CN107081077A - A kind of Positively charged composite nanofiltration membrane and preparation method thereof - Google Patents
A kind of Positively charged composite nanofiltration membrane and preparation method thereof Download PDFInfo
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- CN107081077A CN107081077A CN201710329043.8A CN201710329043A CN107081077A CN 107081077 A CN107081077 A CN 107081077A CN 201710329043 A CN201710329043 A CN 201710329043A CN 107081077 A CN107081077 A CN 107081077A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/08—Polysaccharides
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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
-
- 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
-
- 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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/02—Hydrophilization
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/26—Spraying processes
Abstract
The invention belongs to technical field of membrane separation, there is provided a kind of Positively charged composite nanofiltration membrane and preparation method thereof.Described composite nanometer filtering film has lotus electropositive, including separating. functional layer and supporting layer, and supporting layer is located at below separating. functional layer；Described separating. functional layer is the ultra-thin dense film using dip coating formation, and its thickness is within 200nm；Described ultra-thin dense film is prepared by epoxypropyltrimethylchloride chloride chitosan, additive, crosslinking agent and solvent；The Positively charged composite nanofiltration membrane of the present invention is Flat Membrane or hollow-fibre membrane.Due to employing the epoxypropyltrimethylchloride chloride chitosan of commercialization in preparation process in its functional layer so that the composite membrane of preparation has lotus electropositive character, therefore has higher rejection to high price inorganic salts.This kind of film also has higher inoxidizability simultaneously, has widened it and has used scope, can apply to the processing containing effluent containing heavy metal ions, and other have the processing of the waste water compared with strong oxidizing property.
Description
Technical field
It is applied to desalinization, bitter desalination and a huge sum of money the invention belongs to technical field of membrane separation, more particularly to one kind
Belong to the organic macromolecule-based seperation film of ion removing.
Background technology
Nanofiltration-membrane technique is a kind of new separation technology of energy-conserving and environment-protective, and wherein positively charged nanofiltration membranes are due to being more suitable for weight
Metal ion removing, the separation of high price inorganic salts and good antipollution and anti-microbial property and obtained extensive research.Chitosan
It is a kind of hot macromolecule in day, its abundance is with low cost, hydrophilic good.But because its dissolubility is poor, it is difficult to directly make
Standby seperation film.HACC is to be got by chitosan by chemical modification, with good antibiotic property,
Film forming and ion exchange property and Cation adsorption, are widely used in water treatment field.Because chitosan quaternary ammonium salt has
Higher hydrophily and film forming and charge, can be used for preparing Positively charged composite nanofiltration membrane.Prepared simultaneously with the material
Film typically has stronger acid resistance and chlorine-resistant property, is a kind of excellent lotus positive electricity composite film material.
The content of the invention
It is compound it is an object of the invention to overcome the deficiencies of the prior art and provide a kind of easily prepared lotus positively charged polymer
NF membrane.With the macromolecule of commercialization such as polysulfones, polyether sulfone, PPSU, polyacrylonitrile, polyvinyl chloride, Kynoar, acetic acid
Cellulose etc. prepares the supporting layer of composite membrane using phase inversion, using the epoxypropyltrimethylchloride chloride chitosan of commercialization as
Function film material, composite nanometer filtering film is obtained on support membrane using dip coating.Handled by high-temperature cross-linking and obtained lotus positive electricity
NF membrane.The present invention helps to greatly simplify nanofiltration and counter-infiltration preparation process, while significantly reducing use cost, improving economical
Property, so as to help to realize scale application.
Technical scheme：
A kind of Positively charged composite nanofiltration membrane, described Positively charged composite nanofiltration membrane has lotus electropositive, including separation function
Layer and supporting layer, supporting layer are located at below separating. functional layer；
Described separating. functional layer is the ultra-thin dense film using dip coating formation, and its thickness is within 200nm；Described
Ultra-thin dense film is prepared by epoxypropyltrimethylchloride chloride chitosan, crosslinking agent and solvent；
Used crosslinking agent be glutaraldehyde, epoxychloropropane, epoxypropyltrimethylchloride chloride, pyromellitic trimethylsilyl chloride,
O-phthaloyl chloride, m-phthaloyl chloride, paraphthaloyl chloride or Adipoyl Chloride；
Described solvent is deionized water；
Described supporting layer is by cellulose series derivates, polysulfones, polyether sulfone, PPSU, polyacrylonitrile, polychlorostyrene second
The formation mixed above of one or both of alkene, Kynoar, polyimides, PEI, its thickness is 50~500
μm, aperture is 0~100nm.
Inorganic nano additive is also included in described ultra-thin dense film, described inorganic nano additive is nano oxidized
It is more than one or both of silicon, aluminum oxide, titanium oxide, ferroso-ferric oxide, lanthanum-strontium ferro-cobalt, molecular sieve, graphene, inorganic salts mixed
Close.
