CN107029555A - A kind of solvent resistant NF membrane and preparation method thereof - Google Patents
A kind of solvent resistant NF membrane and preparation method thereof Download PDFInfo
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- CN107029555A CN107029555A CN201710248420.5A CN201710248420A CN107029555A CN 107029555 A CN107029555 A CN 107029555A CN 201710248420 A CN201710248420 A CN 201710248420A CN 107029555 A CN107029555 A CN 107029555A
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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
-
- 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
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- 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
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
-
- 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
-
- 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
-
- 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
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
Abstract
The invention belongs to technical field of membrane separation, there is provided a kind of solvent resistant NF membrane and preparation method thereof.A kind of solvent resistant NF membrane, described solvent resistant NF membrane has charge, its integrated flat board or doughnut solvent resistant NF membrane.Or a kind of solvent resistant NF membrane, described solvent resistant NF membrane has charge, and it includes separating. functional layer and supporting layer, and supporting layer is located at below separating. functional layer.Solvent resistant NF membrane prepared by the present invention can be Flat Membrane or hollow-fibre membrane.Because it have passed through crosslinking Treatment, solvent resistance is more excellent, and use environment extensively, can apply to the processing of the industrial wastewater containing organic solvent, the tolerance especially for highly polar organic solvent is very strong.The limitation that current commercialization NF membrane can not be used in containing highly polar organic solvent is solved, can be by the application extension of NF membrane to petroleum chemical industry and the Industrial Wastewater Treatment containing organic solvent and reuse field.
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 ion removing, be particularly the organic macromolecule-based seperation film in the fields such as the Industrial Wastewater Treatment use containing organic solvent.
Background technology
One kind that membrane separating process belongs in speed separation process, it passes through film as separating medium using selectivity, when in film
Both sides exist certain motive force when (such as pressure differential, concentration difference and potential difference), motive force effect under different component in film
In have different penetrating powers, so as to selectively pass through film, and then reach the purpose of separating-purifying.The method is with passing
The separation method of system is compared, not only with separative efficiency is high, energy consumption is low, floor space is small, process is simple and convenient to operate, not dirty
Dye environment, be easy to other technologies it is integrated the advantages of, and can be directly separated some insoluble systems according to a conventional method,
Such as azeotropic system, thermal sensitivity system.
The membrane technology applied to desalinization and ion removing field is mainly hyperfiltration, electroosmose process and nanofiltration at present
Method.Wherein, hyperfiltration salt rejection rate is higher, film permeation flux is smaller, it is necessary to operating pressure it is also higher (about 1.5~
20MPa);The voltage of its DC electric field of electroosmose process desalination processes is higher (100~300V), compared with reverse osmosis membrane, and it takes off
Salt rate and Water Sproading rate are relatively low, and easily occur concentration polarization and cause fouling, equipment complexity rapid wear;Nanofiltering membrane is inorganic in high price
Salt ion removing field has higher separation selectivity.In above-mentioned membrane separation technique, the seperation film used is polymer-based
Seperation film, its preparation process typically all comes preparative separation film functional layer or basement membrane using organic solvent, therefore these films are organic
Solvent is particularly the less stable in highly polar organic solvent, is easily swelled or even dissolves.In recent years, also researched and developed micro-
The nanofiltration membrane technology of pore structure, but inorganic ceramic material used in the technology has the more difficult control of building-up process, nothing
The problems such as control of machine membrane aperture is difficult, permeation flux is relatively low, limits the scope of its commercial Application.Simultaneously as inorganic material
Rigidity and Brittleness, be that assembling design brings limitation, loading density is relatively low, effective active area is small, operating cost is high,
It is difficult to scale application.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of easily prepared solvent resistant polymer ultrafiltration
Film, and obtain composite nanometer filtering film in coating thereon or interfacial polymerization.Obtained by crosslinking Treatment in highly polar organic solvent such as
Film properties do not have in DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, dimethyl sulfoxide (DMSO) or the 1-METHYLPYRROLIDONE aqueous solution
There is the solvent resistant seperation film of decline.The present invention helps to realize the advanced treating of the waste water containing organic solvent, while significantly reducing makes
With cost, economy is improved, so as to help to realize scale application.
