CN106512728A - Preparing method of anti-pollution super-thin nanofiltration membrane - Google Patents
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- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
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Abstract
The invention relates to a preparing method of an anti-pollution super-thin nanofiltration membrane. The method comprises the steps of 1,adopting a polymer ultrafiltration membrane as a basilemma, and covering a porous carrier layer on the surface of the basilemma; 2, conducting ion treatment on the basilemma covered by the porous carrier layer; 3, preparing the nanofiltration membrane with the ion-treated basilemma; 4, coating a protective layer on the outer surface of the nanofiltration membrane, and obtaining the anti-pollution super-thin nanofiltration membrane. According to the preparing method of the anti-pollution super-thin nanofiltration membrane, the basilemma is pretreated through ion treatment technology, so that the basilemma has a polyanionic membrane layer and a polycation-membrane layer, and has preliminary nanofiltration membrane performance; then by subsequent processing, the nanofiltration membrane is more efficient.
Description
Technical field
The present invention relates to a kind of preparation method of resistant to pollution ultra-thin NF membrane, belongs to filter plant technical field.
Background technology
NF membrane：In more than 1nm, general 1-2nm is to allow solvent molecule or some low molecular weight solutes or low price in aperture
A kind of functional semipermeable membrane of ion permeable.It is a kind of special and up-and-coming seperation film kind, and it is because retaining
The size of material is about nanometer and gains the name, and it is about 150-500 or so that it retains the molecular weight of Organic substance, retains dissolubility salt
Ability be, between 2-98%, high-valence anion saline solution to be less than to the desalination of monovalent anion saline solution.It is used to remove ground
The Organic substance of table water and colourity, remove underground hardness of water, and part removes dissolubility salt, in concentrated fruit juice and separation medicine
Utility etc..
NF membrane is the key of nanofiltration process, and requirement of the nanofiltration to membrane material is：With good film property, thermally-stabilised
Property, chemical stability, high mechanical strength, acid and alkali-resistance and microbial attack, chlorine-resistant and other oxidizing substances, have high water flux and
High salt rejection rate, anticol body and suspended solid pollutant, low price and the NF membrane for adopting mostly are aromatic series and polyacids hydrogen species are compound
NF membrane.Composite membrane is anisotropic membrane, is made up of two-part structure：A part is passive perforated membrane, and its mechanism is
Sieving actoion;Another part has been the dense film of the layer of centrifugation, and its separating mechanism can be entered with dissolve-diffusion model
Row is explained.For composite membrane, the optimization of material and structure can be carried out to the epidermal area of a centrifugation and supporting layer respectively, can
The composite membrane of excellent.The form of membrane module has doughnut, rolling, plate and frame and tubular type etc..Wherein, doughnut
It is high with the packed density of rolled membrane module, low cost, in component, hydrodynamic conditions are good;But the manufacture skill of both membrane modules
Art has high demands, and sealing is difficult, and in use, contamination resistance is poor, high to feed liquid pre-processing requirements.And plate and frame and tubular membrane component
Although easy to clean, anti-pollution, the packed density of film is low, cost is high.Therefore, it is in nanofiltration system to use hollow fiber form more
Or rolled membrane module.
The content of the invention
The technical problem to be solved in the present invention is, not enough for prior art, proposes a kind of with impurity screening function, energy
The preparation method of the resistant to pollution ultra-thin NF membrane of nanofiltration membrane pollution is prevented enough.
