heating state, stopping stirring and defoaming;
(3) preparation of a base film: preparing the membrane casting solution into a base membrane by a phase inversion method, and placing the base membrane in deionized water for later use;
(4) preparation of a loose nanofiltration membrane: preparing 15% m-phenylenediamine ethanol solution, coating the solution on the surface of the base membrane, and crosslinking for 30 minutes to obtain the loose nanofiltration membrane.
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| CN112978862A (en) * | 2021-05-11 | 2021-06-18 | 上海集熠节能环保技术有限公司 | Concentration filtering desalination device and filtering component |
| CN117000045B (en) * | 2023-06-01 | 2024-02-20 | 贵州省材料产业技术研究院 | Loose nanofiltration membrane for removing heavy metals and preparation method thereof |
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