CN108126530A - A kind of preparation method and reverse osmosis composite membrane of anti-pollution reverse-osmosis composite membrane - Google Patents
A kind of preparation method and reverse osmosis composite membrane of anti-pollution reverse-osmosis composite membrane Download PDFInfo
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- CN108126530A CN108126530A CN201711400593.0A CN201711400593A CN108126530A CN 108126530 A CN108126530 A CN 108126530A CN 201711400593 A CN201711400593 A CN 201711400593A CN 108126530 A CN108126530 A CN 108126530A
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- composite membrane
- osmosis composite
- antipollution
- polyacrylamide
- water
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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
- B01D69/12—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
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
-
- 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
-
- 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
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The present invention discloses a kind of preparation method of anti-pollution reverse-osmosis composite membrane, including:By polyamine aqueous phase solution and with aromatic polycarboxylic acyl chlorides organic phase solution polysulfones support film surface on contact and occur interface polymerization reaction formed aromatic polyamides desalination layer, prepared antipollution coating solution is coated in aromatic polyamides desalination layer, antipollution coating is formed after heat treatment, antipollution coating solution is the acidic mixed solution containing polyacrylamide, aldehydes.Further, the invention also discloses the anti-pollution reverse-osmosis composite membranes prepared in aforementioned manners.Crosslinked antipollution coating is formed in polyamide desalination layer surface by the present invention, the coating uniform is smooth and is not easy to elute, improve the service life of film, and pass through and select different electrical polyacrylamides, make anti-pollution reverse osmosis membrane surface electrical behavior controllable, widen the application field of reverse osmosis membrane obtained.
Description
Technical field
Patent of the present invention belongs to the composite membrane technology in water-treatment technology field, and in particular to a kind of anti-pollution reverse-osmosis is answered
The anti-pollution reverse-osmosis composite membrane for closing the preparation method of film and being prepared by this method.
Background technology
Reverse osmosis membrane is widely used in the necks such as electric power, petrochemical industry, steel, electronics, medicine, food and drink, municipal administration and environmental protection
Domain, in seawater and brackish water desalination, prepared by boiler feedwater, industrial pure water and electronic grade ultrapure water, drinking pure water production, waste water
It is played an important role during processing and special separation.Reverse osmosis membrane is generally made of polymer material, such as cellulose acetate
Film, aromatic polyhydrazide film, aromatic polyamide film etc..In actual application, reverse osmosis membrane need to have under a certain pressure
There are appropriate salt rejection rate and water flux, to reach this purpose, the reverse osmosis membrane of commercialization at present is largely composite membrane, mainly
Using porous polysulfones microporous barrier as supporting layer, polyamide desalination layer is prepared by the method for interfacial polymerization on its surface.
Reverse osmosis membrane performance mainly includes three performance indicators:Water flux, salt rejection rate, stability.High throughput can reduce
System investment and operating cost, equipment with high desalinization can improve producing water water quality, and stability refers to water yield and producing water water quality during film use
Stablize and weigh the important indicator of reverse osmosis membrane system performance driving economy.Influence film property stabilizability factor it is very much, such as into
Water condition, operating condition, fouling membrane etc., wherein fouling membrane influence more difficult to control.Fouling membrane normally behaves as one section of system operation
After time, flux depression, producing water water quality is deteriorated.Fouling membrane includes biological pollution, inorganic matter pollution and organic pollution.Occur
After fouling membrane, fouling membrane type need to be distinguished, is rinsed or pickling, alkali cleaning, these processes are restoring membrane flux and salt rejection rate
The service life of film can be shortened simultaneously.
The method of processing membrane pollution problem mainly has optimization pretreating process and selects anti-pollution reverse osmosis membrane at present.Wherein
The method for preparing anti-pollution reverse osmosis membrane mainly includes improving film surface slickness, hydrophily and selects suitable film surface electrical
To realize.
