CN108380050A - A kind of water process resistance to erosion, antipollution complex reverse osmosis membrane and preparation method - Google Patents
A kind of water process resistance to erosion, antipollution complex reverse osmosis membrane and preparation method Download PDFInfo
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- CN108380050A CN108380050A CN201810200539.XA CN201810200539A CN108380050A CN 108380050 A CN108380050 A CN 108380050A CN 201810200539 A CN201810200539 A CN 201810200539A CN 108380050 A CN108380050 A CN 108380050A
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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
- B01D67/0006—Organic membrane manufacture by chemical reactions
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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
- 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
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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
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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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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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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- 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 provides a kind of water process resistance to erosion, antipollution complex reverse osmosis membrane and preparation methods.N is added in polyamide, polyvinyl alcohol and polyethylene glycol, in N dimethylacetylamides, stirring and dissolving and casting film-forming, obtain the polyamide desalination layer containing polyvinyl alcohol molecule, in surface coating polyethylene alcohol/hexafluoroisopropanol coating liquid of polyamide desalination layer and polyacrylonitrile hydrolyzed solution, with non-woven fabric compounded rear compaction drying, you can water process resistance to erosion, antipollution complex reverse osmosis membrane is made.This method passes through in polyamide desalination layer surface coating polyethylene alcohol/hexafluoroisopropanol coating liquid and polyacrylonitrile hydrolyzed solution, form chemical hydrogen bond, greatly improve the intensity of polyvinyl alcohol layer, it is not easily to fall off and damaged under current scour, effectively extend the service life of reverse osmosis membrane, and complex reverse osmosis membrane resistance tocrocking obtained is strong, and water treatment efficiency is good, can be applicable.
Description
Technical field
The present invention relates to field of membrane material, and in particular to the preparation of reverse osmosis membrane, more particularly to a kind of water process with resistance to
It washes away, antipollution complex reverse osmosis membrane and preparation method.
Background technology
Reverse osmosis membrane filtration technology is a kind of efficient, low energy and easy-operating liquid separation technology, than traditional water process
Method effect is good, it can be achieved that sea water desalination, waste water recycling and effectively recycled to utility.But with its application field
Expansion, membrane pollution problem shows especially increasingly：Reverse osmosis membrane is highly prone to the invasion of biological pollution in use, causes film property
It can irreversible decline.Fouling membrane refers to pollutant and blocks irreversible flux depression caused by fenestra road, concentration polarization, filter cake compression
Caused reversible flux depression and other factors cause the physical damnification of film and chemical damage to make separation rate decline etc., point
Two types are polluted for organic matter absorption pollution, inorganic matter precipitation, are mostly that both types occur together in actual motion, jointly
Effect, membrane biological pollution problem can be effectively relieved by preparing the reverse osmosis membrane with sterilizing function.
Currently, the exploitation of anti-pollution film is broadly divided into two major classes mode, i.e. composite coating class and film surface is modified class.It is wherein multiple
It is to be coated with thin film on reverse osmosis membrane surface using macromolecules such as polyvinyl alcohol, polyethers to close coating class.Due to polyvinyl alcohol
Good hydrophilic property, polyvinyl alcohol can gradually dissolve and eventually fall out during reverse osmosis membrane surface is subjected to rinsing, to lose
Resistance tocrocking caused by polyethylene coating.The prior art prepares crosslinked polyethylene coating, this method by heating
Defect be in solution simultaneously contain polyvinyl alcohol, crosslinking agent and catalyst, partial cross-linked, shape can also occur when not heating up
The cross-linked polymer of gelled influences to coat effect.Reduce the formation of gel cross-linking agent, catalysis can only be may be decreased unexpectedly
The concentration of agent and crosslinking agent, this can cause the degree of cross linking too low, and strength of coating is low, be easy to fall off under current scour and damaged.Cause
This, improve antimicrobial coating performance and intensity be current reverse osmosis membrane area research important topic.