Technical scheme:
A kind of solvent resistant NF membrane, the described integrated flat board of solvent resistant NF membrane or doughnut solvent resistant nanofiltration
Film;Described integral flat or hollow fiber nanofiltration membrane are by cellulose series derivates, chitosan series derivates, poly- second
Alkene imines, sulfonated polyether sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethyl polysulphone,
Chloromethylation polyether-ketone, chloromethylation PPSU or polyacrylonitrile formation, its thickness be 50~500 μm, aperture be 0~
100nm。
A kind of solvent resistant NF membrane, described solvent resistant NF membrane includes separating. functional layer and supporting layer, and supporting layer is located at
Below separating. functional layer;
Described separating. functional layer is by cellulose series derivates, chitosan series derivates, polyethyleneimine, sulfonation
Polyether sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethyl polysulphone, chloromethylation gather
Ether ketone, chloromethylation PPSU or polyacrylonitrile formation dense film or perforated membrane, thickness be 1~20 μm, aperture be 0~
100nm;
Described supporting layer is by cellulose series derivates, chitosan series derivates, polyvinyl alcohol or polyacrylamide
Amine formation, its thickness is 50~500 μm, and aperture is 0~100nm.
Organic-inorganic hybrid films formed by inorganic nano additive are introduced in described separating. functional layer, inorganic nano adds
Plus agent includes nano silicon oxide, aluminum oxide, titanium oxide, ferroso-ferric oxide, lanthanum-strontium ferro-cobalt, molecular sieve, graphene and inorganic salts.
Nano silicon oxide, aluminum oxide, titanium oxide, ferroso-ferric oxide, lanthanum-strontium ferro-cobalt, molecule are added in described supporting layer
One or both of sieve, graphene, inorganic salts are mixed above.
A kind of preparation method of solvent resistant NF membrane, step is as follows:
Prepare integrated solvent resistant flat board or hollow fiber nanofiltration membrane
Inorganic nano additive, macromolecule organic material and solvent are mixed, mixed solution or dispersion liquid is obtained, nothing is controlled
The quality of machine additive very concentration is that 0~12wt%, the quality very concentration of macromolecule organic material are 8~20wt%
Quality very concentration with solvent is 68~85wt%;Above-mentioned mixed solution or homogeneous dispersion are coated on non-woven fabrics or
Weaved using spinning mode on non-woven fabrics, the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film;With
Crosslinking Treatment is carried out using crosslinking agent afterwards, crosslinking temperature is 10-120 DEG C, and crosslinking time is 1-30 minutes, is then immersed in deionization
In water, that is, obtain the solvent resistant NF membrane of integrated solvent resistant flat board or doughnut.