Invention content
The present invention is to solve the above problems, the present invention discloses a kind of compound membrane preparation method of anti-pollution reverse-osmosis and passes through
Anti-pollution reverse-osmosis composite membrane prepared by this method to improve the surface smoothness of reverse osmosis composite membrane, increases stain resistance, carries
High service life.
The present invention discloses a kind of preparation method of anti-pollution reverse-osmosis composite membrane, including:By polyamine aqueous phase solution and virtue
Fragrant polynary acyl chlorides organic phase solution contacts in polysulfones support film surface and interface polymerization reaction occurs, and forms aromatic polyamides and takes off
Salt deposit;Prepared antipollution coating solution is coated in aromatic polyamides desalination layer, after heat treatment crosslinks reaction, shape
Into antipollution coating;The antipollution coating solution is the acidic mixed solution containing polyacrylamide, aldehydes.
As a preferred embodiment, the polyacrylamide is selected from cationic-type polyacrylamide, anionic polypropylene
One or more of amide, neutral polyacrylamide.
As a preferred embodiment, the aldehydes is selected from one or more of formaldehyde, glyoxal, glutaraldehyde, hexandial.
As a preferred embodiment, the mass fraction of polyacrylamide is 0.05-2% in the antipollution coating solution, aldehyde
The mass fraction of class is 0.05-5%.
As a preferred embodiment, it is 2-6, the pH to control the pH value range of antipollution coating solution by pH adjusting agent
It is worth conditioning agent and is selected from one or more of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid.
As a preferred embodiment, also comprising additive, the additive is selected from poly- the solute of the antipollution coating solution
Ethylene glycol 400, cetomacrogol 1000, polyethylene glycol 2000, Macrogol 6000, polyethylene glycol 10000, PEG 20000,
The one or more of polyvinyl alcohol, mass fraction are not more than 2%.
As a preferred embodiment, the solvent of the antipollution coating solution is water or water and water soluble organic substance;In solvent
During for water and water soluble organic substance, the water soluble organic substance be selected from methanol, ethyl alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol,
One or more of tert-butyl alcohol, and mass fraction is not more than 3%.
As a preferred embodiment, the temperature of heat treatment is 80-120 DEG C, time 0.5-10min.
Invention additionally discloses a kind of anti-pollution reverse-osmosis composite membrane, including nonwoven layer, polysulfones support membrane, aromatic polyamides
Desalination layer and antipollution coating;For polysulfones support membrane coated in nonwoven layer, aromatic polyamides desalination layer is by polyamine water phase
Solution and aromatic polycarboxylic acyl chlorides organic phase solution are formed after interface polymerization reaction occurs in polysulfones support film surface, and antipollution applies
Layer is formed after reaction is crosslinked in heat treatment by the antipollution coating solution being coated in aromatic polyamides desalination layer;It is described
Antipollution coating solution is the acidic mixed solution containing polyacrylamide, aldehydes.
As a preferred embodiment, the solute of the antipollution coating solution be polyacrylamide, aldehydes and additive, solvent
For water or water and water soluble organic substance;The mass fraction of polyacrylamide is 0.05-2%, and the mass fraction of aldehydes is 0.05-
5%;The mass fraction of additive is 0-2%.
Compared with prior art, advantage of the invention is that:
(1) one layer of friendship is formed in polyamide desalination layer surface under conditions of pH is 2-6 by polyacrylamide and aldehydes
The antipollution coating of connection, the coating uniform is smooth and is not easy to elute, and improves the service life of film, widens reverse osmosis obtained significantly
The application field of permeable membrane.
(2) different electrical polyacrylamides can be selected, make anti-pollution reverse osmosis membrane surface electrical behavior obtained controllable, be applicable in
In different application field.
(3) anti-pollution reverse osmosis membrane produced by the present invention, with 25 DEG C of 2000ppm NaCl aqueous solutions, in pressure
It is tested under conditions of 1.55MPa, PH=7.5-8.0, salt rejection rate is more than 99.3%, and water flux is more than 45L/ (m2h), more conventional
Reverse osmosis membrane, performance obviously promoted.