A kind of preparation method of Positively charged composite nanofiltration membrane, step is as follows：
(1) supporting layer of Positively charged composite nanofiltration membrane is prepared
Macromolecule organic material and solvent are mixed, mixed solution A is obtained；Wherein, the quality hundred of macromolecule organic material
It is 8~20wt% to divide hundred concentration, and the quality very concentration of solvent is 68~85wt%；Mixed solution A uniform ground is scraped
On non-woven fabrics/or spinning mode is used, the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film, then soaked
In deionized water, the support membrane of Positively charged composite nanofiltration membrane is obtained；
(2) separating. functional layer of Positively charged composite nanofiltration membrane is prepared
Epoxypropyltrimethylchloride chloride chitosan, inorganic nano additive are mixed with water, solution B, epoxy third is obtained
The quality very concentration of base trimethyl ammonium chloride chitosan is 0.2~5wt%, and the quality of inorganic nano additive is very dense
Spend for 0~0.2wt%；The support layer surface of step (1) preparation is applied to using dip coating solution B, through air-drying, purging or be heat-treated
Afterwards, then it is immersed in the solution containing crosslinking agent, the wherein quality of crosslinking agent very 0.1~2wt% of concentration；Carried out after taking-up
Heat treatment, heat treatment temperature is 20-100 DEG C, and heat treatment time is 2-30min, produces Positively charged composite nanofiltration membrane.
Described macromolecule organic material is cellulose series derivates, polysulfones, polyether sulfone, PPSU, polyacrylonitrile, poly-
One or both of vinyl chloride, Kynoar are mixed above.
Described solvent is N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE or dimethyl
Sulfoxide.
The solution of described crosslinking agent is ethanol solution, the aqueous solution of glutaraldehyde, the ethanol of glutaraldehyde of epoxychloropropane
Solution, the hexane solution of pyromellitic trimethylsilyl chloride, the cyclohexane solution of pyromellitic trimethylsilyl chloride, o-phthaloyl chloride n-hexane it is molten
Liquid, the cyclohexane solution of o-phthaloyl chloride, the cyclohexane solution of m-phthaloyl chloride, m-phthaloyl chloride n-hexane it is molten
Liquid, the hexane solution of paraphthaloyl chloride, the cyclohexane solution of paraphthaloyl chloride, the cyclohexane solution of Adipoyl Chloride, oneself
The hexane solution of diacid chloride and the aqueous solution of epoxypropyltrimethylchloride chloride.
Beneficial effects of the present invention：Positively charged nanofiltration membranes prepared by the present invention can be Flat Membrane or hollow
Tunica fibrosa.Due to employing the epoxypropyltrimethylchloride chloride chitosan of commercialization in preparation process in its functional layer so that
The composite membrane of preparation has lotus electropositive character, therefore has higher rejection to high price inorganic salts.This kind of film also has simultaneously
Higher inoxidizability, has widened it and has used scope, can apply to the processing containing effluent containing heavy metal ions, and other tools
There is the processing of the waste water compared with strong oxidizing property.
Embodiment
Below in conjunction with technical scheme, the embodiment of the present invention is further illustrated.
Embodiment one：
(1) preparation of seperation film：
Using polyether sulfone as support film material, DMA (DMAc) is solvent, is prepared using phase inversion
Into poly (ether-sulfone) ultrafiltration membrane.Using it as basement membrane, composite nanometer filtering film functional layer is prepared using dip coating thereon.It is specific as follows：Will
1wt% epoxypropyltrimethylchloride chloride chitosan is as solute, and deionized water is solvent, is film-made using dip coating.Formed
Primary membrane in an oven drying temperature be 60 DEG C, the time is 5min.It is immersed in 1% glutaraldehyde solution 10 seconds, takes out afterwards
60 DEG C of drying, the time is 5min.
(2) apply：
Processing solution is 1g/L magnesium chloride solution, and when external pressure is 0.3MPa, seperation film is cut to inorganic salts magnesium chloride
It is 92% to stay rate, and water flux is up to 20L/m2h。
Embodiment two：
(1) preparation of seperation film：
Using PEI as support film material, 1-METHYLPYRROLIDONE is solvent, is prepared into using phase inversion poly-
Ether sulfone milipore filter.Using it as basement membrane, composite nanometer filtering film functional layer is prepared using dip coating thereon.It is specific as follows：By 1wt%'s
Epoxypropyltrimethylchloride chloride chitosan is solute, and 0.5% nano lanthanum-strontium ferro-cobalt is additive, and deionized water is scattered
Agent, is film-made using dip coating.Drying temperature is 60 DEG C to the primary membrane of formation in an oven, and the time is 5min.It is then immersed in immersion
Into 1% epoxychloropropane ethanol solution 10 seconds, 60 DEG C of drying is taken out, the time is 5min.
