CN106512732A - Preparation method of ultrathin reverse osmosis membrane - Google Patents
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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
- B01D61/025—Reverse osmosis; Hyperfiltration
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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
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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
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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
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
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- 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
- B01D71/12—Cellulose derivatives
- B01D71/14—Esters of organic acids
- B01D71/16—Cellulose acetate
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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
- B01D71/26—Polyalkenes
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
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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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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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
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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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
- B01D71/48—Polyesters
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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
- B01D71/56—Polyamides, e.g. polyester-amides
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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
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a preparation method of an ultrathin reverse osmosis membrane. The preparation method includes following steps: 1, adopting a macromolecular ultrafiltration membrane as a base membrane, and covering the surface of the base membrane with a porous carrier layer; 2, performing ion treatment on the base membrane; 3, soaking the base membrane in a mixed water solution of metaphenylene diamine and ethanol amine to obtain a wet membrane; 4, soaking the wet membrane in an oil phase tank of a normal hexane solution containing trimesoyl chloride as an additive for polymerization reaction; 5, dipping and coating a polyethylene glycol polyelectrolyte water solution on the surface of the base membrane after being dried; 6, soaking the base membrane in a PVA water solution, and forming a protection layer on the surface of the base membrane; 7, putting the base membrane in a vacuum dryer for heating and drying to obtain the ultrathin reverse osmosis membrane. The macromolecular ultrafiltration membrane is soaked by the mixed water solution of metaphenylene diamine and ethanol amine, so that water flux of the reverse osmosis membrane is improved greatly; the ultrathin reverse osmosis membrane is higher than existing reverse osmosis membrane in desalting rate, and the preparation method is simple.
Description
Technical field
The present invention relates to a kind of preparation method of ultra-thin reverse osmosis membrane, belongs to filter plant technical field.
Background technology
Water is Source of life, and water occupies the 70% of human body ingredient, therefore, the quality of drinking water directly decides people
The health of body.With the development of modern industry, especially water body all receives pollution in varying degrees to environment, it is general originally
Water directly cannot be drunk, for this purpose, people drink bottled water mostly at present.
Although drinking bottled water than direct drinking public water supply health, however, bottled water price is than tap water price, into
This increase, and as bottled water is stagnant water, when overlong time is put, the water capacity easily receives secondary pollution, people to drink these and received
After the water of pollution, can cause uncomfortable, affect healthy;Also various water purifiers are had on the market at present,
However, its structure of a variety of water purifier is complicated in the extreme, expensive, and it is not to manage very much to the filter effect of tap water
Think.To sum up, current people are faced with and drink up the difficult problem of safe drinking water.
At present, start to obtain clean water source using reverse osmosis technology where more and more, reverse osmosis technology is to adopt
The water technology of membrane separating, is that the inverse process of phenomenon of osmosis in nature (is overcome with extraneous motive force to the water of saliferous and oozed
Press thoroughly and make reverse osmosis process of the hydrone by film).Anti-penetration wastewater disposal technique substantially belongs to physics desalination process, it
All many-sided with traditional unexistent advantage of method for treating water.Generally, reverse osmosis unit (reverse osmose pure-water system)
It is with reverse osmosis membrane as core, including the defecators at different levels in front and back including force (forcing) pump, water butt and reverse osmosis membrane device, raw water
After each filtration system is processed for users to use., there is mostly filtration, purification not thorough enough in current reverse osmosis water purifier
The problem at bottom.
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 the ultra-thin of good purification
The preparation method of reverse osmosis membrane.