A kind of preparation method of solvent resistant NF membrane, step is as follows:
(1) support membrane of solvent resistant NF membrane is prepared
Inorganic additive, macromolecule organic material A and solvent are mixed, mixed solution A or dispersion liquid A is obtained;Wherein, nothing
The quality of machine additive very concentration be 0~12wt%, the quality very concentration of macromolecule organic material be 8~
20wt%, the quality very concentration of solvent are 68~85wt%;Scrape above-mentioned mixed solution or homogeneous dispersion are smooth in nothing
Spin on cloth/or by the way of spinning, the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film;Then adopt
Crosslinking Treatment is carried out with crosslinking agent, crosslinking time is 1-30min, and crosslinking temperature is 10-120 DEG C, is then soaked in deionized water,
Obtain the support membrane of solvent resistant NF membrane;
Described macromolecule organic material A include cellulose series derivates, chitosan series derivates, polyvinyl alcohol and
Polyacrylamide;
(2) separating. functional layer of solvent resistant NF membrane is prepared
Inorganic additive, macromolecule organic material B and solvent are mixed, mixed solution B or dispersion liquid B is obtained;Wherein without
The quality of machine additive very concentration be 0~2wt%, the quality very concentration of macromolecule organic material be 0.3~
5wt%, the quality very concentration of solvent are 83~98wt%;One layer of mixing of blade coating is molten on support membrane prepared by step (1)
Liquid B or dispersion liquid B, after heat treatment, obtains solvent resistant NF membrane;Heat treatment temperature is 20-80 DEG C, and heat treatment time is 5-
50min;
Described macromolecule organic material B includes cellulose series derivates, chitosan series derivates, polyethyleneimine
Amine, sulfonated polyether sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethyl polysulphone, chloromethane
Base polyether-ketone, chloromethylation PPSU and polyacrylonitrile;
(3) the solvent resistant NF membrane for preparing step (2) is immersed in cross-linking agent solution, and soak time is 5s-
300s, soaking temperature is 10-60 DEG C;Then crosslinking temperature be 10-100 DEG C under the conditions of, be crosslinked 1-30 minutes, after be immersed in from
Sub- water, produces stable solvent resistant NF membrane.
Described crosslinking agent is the concentrated sulfuric acid, trimethylamine, ethylenediamine, triethylene tetramine, polyethyleneimine, glutaraldehyde, equal benzene
Three formyl chlorides, paraphthaloyl chloride, o-phthaloyl chloride, epoxychloropropane, pentaerythrite, ethylene glycol or glycerine.
Described solvent is DMAC N,N' dimethyl acetamide, N,N-dimethylformamide, dimethyl sulfoxide (DMSO) or N- methylpyrroles
Alkanone.
Can be added in described supporting layer nano silicon oxide, aluminum oxide, titanium oxide, ferroso-ferric oxide, lanthanum-strontium ferro-cobalt, point
The inorganic additives such as sub- sieve, graphene.
Described supporting layer through polyamine monomers such as the concentrated sulfuric acid, trimethylamine, ethylenediamine, triethylene tetramine, polyethyleneimines or
Glutaraldehyde, pyromellitic trimethylsilyl chloride, paraphthaloyl chloride, o-phthaloyl chloride, epoxychloropropane, pentaerythrite, ethylene glycol, the third three
The polyfunctional group organic molecule such as alcohol is cross-linked to form solvent-proof supporting layer.
Beneficial effects of the present invention:Solvent resistant NF membrane prepared by the present invention can be Flat Membrane or hollow
Tunica fibrosa.Because it have passed through crosslinking Treatment, solvent resistance is more excellent, and use environment extensively, can apply to containing organic
The processing of the industrial wastewater of solvent, the tolerance especially for highly polar organic solvent is very strong.Current commercialization is solved to receive
The limitation that filter membrane can not be used in containing highly polar organic solvent, can be by the application extension of NF membrane to petroleum chemical industry
With the Industrial Wastewater Treatment containing organic solvent and reuse field.
Embodiment
Below in conjunction with technical scheme, the embodiment of the present invention is further illustrated.
Embodiment one:
(1) preparation of seperation film:
Using cellulose diacetate as organic phase, DMA (DMAc) is solvent, is prepared using phase inversion
Into cellulose-acetafolic.Handled using glutaraldehyde cross-linking and solvent resistant milipore filter is made.Using it as basement membrane, one is applied thereon
Quantitative chloromethylation PPSU (PPSU), and obtain solvent-proof composite separating film using triethylene tetramine is cross-linking modified.Tool
Body is as follows:By 12wt% cellulose diacetate, 88wt% DMAc it is well mixed, vacuumize, the knifing on non-woven fabrics,
Inversion of phases occurs in coagulation bath and obtains milipore filter film, immersion treatment 30 minutes in 5% glutaraldehyde solution are made solvent-proof
Milipore filter.In the chloromethylation PPSU of coating 1% thereon, solvent resistant is prepared using 2% triethylene tetramine is cross-linking modified
Composite separating film.