The present invention is that the technical scheme for solving above-mentioned technical problem proposition is：A kind of preparation of resistant to pollution ultra-thin NF membrane
Method, comprises the following steps：
(i). polymer ultrafiltration membrane is adopted for basement membrane, cover porous carrier layer in membrane surface；
In described polymer ultrafiltration membrane material, the mass percent of each composition is：Polyether sulfone：1.33-2.45%, polycaprolactam
Amine：2.13-3.15%, polypropylene：0.56-0.87%, polyethylene：0.41-0.66%, Kynoar：3.73-4.15%, acetic acid
Cellulose：2.45-3.11%, cellulose diacetate：1.73-2.33%, Triafol T：1.33-1.56%, cellulose propionate：
0.35-0.47%, cellulose butyrate：2.36-3.67%, cellulose acetate propionate：1.55-1.86%, two cellulose butyrates：0.21-
0.32%th, three cellulose butyrate：1.13-1.48%, Polyurethane：0.82-1.26%, polrvinyl chloride：0.53-0.75%, sulfonation polyamides
Imines：1.42-1.66%, sulfonated polyether sulfone：1.47-1.65%, polybenzimidazoles：0.23-0.34%, balance of polyacrylonitrile；
(ii). the basement membrane covered after porous carrier layer is carried out into ion processing, it is specific as follows：
A, the process of polyanion solution：Basement membrane is immersed into Sodium Polystyrene Sulfonate solution of the concentration for 0.05-0.2mol/L, control
The pH value of solution be 3-5, impregnate 25-30 minutes, after use pure water；
B, said polycation solution process：The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.05-0.2mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water；
(iii). NF membrane is prepared with the basement membrane after ion processing, concrete grammar is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng
Sour potassium, stirs, and is heated to 45～50 DEG C in being placed on water bath with thermostatic control, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, heat up in water bath with thermostatic control
To 95-100 DEG C, 25-30 minutes are stirred, add hydrogen peroxide solution to the solution that mass fraction is 25% after natural cooling and be changed into bright
The suspension of yellow；
C. suspension obtained by step B is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality
Ultrasonic disperse centrifugally operated in pure water, supernatant are placed in 65～75 DEG C of drying bakers and dry to obtain graphene oxide powder；
D. in step C, gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent, removes supernatant, obtain after centrifugation
To graphene oxide solution；
E. graphene oxide solution is filtered using the basement membrane after ion processing, constantly promote under 0.05-0.5MPa static pressures
Graphene oxide solution makes solvent molecule pass through basement membrane, and the NF membrane of moistening is obtained；
F. and then by obtained NF membrane in E it is immersed in the organic phase solution containing polynary acyl chlorides monomer, reacts 0.5～2 point
Clock, by interfacial polymerization, forms one layer of polyamide functional layer containing amphion group on NF membrane surface；
G. it is last, by above-mentioned NF membrane at 40～65 DEG C heat treatment 45～60 minutes, rinsed using distilled water；
H. the NF membrane moistened after rinsing is placed in vacuum drying oven and is dried；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive
Filter membrane reaction is dried in being placed in vacuum drying oven, and resistant to pollution ultra-thin NF membrane is obtained.
The improvement of above-mentioned technical proposal is：Porous carrier layer by the one kind in textile fabric, adhesive-bonded fabric and microporous membrane or
Various compositions.
The improvement of above-mentioned technical proposal is：The step of preparation method, (iii) polar solvent was water or alcohols in middle operation D.
The improvement of above-mentioned technical proposal is：The step of preparation method (i) in polymer ultrafiltration membrane material in each composition
Mass percent be：Polyether sulfone：1.33%th, polycaprolactam：3.15%th, polypropylene：0.56%th, polyethylene：0.66%th, gather inclined fluorine
Ethylene：4.15%th, cellulose acetate：2.45%th, cellulose diacetate：1.73%th, Triafol T：1.56%th, cellulose propionate：
0.47%th, cellulose butyrate：2.36%th, cellulose acetate propionate：1.86%th, two cellulose butyrate：0.21%th, three cellulose butyrate：
1.13%th, Polyurethane：0.82%th, polrvinyl chloride：0.75%th, sulfonated polyimide：1.42%th, sulfonated polyether sulfone：1.65%th, polyphenyl is simultaneously
Imidazoles：0.23%, balance of polyacrylonitrile.