(4) preparation method of anti-pollution reverse osmosis membrane of the present invention has relatively low equipment operation requirement, it can be achieved that industry is raw
The scale of production and continuity, and cost is relatively low.
Specific embodiment
Embodiment discloses the antipollution that a kind of preparation method of preferred reverse osmosis composite membrane and this method are prepared
Reverse osmosis composite membrane, the preparation method concrete operation step are:
Step 1:Prepare polysulfones support membrane:
Prior art preparation polysulfones support membrane can be used.Polysulfones (PSf), additive are dissolved in solvent, are configured to cast
Film liquid;Then it is cast on non-woven fabrics after filtering, deaeration;Gel in deionized water is immersed again, so as to which polysulfones support membrane be made.
Wherein:Additive for polyvinylpyrrolidone (PVP), polyethylene glycol (PEG), glycol monoethyl ether (EGME),
One or more of neopelex (SDBS), dodecyl sodium sulfate (SDS);Solvent is N, N- dimethyl formyls
Amine (DMF), DMAC N,N' dimethyl acetamide (DMAc), N-Methyl pyrrolidone (NMP), one kind in dimethyl sulfoxide (DMSO) (DMSO) or
It is several;Polysulfones mass fraction is 15-20% in casting solution, and additive mass fraction is 0.5-10%.
Step 2:Prepare aromatic polyamides desalination layer:
Prior art preparation can also be used in aromatic polycarboxylic acyl chlorides organic phase solution.Polysulfones support membrane made from step 1 is soaked
Enter in polyamine aqueous phase solution, after residence time 3-60 second, take out through extruding or air purging removal redundant solution;Support membrane
Side contacts with aromatic polycarboxylic acyl chlorides organic phase solution and interface polymerization reaction occurs;After being then placed in baking oven heat treatment, baking oven heat
Treatment temperature is 30-90 DEG C;It rinses, dry through deionized water again, to form aromatic polyamides desalination layer.
Wherein:Polyamine aqueous phase solution, solute is o-phenylenediamine, m-phenylene diamine (MPD), p-phenylenediamine, piperazine, triethylamine, second
One or more of diamines, Solute mass fraction 0.8-5%, solvent are water.Aromatic polycarboxylic acyl chlorides organic phase solution,
Its solute is one or more of pyromellitic trimethylsilyl chloride, m-phthaloyl chloride, paraphthaloyl chloride, and Solute mass fraction is
0.05-0.5%, solvent is n-hexane, in hexamethylene, normal heptane, normal octane, isooctane, dimethylbenzene, ISOPAR solvent naphthas
It is one or more of.
Step 3:Prepare antipollution coating
First, antipollution coating solution is prepared, antipollution coating solution is mainly by polyacrylamide, additive, aldehydes, pH value tune
Save agent and solvent composition.Wherein:
The solvent of antipollution coating solution is water, can also use water and water soluble organic substance according to demand, wherein, it is water-soluble
Organic matter is selected from one or more of methanol, ethyl alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol, tert-butyl alcohol, and water solubility has
The mass fraction of machine object is not more than 3%.Polyacrylamide be selected from cationic-type polyacrylamide, anion-polyacrylamide,
One or more of neutral polyacrylamide, the mass fraction of polyacrylamide is 0.05-2% in antipollution coating solution.Add
Agent is added to be selected from polyethylene glycol 400, cetomacrogol 1000, polyethylene glycol 2000, Macrogol 6000, polyethylene glycol 10000, poly- second
One or more of glycol 20000, polyvinyl alcohol, the mass fraction of additive is 0-2% in antipollution coating solution.Aldehydes selects
From one or more of formaldehyde, glyoxal, glutaraldehyde, hexandial, the mass fraction of the aldehydes in antipollution coating solution is
0.05-5%.PH adjusting agent is selected from one or more of sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, formic acid, acetic acid, passes through pH value tune
Agent is saved to control antipollution coating solution pH value in 2-6.