Chinese invention patent application number 201611141165.6 discloses a kind of preparation method of anti-pollution reverse osmosis membrane, packet
Include following steps：（1）Porous carrier layer is covered in membrane surface and carries out ion processing；（2）By the basement membrane leaching after ion processing
Enter the aqueous solution of m-phenylene diamine (MPD)；（3）Wet film is immersed in oil phase slot and carries out polymerisation；（4）Wet film is thermally dried；Afterwards
With the membrane surface by the uniform dip-coating of polyethylene glycol polyelectrolyte aqueous solution after the drying；（5）It is water-soluble that above-mentioned basement membrane is immersed into PVA
In liquid（6）Basement membrane in dipped PVA aqueous solutions is put into vacuum drier and is thermally dried；（7）By the basement membrane after drying
Antipollution processing is carried out, anti-pollution reverse osmosis membrane is made.The preparation method of the anti-pollution reverse osmosis membrane of the invention passes through isophthalic two
The mixed aqueous solution of amine and ethanol amine impregnates polymer ultrafiltration membrane so that the water flux of reverse osmosis membrane is carried significantly
Height, and the salt rejection rate of the permeable membrane of the invention is higher than existing reverse osmosis membrane, preparation process is simple.
Chinese invention patent application number 201410327671.9 discloses a kind of preparation method of polymer compound film, specifically
Refer to a kind of antipollution method of modifying of complex reverse osmosis membrane, the invention through the following steps that：（1）It is dissolved in the water with acid,
A certain amount of chitosan and surfactant are added, it is molten that stirring obtains A after being completely dissolved to chitosan and surfactant
Liquid；（2）It is dissolved in the water with alkaline matter, up to B solution after stirring and dissolving；（3）Again on polyamide composite reverse osmosis membrane surface
Solution A is coated, after removing the extra solution A of film surface, it is made to be contacted with B solution, that is, completes the antipollution of complex reverse osmosis membrane
It is modified.The advantages of the invention is to carry two kinds of hydrophilic radicals of-NH2 and-OH with the modified film surface of this method, is had more good
Hydrophilicity and antifouling property；Meanwhile chitosan need to be only dissolved in acid solution, without heating, be easy behaviour
Make.Thus, there is apparent competitive advantage on membrane modifying operation, production cost.
Chinese invention patent application number 201710235964.8 disclose a kind of high temperature resistant high-flux composite reverse osmosis membrane and
Preparation method.It is to be formed above base material that certain density fluorinated poly arylene ether ketone containing graphene oxide, which is coated in non-woven fabrics,
Then supporting layer successively applies in support layer surface and is covered with solution A and solution B, polyamide/polyamidoimide is formed by reaction
Desalination layer, the upper modified polyvinylalcohol anti-pollution layer of desalination layer re-coating.The complex reverse osmosis membrane is made；With the prior art
Compare, the invention as supporting layer and adulterates graphene oxide composite material using fluorinated poly arylene ether ketone, can prepare high temperature resistant, high intensity,
The complex reverse osmosis membrane of high water-flowing amount, the present invention have higher resistance tocrocking using modified polyvinylalcohol as anti-pollution layer.
Chinese invention patent application number 201710416654.6 discloses a kind of compound reverse osmosis of high-throughput antipollution polyamide
Permeable membrane and preparation method thereof, the reverse osmosis membrane be by aromatic polyamide complex reverse osmosis membrane and its surface-active acid chloride groups with
The hydrophilic layer of amino reaction dehydrating condensation in Amino End Group polyol is constituted, the more initial aromatic polyamide of water flux
Complex reverse osmosis membrane improves 13 ~ 30%, and reverse osmosis membrane water flux after the pollution cleaning of first time bovine serum albumin(BSA) is extensive
Multiple rate is the 88.5 ~ 92.4% of initial virginal membrane water flux；After the pollution cleaning of first time dodecyl trimethyl ammonium bromide
Flux recovery rate is the 90.3 ~ 93.5% of initial virginal membrane water flux.The invention reverse osmosis membrane has good separation property
Can, antifouling property and water flux are high, the features such as being readily cleaned, preparation method is also simple, easily operated.
According to above-mentioned, the reverse osmosis membrane in existing scheme has been contaminated and then has influenced performance and used, and traditional handicraft is provided
Method obtained by polyethylene coating and polyamide coating layer between be physisorption, the not link of chemical bond, apply
Easy full wafer falls off in the case that breakage occurs in layer, poor impact resistance, and antifouling property is ineffective.