The present invention using the beneficial effect of above-mentioned technical proposal is：
（1）Basement membrane is carried out pretreatment by ion processing technique by the present invention so that is had polyanion film layer on basement membrane and is gathered
Cation film layer, is provided with preliminary nanofiltration film properties, then by subsequent treatment so that nanofiltration membrane it is more efficient, and
And it is thinner；
（2）The preparation method of the resistant to pollution ultra-thin NF membrane of the present invention is due to being combined with basement membrane using porous carrier layer and being covered
Lid protective layer, enhances the structural strength and service life of NF membrane while nanofiltration efficiency is ensured, extends use time,
Reduce cost；
（3）The preparation method of the resistant to pollution ultra-thin NF membrane of the present invention also has to ion due to graphene oxide interlamellar spacing very well
Crown_interception, the oxygen-containing functional group on its surface can also increase hydrophilic, and then make film possess good permeability and rejection,
So that the filtration of NF membrane is more efficient；
（4）The preparation method of the resistant to pollution ultra-thin NF membrane of the present invention a large amount of free carboxyls as the film surface of NF membrane has
And hydroxyl, with high-hydrophilic, high-throughout feature, while film surface bear is electric, salt-stopping rate can be effectively improved, so as to significantly carry
The flux and desalting effect of high NF membrane, substantially increases strainability, with good heavy industrialization application prospect；
（5）The preparation method of the resistant to pollution ultra-thin NF membrane of the present invention is immersed in containing polynary acyl chlorides monomer due to NF membrane
In organic phase solution, react 0.5～2 minute, by interfacial polymerization, one layer is formed on NF membrane surface and contain amphion group
Polyamide functional layer, by high-hydrophilic, high flux the characteristics of amphion hydrophilic and resistance tocrocking with carboxyl and hydroxyl
The characteristics of effectively combine, obtained resistant to pollution ultra-thin NF membrane high working efficiency and with excellent resistance tocrocking.
Specific embodiment
Embodiment
The preparation method of the resistant to pollution ultra-thin NF membrane of the present embodiment, the preparation method of nanofiltration layer are comprised the following steps：
(i). polymer ultrafiltration membrane is adopted for basement membrane, cover porous carrier layer in membrane surface；
In described polymer ultrafiltration membrane material, the mass percent of each composition is：Polyether sulfone：1.33%th, polycaprolactam：
3.15%th, polypropylene：0.56%th, polyethylene：0.66%th, Kynoar：4.15%th, cellulose acetate：2.45%th, diacetate fiber
Element：1.73%th, Triafol T：1.56%th, cellulose propionate：0.47%th, cellulose butyrate：2.36%th, cellulose acetate propionate：
1.86%th, two cellulose butyrate：0.21%th, three cellulose butyrate：1.13%th, Polyurethane：0.82%th, polrvinyl chloride：0.75%th, sulfonation
Polyimides：1.42%th, sulfonated polyether sulfone：1.65%th, polybenzimidazoles：0.23%, balance of polyacrylonitrile；
(ii). the basement membrane covered after porous carrier layer is carried out into ion processing, it is specific as follows：
A, the process of polyanion solution：Basement membrane is immersed into Sodium Polystyrene Sulfonate solution of the concentration for 0.05-0.2mol/L, control
The pH value of solution be 3-5, impregnate 25-30 minutes, after use pure water；
B, said polycation solution process：The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.05-0.2mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water；
(iii). NF membrane is prepared with the basement membrane after ion processing, concrete grammar is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng
Sour potassium, stirs, and is heated to 45～50 DEG C in being placed on water bath with thermostatic control, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, heat up in water bath with thermostatic control
To 95-100 DEG C, 25-30 minutes are stirred, add hydrogen peroxide solution to the solution that mass fraction is 25% after natural cooling and be changed into bright
The suspension of yellow；
C. suspension obtained by step B is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality
Ultrasonic disperse centrifugally operated in pure water, supernatant are placed in 65～75 DEG C of drying bakers and dry to obtain graphene oxide powder；
D. in step C, gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent, removes supernatant, obtain after centrifugation
To graphene oxide solution；
E. graphene oxide solution is filtered using the basement membrane after ion processing, constantly promote under 0.05-0.5MPa static pressures
Graphene oxide solution makes solvent molecule pass through basement membrane, and the NF membrane of moistening is obtained；
F. and then by obtained NF membrane in E it is immersed in the organic phase solution containing polynary acyl chlorides monomer, reacts 0.5～2 point
Clock, by interfacial polymerization, forms one layer of polyamide functional layer containing amphion group on NF membrane surface；
G. it is last, by above-mentioned NF membrane at 40～65 DEG C heat treatment 45～60 minutes, rinsed using distilled water；
H. the NF membrane moistened after rinsing is placed in vacuum drying oven and is dried；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive
Filter membrane reaction is dried in being placed in vacuum drying oven, and resistant to pollution ultra-thin NF membrane is obtained.