(2) apply:
Processing solution is 1g/L MgCl2Solution, wherein containing 30% DMAc.When external pressure is 0.4MPa, seperation film
Rejection to inorganic ion is 76%, and water flux is up to 16L/m2h.Film in continuous operation 30 days, performance not under
Drop.
Embodiment two:
(1) preparation of seperation film:
Using the DMAC N,N' dimethyl acetamide (DMAc) of 15wt% cellulose acetates, 3% nano aluminium oxide and 85wt%
It is well mixed, vacuumize, the knifing on non-woven fabrics, in coagulation bath after film forming, crosslinking obtains solvent resistant in glutaraldehyde solution
Milipore filter.
(2) apply
Processing solution is 1g/L PEG1000 solution, wherein containing 30% DMAc.When external pressure is 0.1MPa, separation
Film is 92% to PEG1000 rejection, and water flux is 176L/m2h.Film is in continuous run 30 days, and performance does not decline.
Embodiment three:
(1) preparation of seperation film:
Uniformly mixed using 16wt% cellulose acetates and 84% DMAc, standing knifing through deaeration prepares acetate fiber
Plain milipore filter.It is crosslinked using 5% epoxypropyltrimethylchloride chloride and modification, preparing has high-throughout fiber
Plain sodium filter membrane.
(2) apply
Processing solution is 1g/L MgCl2Solution, wherein containing 10% DMAc.When external pressure is 0.3MPa, seperation film
Rejection to inorganic ion is 75%, and water flux is 27L/m2h。
Claims (8)
1. a kind of solvent resistant NF membrane, it is characterised in that the described integrated flat board of solvent resistant NF membrane or doughnut are resistance to
Solvent nanofiltration film;Described integral flat or hollow fiber nanofiltration membrane are to be spread out by cellulose series derivates, chitosan series
Biology, polyethyleneimine, sulfonated polyether sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethane
What base polysulfones, chloromethylation polyether-ketone, chloromethylation PPSU or polyacrylonitrile were formed, its thickness is 50~500 μm, aperture
For 0~100nm.
2. a kind of solvent resistant NF membrane, it is characterised in that described solvent resistant NF membrane includes separating. functional layer and supporting layer, branch
Layer is supportted to be located at below separating. functional layer;
Described separating. functional layer is by cellulose series derivates, chitosan series derivates, polyethyleneimine, sulfonated polyether
Sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethyl polysulphone, chloromethylation polyether-ketone,
Chloromethylation PPSU or the dense film or perforated membrane of polyacrylonitrile formation, thickness is 1~20 μm, and aperture is 0~100nm;
Described supporting layer is by cellulose series derivates, chitosan series derivates, polyvinyl alcohol or polyacrylamide shape
Into, its thickness is 50~500 μm, and aperture is 0~100nm.
3. solvent resistant NF membrane according to claim 2, it is characterised in that inorganic receive is introduced in described separating. functional layer
Organic-inorganic hybrid films formed by rice additive, inorganic nano additive includes nano silicon oxide, aluminum oxide, titanium oxide, four
Fe 3 O, lanthanum-strontium ferro-cobalt, molecular sieve, graphene and inorganic salts.
4. solvent resistant NF membrane according to claim 3, it is characterised in that added in described supporting layer 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.
5. the preparation method of the solvent resistant NF membrane described in a kind of claim 1, it is characterised in that step is as follows:
Prepare integrated solvent resistant flat board or hollow fiber nanofiltration membrane
Inorganic nano additive, macromolecule organic material and solvent are mixed, mixed solution or dispersion liquid is obtained, inorganic add is controlled
Plus the quality of agent very concentration is that 0~12wt%, the quality very concentration of macromolecule organic material are 8~20wt% and molten
The quality of agent very concentration is 68~85wt%;Above-mentioned mixed solution or homogeneous dispersion are coated on non-woven fabrics or used
Spinning mode is weaved on non-woven fabrics, and the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film;Then adopt
Crosslinking Treatment is carried out with crosslinking agent, crosslinking temperature is 10-120 DEG C, and crosslinking time is 1-30 minutes, is then immersed in deionized water
In, that is, obtain the solvent resistant NF membrane of integrated solvent resistant flat board or doughnut.