Invention content
For antimicrobial coating there are shock resistances poor, the intensity of the wider composite coating class reverse osmosis membrane of current application
Low, cracky falls off, and then influences antifouling property, and service life is short, a kind of water process resistance to erosion of present invention proposition, anti-pollution
Complex reverse osmosis membrane and preparation method are contaminated, the scour resistance of reverse osmosis membrane antimicrobial coating and strong is improved to effectively realize
Degree.
Specific technical solution of the present invention is as follows：
A kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane, include the following steps：
（1）By 35 ~ 40 dry weight parts of polyamide particles, 5 ~ 10 weight account polyethylene alcohol particles and the poly- second of 1 ~ 2 parts by weight two
Alcohol is added in 48 ~ 59 parts by weight n,N-dimethylacetamide, is sufficiently stirred dissolving, then standing and defoaming utilizes scraper in glass
Casting film-forming is carried out on plate, and is steadily put into ultrafiltration water, maintenance is stood, and the polyamide desalination containing polyvinyl alcohol molecule is made
Layer；
（2）4 ~ 6 weight account polyethylene alcohol particles, 30 ~ 40 parts by weight hexafluoroisopropanols and 54 ~ 66 parts by weight water are mixed, heating
And promotion dissolving is stirred, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；
（3）30 ~ 40 parts by weight of polypropylene chlorfenapyr particles, 1 ~ 2 part by weight of catalyst and 58 ~ 69 parts by weight water are added in autoclave,
Pressurization heating makes polyacrylonitrile hydrolyzed, obtained polyacrylonitrile hydrolyzed solution；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane.
Preferably, step（1）The temperature of the stirring and dissolving is 70 ~ 80 DEG C, and the time is 40 ~ 60h.
Preferably, step（1）The time of the standing and defoaming is 20 ~ 25h.
Preferably, step（1）The temperature of the ultrafiltration water is 22 ~ 28 DEG C, and curing time is 25 ~ 35min.
Preferably, step（2）The heating temperature is 90 ~ 98 DEG C, and dissolution time is 5 ~ 8h.
Preferably, step（3）The moulding pressure is 1 ~ 1.5MPa, is warming up to 170 ~ 200 DEG C.
Preferably, step（4）The non-woven fabrics is one in terylene, polypropylene fibre, polyamide fibre, spandex, acrylic fibers, polyethylene or polyvinyl chloride fibre
Kind.
Preferably, step（4）The pressure of the compacting is 2 ~ 4MPa, and the dwell time is 6 ~ 10s.
Preferably, step（4）The drying temperature is 60 ~ 70 DEG C, and the time is 2 ~ 3h.
The present invention also provides a kind of water process resistance to erosion that above-mentioned preparation method is prepared, antipollution are compound reverse osmosis
Film.By in polyamide desalination layer surface coating polyethylene alcohol/hexafluoroisopropanol coating liquid and polyacrylonitrile hydrolyzed solution, shape
At numerous intramolecular and intermolecular hydrogen bonding, it is keyed to make polyethylene coating and polyamide desalination layer pass through chemistry
Come, not only improves the resistance tocrocking of reverse osmosis membrane, while substantially increasing the intensity of polyvinyl alcohol layer, be not easy in current scour
Under fall off and damaged, extend the service life of reverse osmosis membrane.
Complex reverse osmosis membrane prepared by the present invention, it is anti-with common polythene alcohol coating reverse osmosis membrane and common polyether coating
Permeable membrane is compared, and in flux depression rate, salt rejection rate rate of descent and is washed away on coating quality residual rate, is had apparent excellent
Gesture, as shown in table 1.
Table 1：
The present invention provides a kind of water process resistance to erosion, antipollution complex reverse osmosis membrane and preparation methods, with prior art phase
Than the feature and excellent effect protruded is：
1, it proposes polyamide desalination layer and non-woven fabric compounded preparation water process resistance to erosion, the side of antipollution complex reverse osmosis membrane
Method.