In the preparation method：Porous carrier layer is made up of one or more in textile fabric, adhesive-bonded fabric and microporous membrane.
In the preparation method, (iii) polar solvent is water or alcohols to step in middle operation D.
The present invention is not limited to above-described embodiment.The technical scheme that all employing equivalents are formed, all falling within the present invention will
The protection domain asked.
Claims (4)
1. a kind of preparation method of resistant to pollution ultra-thin NF membrane, it is characterised in that：Comprise the following steps：
(i). polymer ultrafiltration membrane is adopted for basement membrane, cover porous carrier layer in membrane surface；
In described polymer ultrafiltration membrane material, the mass percent of each composition is：Polyether sulfone：1.33-2.45%, polycaprolactam
Amine：2.13-3.15%, polypropylene：0.56-0.87%, polyethylene：0.41-0.66%, Kynoar：3.73-4.15%, acetic acid
Cellulose：2.45-3.11%, cellulose diacetate：1.73-2.33%, Triafol T：1.33-1.56%, cellulose propionate：
0.35-0.47%, cellulose butyrate：2.36-3.67%, cellulose acetate propionate：1.55-1.86%, two cellulose butyrates：0.21-
0.32%th, three cellulose butyrate：1.13-1.48%, Polyurethane：0.82-1.26%, polrvinyl chloride：0.53-0.75%, sulfonation polyamides
Imines：1.42-1.66%, sulfonated polyether sulfone：1.47-1.65%, polybenzimidazoles：0.23-0.34%, balance of polyacrylonitrile；
(ii). the basement membrane covered after porous carrier layer is carried out into ion processing, it is specific as follows：
A, the process of polyanion solution：Basement membrane is immersed into Sodium Polystyrene Sulfonate solution of the concentration for 0.05-0.2mol/L, control
The pH value of solution be 3-5, impregnate 25-30 minutes, after use pure water；
B, said polycation solution process：The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.05-0.2mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water；
(iii). NF membrane is prepared with the basement membrane after ion processing, concrete grammar is comprised the following steps：
A. it is that 98% concentrated sulphuric acid adds into expansible graphite raw material by mass fraction in 0 DEG C of ice-water bath, is slowly added Gao Meng
Sour potassium, stirs, and is heated to 45～50 DEG C in being placed on water bath with thermostatic control, keeps 0.5-2h；
B. deionized water is slowly added dropwise in resulting solution in step A to produce to reaction system bubble-free, heat up in water bath with thermostatic control
To 95-100 DEG C, 25-30 minutes are stirred, add hydrogen peroxide solution to the solution that mass fraction is 25% after natural cooling and be changed into bright
The suspension of yellow；
C. suspension obtained by step B is filtered into obtain brown color colloid, Jing pickling and deionized water wash are dried after super to neutrality
Ultrasonic disperse centrifugally operated in pure water, supernatant are placed in 65～75 DEG C of drying bakers and dry to obtain graphene oxide powder；
D. in step C, gained graphene oxide powder is placed in ultrasonic disperse 1-5h in polar solvent, removes supernatant, obtain after centrifugation
To graphene oxide solution；
E. graphene oxide solution is filtered using the basement membrane after ion processing, constantly promote under 0.05-0.5MPa static pressures
Graphene oxide solution makes solvent molecule pass through basement membrane, and the NF membrane of moistening is obtained；
F. and then by obtained NF membrane in E it is immersed in the organic phase solution containing polynary acyl chlorides monomer, reacts 0.5～2 point
Clock, by interfacial polymerization, forms one layer of polyamide functional layer containing amphion group on NF membrane surface；
G. it is last, by above-mentioned NF membrane at 40～65 DEG C heat treatment 45～60 minutes, rinsed using distilled water；
H. the NF membrane moistened after rinsing is placed in vacuum drying oven and is dried；
(iv). it is armor coated in nanofiltration film layer outer surface, the protective layer adopt concentration for 11-15% PVA aqueous solutions with receive
Filter membrane reaction is dried in being placed in vacuum drying oven, and resistant to pollution ultra-thin NF membrane is obtained.