(2) apply
Processing solution is 1g/L magnesium chloride solution, when external pressure is 0.3MPa, retention of the seperation film to inorganic ion
Rate is 90%, and water flux is up to 25L/m2h。
Claims (8)
1. a kind of Positively charged composite nanofiltration membrane, it is characterised in that described Positively charged composite nanofiltration membrane has lotus electropositive, including
Separating. functional layer and supporting layer, supporting layer are located at below separating. functional layer；
Described separating. functional layer is the ultra-thin dense film using dip coating formation, and its thickness is within 200nm；Described is ultra-thin
Dense film is prepared by epoxypropyltrimethylchloride chloride chitosan, crosslinking agent and solvent；
Used crosslinking agent is glutaraldehyde, epoxychloropropane, epoxypropyltrimethylchloride chloride, pyromellitic trimethylsilyl chloride, adjacent benzene
Dimethyl chloride, m-phthaloyl chloride, paraphthaloyl chloride or Adipoyl Chloride；
Described solvent is deionized water；
Described supporting layer is by cellulose series derivates, polysulfones, polyether sulfone, PPSU, polyacrylonitrile, polyvinyl chloride, poly-
The formation mixed above of one or both of vinylidene, polyimides, PEI, its thickness is 50~500 μm, hole
Footpath is 0~100nm.
2. the Positively charged composite nanofiltration membrane described in requirement 1 according to right, it is characterised in that in described ultra-thin dense film
Also include inorganic nano additive.
3. Positively charged composite nanofiltration membrane according to claim 2, it is characterised in that described inorganic nano additive is to receive
One or both of rice silica, aluminum oxide, titanium oxide, ferroso-ferric oxide, lanthanum-strontium ferro-cobalt, molecular sieve, graphene, inorganic salts
It is mixed above.
4. a kind of preparation method of Positively charged composite nanofiltration membrane, it is characterised in that step is as follows：
(1) supporting layer of Positively charged composite nanofiltration membrane is prepared
Macromolecule organic material and solvent are mixed, mixed solution A is obtained；Wherein, the quality of macromolecule organic material is very
Concentration is 8~20wt%, and the quality very concentration of solvent is 68~85wt%；Mixed solution A uniform ground is scraped in nonwoven
On cloth/or spinning mode is used, the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film, is then immersed in
In ionized water, the support membrane of Positively charged composite nanofiltration membrane is obtained；
(2) separating. functional layer of Positively charged composite nanofiltration membrane is prepared
Epoxypropyltrimethylchloride chloride chitosan, inorganic nano additive are mixed with water, solution B, glycidyl three is obtained
The quality of ammonio methacrylate chitosan very concentration is 0.2~5wt%, and the quality very concentration of inorganic nano additive is
0~0.2wt%；The support layer surface of step (1) preparation is applied to using dip coating solution B, after air-drying, purging or be heat-treated,
It is immersed in again in the solution containing crosslinking agent, wherein the quality of crosslinking agent very 0.1~2wt% of concentration；Heat is carried out after taking-up
Processing, heat treatment temperature is 20-100 DEG C, and heat treatment time is 2-30min, produces Positively charged composite nanofiltration membrane.
5. preparation method according to claim 4, it is characterised in that described macromolecule organic material is cellulose series
One or both of derivative, polysulfones, polyether sulfone, PPSU, polyacrylonitrile, polyvinyl chloride, Kynoar are mixed above.
6. the preparation method according to claim 4 or 5, it is characterised in that described solvent be DMF,
DMAC N,N' dimethyl acetamide, 1-METHYLPYRROLIDONE or dimethyl sulfoxide (DMSO).
7. the preparation method according to claim 4 or 5, it is characterised in that the solution of described crosslinking agent is epoxy chloropropionate
The ethanol solution of alkane, the aqueous solution of glutaraldehyde, the ethanol solution of glutaraldehyde, the hexane solution of pyromellitic trimethylsilyl chloride, equal benzene three
The cyclohexane solution of formyl chloride, the hexane solution of o-phthaloyl chloride, the cyclohexane solution of o-phthaloyl chloride, isophthalic diformazan
The cyclohexane solution of acyl chlorides, the hexane solution of m-phthaloyl chloride, the hexane solution of paraphthaloyl chloride, paraphenylene terephthalamide
The cyclohexane solution of chlorine, the cyclohexane solution of Adipoyl Chloride, the hexane solution and epoxypropyl trimethylammonium chloride of Adipoyl Chloride
The aqueous solution of ammonium.