2, by polyamide desalination layer surface coating polyethylene alcohol/hexafluoroisopropanol coating liquid and polyacrylonitrile hydrolyzed
Solution forms chemical hydrogen bond, greatly improves the intensity of polyvinyl alcohol layer, not easily to fall off and damaged under current scour, effectively prolongs
The service life of reverse osmosis membrane is grown.
3, complex reverse osmosis membrane resistance tocrocking produced by the present invention is strong, and water treatment efficiency is good, can be applicable.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Preparation process is：
（1）37 dry weight parts of polyamide particles, 8 weight account polyethylene alcohol particles and 1 parts by weight polyethylene glycol are added 54
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 76 DEG C, time 55h；The time of standing and defoaming is 23h；The temperature of ultrafiltration water is 26 DEG C, curing time 32min；
（2）5 weight account polyethylene alcohol particles, 36 parts by weight hexafluoroisopropanols and 59 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 95 DEG C, and heat preservation dissolution time is 7h；
（3）36 parts by weight of polypropylene chlorfenapyr particles, 2 part by weight of catalyst and 62 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1.3MPa, and temperature is 190 DEG C；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is terylene；The pressure of compacting is 3MPa, pressurize
Time is 8s；Drying temperature is 66 DEG C, time 2.5h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 1 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 1 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 1 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 1 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Embodiment 2
Preparation process is：
（1）35 dry weight parts of polyamide particles, 5 weight account polyethylene alcohol particles and 1 parts by weight polyethylene glycol are added 59
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 70 DEG C, time 60h；The time of standing and defoaming is 20h；The temperature of ultrafiltration water is 22 DEG C, curing time 35min；
（2）4 weight account polyethylene alcohol particles, 30 parts by weight hexafluoroisopropanols and 66 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 90 DEG C, and heat preservation dissolution time is 8h；
（3）30 parts by weight of polypropylene chlorfenapyr particles, 1 part by weight of catalyst and 69 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1MPa, and temperature is 170 DEG C；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is polypropylene fibre；The pressure of compacting is 2MPa, pressurize
Time is 10s；Drying temperature is 60 DEG C, time 3h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 2 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 2 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 2 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 2 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Embodiment 3
Preparation process is：
（1）40 dry weight parts of polyamide particles, 10 weight account polyethylene alcohol particles and 2 parts by weight polyethylene glycol are added 48
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 80 DEG C, time 40h；The time of standing and defoaming is 25h；The temperature of ultrafiltration water is 28 DEG C, curing time 25min；
（2）6 weight account polyethylene alcohol particles, 40 parts by weight hexafluoroisopropanols and 54 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 98 DEG C, and heat preservation dissolution time is 5h；
（3）40 parts by weight of polypropylene chlorfenapyr particles, 2 part by weight of catalyst and 58 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1.5MPa, 200 DEG C of temperature；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is polyamide fibre；The pressure of compacting is 4MPa, pressurize
Time is 6s；Drying temperature is 70 DEG C, time 2h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 3 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 3 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 3 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 3 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Embodiment 4
Preparation process is：
（1）36 dry weight parts of polyamide particles, 6 weight account polyethylene alcohol particles and 1 parts by weight polyethylene glycol are added 57
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 72 DEG C, time 55h；The time of standing and defoaming is 21h；The temperature of ultrafiltration water is 24 DEG C, curing time 32min；
（2）4 weight account polyethylene alcohol particles, 32 parts by weight hexafluoroisopropanols and 64 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 92 DEG C, and heat preservation dissolution time is 7h；
（3）32 parts by weight of polypropylene chlorfenapyr particles, 1 part by weight of catalyst and 67 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1.3MPa, and temperature is 180 DEG C；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is spandex；The pressure of compacting is 2.5MPa, is protected