6. the preparation method of the solvent resistant NF membrane described in a kind of claim 4, it is characterised in that step is as follows:
(1) support membrane of solvent resistant NF membrane is prepared
Inorganic additive, macromolecule organic material A and solvent are mixed, mixed solution A or dispersion liquid A is obtained;Wherein, it is inorganic to add
Plus the quality of agent very concentration be 0~12wt%, the quality very concentration of macromolecule organic material be 8~20wt%, it is molten
The quality of agent very concentration is 68~85wt%;By above-mentioned mixed solution or homogeneous dispersion it is smooth scrape on non-woven fabrics/or
By the way of spinning, the mode for being then immersed in coagulating bath or solvent evaporated obtains preliminary seperation film;Then use crosslinking agent
Crosslinking Treatment is carried out, crosslinking time is 1-30min, and crosslinking temperature is 10-120 DEG C, then soaks in deionized water, obtains resistance to molten
The support membrane of agent NF membrane;
Described macromolecule organic material A includes cellulose series derivates, chitosan series derivates, polyvinyl alcohol and poly- third
Acrylamide;
(2) separating. functional layer of solvent resistant NF membrane is prepared
Inorganic additive, macromolecule organic material B and solvent are mixed, mixed solution B or dispersion liquid B is obtained;It is wherein inorganic to add
Plus the quality of agent very concentration be 0~2wt%, the quality very concentration of macromolecule organic material be 0.3~5wt%, it is molten
The quality of agent very concentration is 83~98wt%;One layer of mixed solution B of blade coating or scattered on support membrane prepared by step (1)
Liquid B, after heat treatment, obtains solvent resistant NF membrane;Heat treatment temperature is 20-80 DEG C, and heat treatment time is 5-50min;
Described macromolecule organic material B includes cellulose series derivates, chitosan series derivates, polyethyleneimine, sulphur
Change polyether sulfone, SPSF, sulfonated polyphenyl sulfone, sulfonated polyether ketone, chloromethylation polyether sulfone, chloromethyl polysulphone, chloromethylation
Polyether-ketone, chloromethylation PPSU and polyacrylonitrile;
(3) the solvent resistant NF membrane for preparing step (2) is immersed in cross-linking agent solution, and soak time is 5s-300s, leaching
It is 10-60 DEG C to steep temperature;Then crosslinking temperature be 10-100 DEG C under the conditions of, be crosslinked 1-30 minutes, after be immersed in deionized water, i.e.,
The solvent resistant NF membrane that must stablize.
7. the preparation method according to claim 5 or 6, it is characterised in that described crosslinking agent be the concentrated sulfuric acid, trimethylamine,
Ethylenediamine, triethylene tetramine, polyethyleneimine, glutaraldehyde, pyromellitic trimethylsilyl chloride, paraphthaloyl chloride, o-phthaloyl chloride, ring
Oxygen chloropropane, pentaerythrite, ethylene glycol or glycerine.
8. the preparation method according to claim 5 or 6, it is characterised in that described solvent be DMA,
N,N-dimethylformamide, dimethyl sulfoxide (DMSO) or 1-METHYLPYRROLIDONE.
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CN109745874A (en) * | 2019-03-15 | 2019-05-14 | 福州大学 | A kind of preparation method of chloromethyl polyether-ketone antipollution ultrafiltration membrane |
CN110052178A (en) * | 2019-05-23 | 2019-07-26 | 中国科学院长春应用化学研究所 | A kind of high tolerance organic solvent seperation film and preparation method thereof |
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