The present invention is that the technical scheme for solving above-mentioned technical problem proposition is:A kind of preparation side of ultra-thin reverse osmosis 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:3.33-3.45%, polycaprolactam
Amine:1.13-1.65%, polypropylene:1.56-1.87%, Kynoar:2.43-3.05%, cellulose diacetate:1.23-
1.63%th, Triafol T:2.33-2.56%, cellulose propionate:1.35-1.47%, cellulose butyrate:0.36-0.67%, vinegar
Sour cellulose propionate:2.55-2.86%, two cellulose butyrates:1.21-1.32%, Polyurethane:1.82-2.16%, polrvinyl chloride:
0.63-0.85%, sulfonated polyimide:0.46-0.86%, sulfonated polyether sulfone:2.17-2.35%, polybenzimidazoles:0.13-
0.24%, 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 0.02-0.09mol/L, control
The pH value of solution processed be 4-6, impregnate 35-40 minutes, after use pure water;
B, said polycation solution process:The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.02-0.09mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water;
(iii) 15-30 minutes in the mixed aqueous solution of basement membrane immersion m-diaminobenzene. and ethanolamine after ion processing are obtained into wet film,
Wherein the concentration of m-diaminobenzene. is 1.2-1.6g/L, and the concentration of ethanolamine is 1.3-1.7g/L;
(iv) by 35-55 in the oil phase groove of the hexane solution of above-mentioned wet film pyromellitic trimethylsilyl chloride of the immersion containing a certain amount of additive
Minute carries out polyreaction;
The mass percent of the wherein each component of additive is:Tbp:0.24-0.56%, triphenylphosphine:0.58-
0.77%th, acetone:1.57-1.96%, aluminium acetylacetonate:2.24-2.55%, nickel acetylacetonate:0.56-1.04%, levulinic
Ketone ferrum:0.56-0.93%, chromium acetylacetonate:1.27-2.13%, balance of acetylacetone,2,4-pentanedione gallium;
(v) the above-mentioned wet film carried out after polyreaction is put in vacuum drier and is thermally dried, setting temperature is 43-55
Degree Celsius, the time is 1.5-3 hours;The uniform dip-coating of Polyethylene Glycol polyelectrolyte aqueous solution base after the drying is dipped with Glass rod
Film surface, is placed in 0.5-1 hours in 50-70 DEG C of baking oven afterwards, obtains being coated with the basement membrane of Polyethylene Glycol polyelectrolyte;
(vi) above-mentioned basement membrane is immersed into 5-15 minutes in PVA aqueous solutions of the concentration for 17-19%, membrane surface forms protective layer;Will
The base filter membrane of dipped PVA aqueous solutions is cleaned in sending into ultrasonic washing unit;
(vii) the basement membrane after cleaning is put in vacuum drier and is thermally dried, it is 45-60 degree Celsius to arrange temperature, and the time is
1.5-3 hours, are obtained ultra-thin reverse osmosis membrane.
The improvement of above-mentioned technical proposal is:The step of preparation method (i) in middle polymer ultrafiltration membrane material each composition quality
Percentage ratio is:Polyether sulfone:3.33%th, polycaprolactam:1.65%th, polypropylene:1.87%th, Kynoar:2.43%th, two acetic acid are fine
Dimension element:1.23%th, Triafol T:2.56%th, cellulose propionate:1.35%th, cellulose butyrate:0.67%th, acetate propionate fiber
Element:2.86%th, two cellulose butyrate:1.21%th, Polyurethane:2.16%th, polrvinyl chloride:0.63%th, sulfonated polyimide:0.46%th, sulphur
Change polyether sulfone:2.35%th, polybenzimidazoles:0.13%, balance of polyacrylonitrile.
The improvement of above-mentioned technical proposal is:The step of preparation method, the mass percent of the (iv) each component of middle additive was:
Tbp:0.24%th, triphenylphosphine:0.77%th, acetone:1.96%th, aluminium acetylacetonate:2.24%th, nickel acetylacetonate:
0.56%th, ferric acetyl acetonade:0.93%th, chromium acetylacetonate:1.27%, balance of acetylacetone,2,4-pentanedione gallium.
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 reverse osmosiss performance, then by subsequent treatment so that reverse osmosis membrane filtration it is more efficient,
And it is thinner;
(2)The present invention is applied or dip-coating is in basement membrane using Polyethylene Glycol polyelectrolyte as the active layer material on reverse osmosis membrane surface
On surface, can cause the reverse osmosis membrane for preparing that there is high-hydrophilic and reverse osmosiss performance is improved;
(3)The preparation method of the ultra-thin reverse osmosis membrane of the present invention passes through the mixed aqueous solution of m-diaminobenzene. and ethanolamine to basement membrane
Soaked so that the water flux of reverse osmosis membrane is greatly enhanced, and the salt rejection rate of the permeable membrane of the present invention is anti-higher than existing
Permeable membrane, preparation process is simple;
(4)Basement membrane is immersed in PVA aqueous solutions when prepared by the preparation method of the ultra-thin reverse osmosis membrane of the present invention, obtained reverse osmosis
The surface of permeable membrane covers matcoveredn, extends the service life of reverse osmosis membrane.