The pressure time is 9s；Drying temperature is 62 DEG C, time 3h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 4 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 4 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 4 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 4 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Embodiment 5
Preparation process is：
（1）36 dry weight parts of polyamide particles, 7 weight account polyethylene alcohol particles and 2 parts by weight polyethylene glycol are added 55
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 78 DEG C, time 45h；The time of standing and defoaming is for 24 hours；The temperature of ultrafiltration water is 26 DEG C, curing time 28min；
（2）6 weight account polyethylene alcohol particles, 38 parts by weight hexafluoroisopropanols and 56 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 96 DEG C, and heat preservation dissolution time is 6h；
（3）38 parts by weight of polypropylene chlorfenapyr particles, 2 part by weight of catalyst and 60 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1.5MPa, and temperature is 185 DEG C；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is acrylic fibers；The pressure of compacting is 4MPa, pressurize
Time is 7s；Drying temperature is 68 DEG C, time 2h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 5 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 5 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 5 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 5 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Embodiment 6
Preparation process is：
（1）38 dry weight parts of polyamide particles, 8 weight account polyethylene alcohol particles and 2 parts by weight polyethylene glycol are added 52
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 76 DEG C, time 50h；The time of standing and defoaming is 23h；The temperature of ultrafiltration water is 25 DEG C, curing time 30min；
（2）5 weight account polyethylene alcohol particles, 35 parts by weight hexafluoroisopropanols and 60 parts by weight water are mixed, heats and stirs rush
Into dissolving, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；Heating temperature is 94 DEG C, and heat preservation dissolution time is 6.5h；
（3）35 parts by weight of polypropylene chlorfenapyr particles, 2 part by weight of catalyst and 63 parts by weight water are added in autoclave, pressurization heats up,
Polyacrylonitrile hydrolyzed solution is made；Pressure is 1.4MPa, and temperature is 180 DEG C；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane；Non-woven fabrics is polyvinyl chloride fibre；The pressure of compacting is 3MPa, pressurize
Time is 8s；Drying temperature is 65 DEG C, time 3h.
Test method：
Flux depression rate：Reverse osmosis membrane made from embodiment 6 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from embodiment 6 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from embodiment 6 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the embodiment 6 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Comparative example 1
Preparation process is：
（1）38 dry weight parts of polyamide particles, 8 weight account polyethylene alcohol particles and 2 parts by weight polyethylene glycol are added 52
In parts by weight n,N-dimethylacetamide, it is sufficiently stirred dissolving, then standing and defoaming is cast on a glass using scraper
Film forming, and be steadily put into ultrafiltration water, maintenance is stood, the polyamide desalination layer containing polyvinyl alcohol molecule is made；Stirring and dissolving
Temperature is 76 DEG C, time 50h；The time of standing and defoaming is 23h；The temperature of ultrafiltration water is 25 DEG C, curing time 30min；
（2）By step（1）Polyamide desalination layer obtained carries out compound, compacting simultaneously drying, you can water process is made with non-woven fabrics
Use complex reverse osmosis membrane；Non-woven fabrics is polyvinyl chloride fibre；The pressure of compacting is 3MPa, dwell time 8s；Drying temperature is 65 DEG C, the time
For 3h.
Test method：
Flux depression rate：Reverse osmosis membrane made from comparative example 1 is added in a certain amount of organic pollution sewage, at 20 DEG C
1h experiments are carried out, 3 membrane fluxs is measured, calculates the rate of descent of membrane flux, characterize its antifouling property；
Salt rejection rate rate of descent：Reverse osmosis membrane made from comparative example 1 is added in a certain amount of brine, 1h examinations are carried out at 20 DEG C
It tests, measures 3 salt fractional doses, calculate the rate of descent of salt rejection rate, characterize its antifouling property.
Wash away coating quality residual rate：Reverse osmosis membrane made from comparative example 1 is subjected to current scour experiment, in 10m/s water
Stream washes away lower 1h, detects the mass ratio of coating on reverse osmosis membrane, calculates coating quality residual rate, characterize its flushing resistance.
The flux depression rate of the complex reverse osmosis membrane of the comparative example 1 measured by the above method, salt rejection rate rate of descent and
It is as shown in table 2 to wash away coating quality residual rate.