2. the preparation method of resistant to pollution ultra-thin NF membrane according to claim 1, it is characterised in that：The porous carrier
Layer is made up of one or more in textile fabric, adhesive-bonded fabric and microporous membrane.
3. the preparation method of resistant to pollution ultra-thin NF membrane according to claim 2, it is characterised in that：The preparation method
The step of (iii) polar solvent is water or alcohols in middle operation D.
4. the preparation method of resistant to pollution ultra-thin NF membrane according to claim 3, it is characterised in that：The preparation method
The step of (i) in polymer ultrafiltration membrane material in the mass percent of each composition be：Polyether sulfone：1.33%th, polycaprolactam：
3.15%th, polypropylene：0.56%th, polyethylene：0.66%th, Kynoar：4.15%th, cellulose acetate：2.45%th, diacetate fiber
Element：1.73%th, Triafol T：1.56%th, cellulose propionate：0.47%th, cellulose butyrate：2.36%th, cellulose acetate propionate：
1.86%th, two cellulose butyrate：0.21%th, three cellulose butyrate：1.13%th, Polyurethane：0.82%th, polrvinyl chloride：0.75%th, sulfonation
Polyimides：1.42%th, sulfonated polyether sulfone：1.65%th, polybenzimidazoles：0.23%, balance of polyacrylonitrile.
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Cited By (6)
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| CN106861465A (en) * | 2017-03-31 | 2017-06-20 | 深圳市国创新能源研究院 | A kind of antipollution combined oxidation Graphene NF membrane and preparation method thereof |
| CN110252155A (en) * | 2019-06-20 | 2019-09-20 | 西华大学 | A kind of pollution-resistant multi-walled carbon nano-tube composite membrane and preparation method thereof |
| CN112058097A (en) * | 2020-05-15 | 2020-12-11 | 山东水发环境科技有限公司 | Preparation method of forward osmosis membrane material |
| CN112295418A (en) * | 2019-07-30 | 2021-02-02 | 上海恩捷新材料科技有限公司 | Polyethylene-based composite graphene oxide nanofiltration membrane and preparation method thereof |
| CN112449614A (en) * | 2018-06-21 | 2021-03-05 | 日东电工株式会社 | Selectively permeable graphene oxide membranes for gas dehydration |
| CN113877447A (en) * | 2021-11-18 | 2022-01-04 | 康膜科技有限公司 | Preparation technology of high-efficiency intrinsically-stable full-aromatic polyamide reverse osmosis membrane with high crosslinking degree |
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| CN106861465A (en) * | 2017-03-31 | 2017-06-20 | 深圳市国创新能源研究院 | A kind of antipollution combined oxidation Graphene NF membrane and preparation method thereof |
| CN112449614A (en) * | 2018-06-21 | 2021-03-05 | 日东电工株式会社 | Selectively permeable graphene oxide membranes for gas dehydration |
| CN110252155A (en) * | 2019-06-20 | 2019-09-20 | 西华大学 | A kind of pollution-resistant multi-walled carbon nano-tube composite membrane and preparation method thereof |
| CN112295418A (en) * | 2019-07-30 | 2021-02-02 | 上海恩捷新材料科技有限公司 | Polyethylene-based composite graphene oxide nanofiltration membrane and preparation method thereof |
| CN112058097A (en) * | 2020-05-15 | 2020-12-11 | 山东水发环境科技有限公司 | Preparation method of forward osmosis membrane material |
| CN113877447A (en) * | 2021-11-18 | 2022-01-04 | 康膜科技有限公司 | Preparation technology of high-efficiency intrinsically-stable full-aromatic polyamide reverse osmosis membrane with high crosslinking degree |
| CN113877447B (en) * | 2021-11-18 | 2023-11-10 | 康膜科技有限公司 | Preparation technology of high-efficiency intrinsically stable type wholly aromatic polyamide reverse osmosis membrane with high crosslinking degree |
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