Specific embodiment
Embodiment
The preparation method of the ultra-thin reverse osmosis membrane of the present embodiment, 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:3.33%th, polycaprolactam:
1.65%th, polypropylene:1.87%th, Kynoar:2.43%th, cellulose diacetate:1.23%th, Triafol T:2.56%th, third
Acid cellulose:1.35%th, cellulose butyrate:0.67%th, cellulose acetate propionate:2.86%th, two cellulose butyrate:1.21%th, polyamine
Ester:2.16%th, polrvinyl chloride:0.63%th, sulfonated polyimide:0.46%th, sulfonated polyether sulfone:2.35%th, polybenzimidazoles:0.13%,
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 0.02-0.09mol/L, control
The pH value of solution processed be 4-6, impregnate 35-40 minutes, after use pure water;
B, said polycation solution process:The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.02-0.09mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water;
(iii) 15-30 minutes in the mixed aqueous solution of basement membrane immersion m-diaminobenzene. and ethanolamine after ion processing are obtained into wet film,
Wherein the concentration of m-diaminobenzene. is 1.2-1.6g/L, and the concentration of ethanolamine is 1.3-1.7g/L;
(iv) by 35-55 in the oil phase groove of the hexane solution of above-mentioned wet film pyromellitic trimethylsilyl chloride of the immersion containing a certain amount of additive
Minute carries out polyreaction;
The mass percent of the wherein each component of additive is:Tbp:0.24%th, triphenylphosphine:0.77%th, acetone:
1.96%th, aluminium acetylacetonate:2.24%th, nickel acetylacetonate:0.56%th, ferric acetyl acetonade:0.93%th, chromium acetylacetonate:
1.27%, balance of acetylacetone,2,4-pentanedione gallium;
(v) the above-mentioned wet film carried out after polyreaction is put in vacuum drier and is thermally dried, setting temperature is 43-55
Degree Celsius, the time is 1.5-3 hours;The uniform dip-coating of Polyethylene Glycol polyelectrolyte aqueous solution base after the drying is dipped with Glass rod
Film surface, is placed in 0.5-1 hours in 50-70 DEG C of baking oven afterwards, obtains being coated with the basement membrane of Polyethylene Glycol polyelectrolyte;
(vi) above-mentioned basement membrane is immersed into 5-15 minutes in PVA aqueous solutions of the concentration for 17-19%, membrane surface forms protective layer;Will
The base filter membrane of dipped PVA aqueous solutions is cleaned in sending into ultrasonic washing unit;
(vii) the basement membrane after cleaning is put in vacuum drier and is thermally dried, it is 45-60 degree Celsius to arrange temperature, and the time is
1.5-3 hours, are obtained ultra-thin reverse osmosis membrane.
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 (3)
1. a kind of preparation method of ultra-thin reverse osmosis membrane, 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:3.33-3.45%, polycaprolactam
Amine:1.13-1.65%, polypropylene:1.56-1.87%, Kynoar:2.43-3.05%, cellulose diacetate:1.23-
1.63%th, Triafol T:2.33-2.56%, cellulose propionate:1.35-1.47%, cellulose butyrate:0.36-0.67%, vinegar
Sour cellulose propionate:2.55-2.86%, two cellulose butyrates:1.21-1.32%, Polyurethane:1.82-2.16%, polrvinyl chloride:
0.63-0.85%, sulfonated polyimide:0.46-0.86%, sulfonated polyether sulfone:2.17-2.35%, polybenzimidazoles:0.13-
0.24%, 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 0.02-0.09mol/L, control
The pH value of solution processed be 4-6, impregnate 35-40 minutes, after use pure water;
B, said polycation solution process:The basement membrane immersion concentration that polyanion solution was processed is the poly- of 0.02-0.09mol/L
In diallyldimethylammonium chloride solution, control solution pH value be 4-6, impregnate 25-30 minutes, after use pure water;
(iii) 15-30 minutes in the mixed aqueous solution of basement membrane immersion m-diaminobenzene. and ethanolamine after ion processing are obtained into wet film,
Wherein the concentration of m-diaminobenzene. is 1.2-1.6g/L, and the concentration of ethanolamine is 1.3-1.7g/L;