Table 2：
Claims (10)
1. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane, which is characterized in that including following step
Suddenly：
（1）By 35 ~ 40 dry weight parts of polyamide particles, 5 ~ 10 weight account polyethylene alcohol particles and the poly- second of 1 ~ 2 parts by weight two
Alcohol is added in 48 ~ 59 parts by weight n,N-dimethylacetamide, is sufficiently stirred dissolving, then standing and defoaming utilizes scraper in glass
Casting film-forming is carried out on plate, and is steadily put into ultrafiltration water, maintenance is stood, and the polyamide desalination containing polyvinyl alcohol molecule is made
Layer；
（2）4 ~ 6 weight account polyethylene alcohol particles, 30 ~ 40 parts by weight hexafluoroisopropanols and 54 ~ 66 parts by weight water are mixed, heating
And promotion dissolving is stirred, polyvinyl alcohol/hexafluoroisopropanol coating liquid is made；
（3）30 ~ 40 parts by weight of polypropylene chlorfenapyr particles, 1 ~ 2 part by weight of catalyst and 58 ~ 69 parts by weight water are added in autoclave,
Pressurization heating makes polyacrylonitrile hydrolyzed, obtained polyacrylonitrile hydrolyzed solution；
（4）In step（1）The surface coating step of polyamide desalination layer obtained（2）Polyvinyl alcohol/hexafluoroisopropanol obtained
Coating liquid is coated with step（3）Polyacrylonitrile hydrolyzed solution obtained further carries out compound, compacting simultaneously drying with non-woven fabrics,
It can be prepared by water process resistance to erosion, antipollution complex reverse osmosis membrane.
2. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（1）The temperature of the stirring and dissolving is 70 ~ 80 DEG C, and the time is 40 ~ 60h.
3. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（1）The time of the standing and defoaming is 20 ~ 25h.
4. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（1）The temperature of the ultrafiltration water is 22 ~ 28 DEG C, and curing time is 25 ~ 35min.
5. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（2）The heating temperature is 90 ~ 98 DEG C, and dissolution time is 5 ~ 8h.
6. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（3）The moulding pressure is 1 ~ 1.5MPa, is warming up to 170 ~ 200 DEG C.
7. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（4）The non-woven fabrics is one kind in terylene, polypropylene fibre, polyamide fibre, spandex, acrylic fibers, polyethylene or polyvinyl chloride fibre.
8. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（4）The pressure of the compacting is 2 ~ 4MPa, and the dwell time is 6 ~ 10s.
9. a kind of water process resistance to erosion, the preparation method of antipollution complex reverse osmosis membrane according to claim 1, feature
It is：Step（4）The drying temperature is 60 ~ 70 DEG C, and the time is 2 ~ 3h.
10. a kind of water process resistance to erosion that any one of claim 1 ~ 9 preparation method is prepared, antipollution are compound anti-
Permeable membrane.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112044280A (en) * | 2019-06-05 | 2020-12-08 | 广州中国科学院先进技术研究所 | Anti-membrane biological pollution coating and preparation method thereof |
| CN112870989A (en) * | 2021-01-11 | 2021-06-01 | 中化(宁波)润沃膜科技有限公司 | Anti-pollution composite reverse osmosis membrane and preparation method thereof |
| US11502323B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell and methods of use thereof |
| US11502322B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11855324B1 (en) | 2022-11-15 | 2023-12-26 | Rahul S. Nana | Reverse electrodialysis or pressure-retarded osmosis cell with heat pump |
-
2018
- 2018-03-12 CN CN201810200539.XA patent/CN108380050A/en not_active Withdrawn
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112044280A (en) * | 2019-06-05 | 2020-12-08 | 广州中国科学院先进技术研究所 | Anti-membrane biological pollution coating and preparation method thereof |
| CN112870989A (en) * | 2021-01-11 | 2021-06-01 | 中化(宁波)润沃膜科技有限公司 | Anti-pollution composite reverse osmosis membrane and preparation method thereof |
| US11502323B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell and methods of use thereof |
| US11502322B1 (en) | 2022-05-09 | 2022-11-15 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11563229B1 (en) | 2022-05-09 | 2023-01-24 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11611099B1 (en) | 2022-05-09 | 2023-03-21 | Rahul S Nana | Reverse electrodialysis cell and methods of use thereof |
| US11699803B1 (en) | 2022-05-09 | 2023-07-11 | Rahul S Nana | Reverse electrodialysis cell with heat pump |
| US11855324B1 (en) | 2022-11-15 | 2023-12-26 | Rahul S. Nana | Reverse electrodialysis or pressure-retarded osmosis cell with heat pump |
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