Then, prepared antipollution coating is coated in aromatic polyamides desalination layer, after heat treatment forms anti-pollution
Contaminate coating.The temperature of heat treatment is 80-120 DEG C, heat treatment time 0.5-10min.
Correspondingly, mainly included based on anti-pollution reverse-osmosis composite membrane made of the above method invention additionally discloses one kind
Nonwoven layer, polysulfones support membrane, aromatic polyamides desalination layer and antipollution coating.
Wherein, the material of nonwoven layer is preferably polyester or polypropylene, and polysulfones support membrane is coated in nonwoven layer.As above
Method institute art is stated, the aromatic polyamides desalination layer in polysulfones support film layer is by polyamine aqueous phase solution and aromatic polycarboxylic acyl chlorides
Organic phase solution occurs interface polymerization reaction in polysulfones support film surface and is formed;Antipollution in aromatic polyamides desalination layer
Coating is after heat treatment formed by that will be coated in antipollution coating solution in aromatic polyamides desalination layer;The antipollution coating solution
Solute include polyacrylamide, additive, aldehydes, pH adjusting agent, solvent is water and water soluble organic substance.
It is worth noting that, in the process, it can be by selecting different electrical polyacrylamides, for example, selecting band just
The cationic-type polyacrylamide of charge, negatively charged anion-polyacrylamide or uncharged neutral polypropylene
Amide makes anti-pollution reverse osmosis membrane surface electrical behavior obtained controllable, to be suitable for different application field.
Below by specific embodiment, further the present invention will be described.
Reverse osmosis composite membrane prepared by the present invention, performance can be characterized by salt rejection rate and water flux, and observe each reality
Apply the reverse osmosis composite membrane hydrophily obtained by example.
The calculation of salt rejection rate R is:
Wherein, CfeedRepresent salinity in water inlet;CpermeateRepresent salinity in production water.
Water flux is defined as:Refer under certain pressure, the volume for the water that the unit interval passes through per membrane area, unit L/
(m2·h)。
The test condition used in the present invention for:25 DEG C of test temperature, concentration 2000ppm NaCl aqueous solutions, test pressure
1.55MPa PH=7.5-8.0.
In embodiment 1-9, polysulfones mass fraction is 18% in casting solution, additive is PVP in casting solution, mass fraction
It is DMF for solvent in 1%, casting solution, mass fraction 82%.
Polysulfones (PSf), additive are dissolved in solvent, are configured to casting solution, curtain coating is in non-woven polyester after filtering, deaeration
On cloth, gel in deionized water is immersed, polysulfones support membrane is made;Polysulfones support membrane is immersed in aqueous phase solution, in aqueous phase solution
M-phenylene diamine (MPD) mass fraction 2%, the water phase residence time be 30s, taking-up with air purge removal redundant solution after, support membrane side with
Interface polymerization reaction occurs for the hexane solution contact of pyromellitic trimethylsilyl chloride mass fraction 0.2%, and reaction time 30s is put into 70
After DEG C baking oven heat treatment 30s, rinse, dry through deionized water, aromatic polyamides desalination layer is made;Antipollution coating solution is prepared,
Coated in aromatic polyamides desalination layer, antipollution coating is formed after heat treatment.The corresponding test of reverse osmosis composite membrane obtained
The test result of performance is shown in Table 1.
Comparative example 1:The operating method and step of comparative example 1 are same as Example 1 in addition to antipollution coating is not used.
Test result is shown in Table 1.