8. preparation method according to claim 6, it is characterised in that the solution of described crosslinking agent is epoxychloropropane
Ethanol solution, the aqueous solution of glutaraldehyde, the ethanol solution of glutaraldehyde, the hexane solution of pyromellitic trimethylsilyl chloride, the formyl of equal benzene three
The cyclohexane solution of chlorine, the hexane solution of o-phthaloyl chloride, the cyclohexane solution of o-phthaloyl chloride, m-phthaloyl chloride
Cyclohexane solution, the hexane solution of m-phthaloyl chloride, the hexane solution of paraphthaloyl chloride, paraphthaloyl chloride
Cyclohexane solution, the cyclohexane solution of Adipoyl Chloride, the hexane solution of Adipoyl Chloride and epoxypropyltrimethylchloride chloride
The aqueous solution.
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Cited By (10)
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| CN108355498A (en) * | 2018-02-08 | 2018-08-03 | 广州中国科学院先进技术研究所 | Bear electricity composite nanometer filtering film and preparation method thereof |
| CN109200823A (en) * | 2018-08-28 | 2019-01-15 | 浙江工业大学 | A kind of preparation method and application for the ecosystem positively charged nanofiltration membranes that polyethyleneimine is amine-modified |
| CN109692585A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Nanofiltration membrane and its preparation method and application |
| CN109692579A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Reverse osmosis membrane and its preparation method and application |
| CN109749145A (en) * | 2018-11-29 | 2019-05-14 | 陶伟珍 | A kind of preparation method of modified lignin resin/chitosan rubber reinforcement filler |
| WO2019171311A1 (en) * | 2018-03-07 | 2019-09-12 | King's Flair Development Ltd. | Functional fibrous membrane, method for manufacturing the same, filter comprising the same |
| CN110917897A (en) * | 2019-12-19 | 2020-03-27 | 中化(宁波)润沃膜科技有限公司 | Composite nanofiltration membrane and preparation method thereof |
| CN113908703A (en) * | 2021-09-22 | 2022-01-11 | 浙江大学 | Charged nanofiltration membrane based on polymer nanoparticles and preparation method thereof |
| CN114471195A (en) * | 2020-10-23 | 2022-05-13 | 宁波方太厨具有限公司 | Casting solution, hollow fiber membrane prepared by using same and preparation method of hollow fiber membrane |
| CN115364684A (en) * | 2022-10-25 | 2022-11-22 | 天津大学 | High-flux positively-charged nanofiltration membrane and preparation method thereof |
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Cited By (16)
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| CN109692585A (en) * | 2017-10-20 | 2019-04-30 | 中国石油化工股份有限公司 | Nanofiltration membrane and its preparation method and application |
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| WO2019171311A1 (en) * | 2018-03-07 | 2019-09-12 | King's Flair Development Ltd. | Functional fibrous membrane, method for manufacturing the same, filter comprising the same |
| CN109200823A (en) * | 2018-08-28 | 2019-01-15 | 浙江工业大学 | A kind of preparation method and application for the ecosystem positively charged nanofiltration membranes that polyethyleneimine is amine-modified |
| CN109749145B (en) * | 2018-11-29 | 2020-08-21 | 陶伟珍 | Preparation method of modified lignin/chitosan rubber reinforced filler |
| CN109749145A (en) * | 2018-11-29 | 2019-05-14 | 陶伟珍 | A kind of preparation method of modified lignin resin/chitosan rubber reinforcement filler |
| CN110917897A (en) * | 2019-12-19 | 2020-03-27 | 中化(宁波)润沃膜科技有限公司 | Composite nanofiltration membrane and preparation method thereof |
| CN110917897B (en) * | 2019-12-19 | 2022-07-29 | 中化(宁波)润沃膜科技有限公司 | Composite nanofiltration membrane and preparation method thereof |
| CN114471195A (en) * | 2020-10-23 | 2022-05-13 | 宁波方太厨具有限公司 | Casting solution, hollow fiber membrane prepared by using same and preparation method of hollow fiber membrane |
| CN114471195B (en) * | 2020-10-23 | 2022-11-29 | 宁波方太厨具有限公司 | Preparation method of hollow fiber membrane |
| CN113908703A (en) * | 2021-09-22 | 2022-01-11 | 浙江大学 | Charged nanofiltration membrane based on polymer nanoparticles and preparation method thereof |
| CN113908703B (en) * | 2021-09-22 | 2023-01-10 | 浙江大学 | Charged nanofiltration membrane based on polymer nanoparticles and preparation method thereof |
| CN115364684A (en) * | 2022-10-25 | 2022-11-22 | 天津大学 | High-flux positively-charged nanofiltration membrane and preparation method thereof |
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Application publication date: 20170822 |