(iv) by 35-55 in the oil phase groove of the hexane solution of above-mentioned wet film pyromellitic trimethylsilyl chloride of the immersion containing a certain amount of additive
Minute carries out polyreaction;
The mass percent of the wherein each component of additive is:Tbp:0.24-0.56%, triphenylphosphine:0.58-
0.77%th, acetone:1.57-1.96%, aluminium acetylacetonate:2.24-2.55%, nickel acetylacetonate:0.56-1.04%, levulinic
Ketone ferrum:0.56-0.93%, chromium acetylacetonate:1.27-2.13%, balance of acetylacetone,2,4-pentanedione gallium;
(v) the above-mentioned wet film carried out after polyreaction is put in vacuum drier and is thermally dried, setting temperature is 43-55
Degree Celsius, the time is 1.5-3 hours;The uniform dip-coating of Polyethylene Glycol polyelectrolyte aqueous solution base after the drying is dipped with Glass rod
Film surface, is placed in 0.5-1 hours in 50-70 DEG C of baking oven afterwards, obtains being coated with the basement membrane of Polyethylene Glycol polyelectrolyte;
(vi) above-mentioned basement membrane is immersed into 5-15 minutes in PVA aqueous solutions of the concentration for 17-19%, membrane surface forms protective layer;Will
The base filter membrane of dipped PVA aqueous solutions is cleaned in sending into ultrasonic washing unit;
(vii) the basement membrane after cleaning is put in vacuum drier and is thermally dried, it is 45-60 degree Celsius to arrange temperature, and the time is
1.5-3 hours, are obtained ultra-thin reverse osmosis membrane.
2. the preparation method of ultra-thin reverse osmosis membrane according to claim 1, it is characterised in that:Described preparation method
(i) the mass percent of each composition is step in middle polymer ultrafiltration membrane material:Polyether sulfone:3.33%th, polycaprolactam:1.65%、
Polypropylene:1.87%th, Kynoar:2.43%th, cellulose diacetate:1.23%th, Triafol T:2.56%th, cellulose propionate
Element:1.35%th, cellulose butyrate:0.67%th, cellulose acetate propionate:2.86%th, two cellulose butyrate:1.21%th, Polyurethane:
2.16%th, polrvinyl chloride:0.63%th, sulfonated polyimide:0.46%th, sulfonated polyether sulfone:2.35%th, polybenzimidazoles:0.13%, it is remaining
Measure as polyacrylonitrile.
3. the preparation method of ultra-thin reverse osmosis membrane according to claim 2, it is characterised in that:Described preparation method
The mass percent of the step (iv) each component of middle additive is:Tbp:0.24%th, triphenylphosphine:0.77%th, acetone:
1.96%th, aluminium acetylacetonate:2.24%th, nickel acetylacetonate:0.56%th, ferric acetyl acetonade:0.93%th, chromium acetylacetonate:
1.27%, balance of acetylacetone,2,4-pentanedione gallium.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111359310A (en) * | 2020-02-21 | 2020-07-03 | 东营远洁环保科技有限公司 | Modified filter material for treating petroleum sewage |
CN114247298A (en) * | 2022-03-01 | 2022-03-29 | 湖南沁森高科新材料有限公司 | Post-treatment method for improving stability of reverse osmosis membrane and reverse osmosis membrane product |
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2016
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CN104474926A (en) * | 2014-12-12 | 2015-04-01 | 杭州水处理技术研究开发中心有限公司 | Preparation method of polyamide reverse osmosis membrane |
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JOUNG-EUN GU等: "Molecular Layer-by-Layer Assembled Thin-Film CompositeMembranes for Water Desalination", 《ADVANCED MATERIALS》 * |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111359310A (en) * | 2020-02-21 | 2020-07-03 | 东营远洁环保科技有限公司 | Modified filter material for treating petroleum sewage |
CN111359310B (en) * | 2020-02-21 | 2021-09-28 | 东营远洁环保科技有限公司 | Modified filter material for treating petroleum sewage |
CN114247298A (en) * | 2022-03-01 | 2022-03-29 | 湖南沁森高科新材料有限公司 | Post-treatment method for improving stability of reverse osmosis membrane and reverse osmosis membrane product |
CN114247298B (en) * | 2022-03-01 | 2022-07-12 | 湖南沁森高科新材料有限公司 | Post-treatment method for improving stability of reverse osmosis membrane and reverse osmosis membrane product |
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