Table 1
Anti-pollution reverse osmosis membrane surface flatness higher produced by the present invention, pollutant attachment can be found based on above-mentioned experiment
It is substantially reduced, the service life of film can be greatly improved;Test result based on table 1 shows that embodiment is prepared anti-by coating
Anti-pollution reverse-osmosis composite membrane made from coating is polluted, under selected test condition, water flux is declined slightly, but salt rejection rate
It is greatly improved than comparative example 1;And the surface electrical behavior of film can be made controllable by the polyacrylamides for selecting difference electrical,
Application range is also wider.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, that is made any repaiies
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of preparation method of anti-pollution reverse-osmosis composite membrane, it is characterised in that:Include the following steps:
Polyamine aqueous phase solution and aromatic polycarboxylic acyl chlorides organic phase solution in polysulfones support film surface are contacted and interface occurs
Polymerisation forms aromatic polyamides desalination layer;
Prepared antipollution coating solution is coated in aromatic polyamides desalination layer, after heat treatment crosslinks reaction, shape
Into antipollution coating;
The antipollution coating solution is the acidic mixed solution containing polyacrylamide, aldehydes.
2. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:The polyacrylamide
Selected from one or more of cationic-type polyacrylamide, anion-polyacrylamide, neutral polyacrylamide.
3. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:The aldehydes is selected from first
One or more of aldehyde, glyoxal, glutaraldehyde, hexandial.
4. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:The antipollution coating
The mass fraction of polyacrylamide is 0.05-2% in liquid, and the mass fraction of aldehydes is 0.05-5%.
5. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:Pass through pH adjusting agent
The pH value range for controlling antipollution coating solution is 2-6, and the pH adjusting agent is selected from sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, formic acid, second
One or more of acid.
6. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:The antipollution coating
For the solute of liquid also comprising additive, the additive is selected from polyethylene glycol 400, cetomacrogol 1000, polyethylene glycol 2000, poly- second
Glycol 6000, polyethylene glycol 10000, PEG 20000, polyvinyl alcohol one or more, mass fraction be not more than 2%.
7. the preparation method of anti-pollution reverse-osmosis composite membrane as described in claim 1, it is characterised in that:The antipollution coating
The solvent of liquid is water or water and water soluble organic substance;When solvent is water and water soluble organic substance, the water soluble organic substance choosing
From one or more of methanol, ethyl alcohol, propyl alcohol, isopropanol, n-butanol, isobutanol, the tert-butyl alcohol, and mass fraction is not more than
3%.
8. the preparation method of the anti-pollution reverse-osmosis composite membrane as described in claim 1 to 7 any one, it is characterised in that:Heat
The temperature of processing is 80-120 DEG C, time 0.5-10min.
9. a kind of anti-pollution reverse-osmosis composite membrane, it is characterised in that:It is taken off including nonwoven layer, polysulfones support membrane, aromatic polyamides
Salt deposit and antipollution coating;For polysulfones support membrane coated in nonwoven layer, aromatic polyamides desalination layer is molten by polyamine water phase
Liquid and aromatic polycarboxylic acyl chlorides organic phase solution are formed after interface polymerization reaction occurs in polysulfones support film surface, antipollution coating
It is to be formed after reaction is crosslinked in heat treatment by the antipollution coating solution being coated in aromatic polyamides desalination layer;It is described anti-
Pollution coating solution is the acidic mixed solution containing polyacrylamide, aldehydes.
10. anti-pollution reverse-osmosis composite membrane as claimed in claim 9, it is characterised in that:The solute of the antipollution coating solution
For polyacrylamide, aldehydes and additive, solvent is water or water and water soluble organic substance;The mass fraction of polyacrylamide is
0.05-2%, the mass fraction of aldehydes is 0.05-5%;The mass fraction of additive is 0-2%.
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CN113262641A (en) * | 2021-04-02 | 2021-08-17 | 蓝星(杭州)膜工业有限公司 | Anti-pollution reverse osmosis membrane and preparation method and application thereof |
CN114053876A (en) * | 2021-12-02 | 2022-02-18 | 万华化学集团股份有限公司 | Preparation method of anti-pollution reverse osmosis membrane |
CN115282783A (en) * | 2022-10-09 | 2022-11-04 | 蓝星(杭州)膜工业有限公司 | Reverse osmosis membrane and preparation method and application thereof |
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