CN106166450A - A kind of high temperature resistant accurate molecular cut off ultrafilter membrane and preparation method thereof - Google Patents
A kind of high temperature resistant accurate molecular cut off ultrafilter membrane and preparation method thereof Download PDFInfo
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- CN106166450A CN106166450A CN201610643149.0A CN201610643149A CN106166450A CN 106166450 A CN106166450 A CN 106166450A CN 201610643149 A CN201610643149 A CN 201610643149A CN 106166450 A CN106166450 A CN 106166450A
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- Prior art keywords
- membrane
- preparation
- high temperature
- ultrafilter membrane
- temperature resistant
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- 238000002360 preparation method Methods 0.000 title claims abstract description 38
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- 230000007613 environmental effect Effects 0.000 description 1
- FKRCODPIKNYEAC-UHFFFAOYSA-N ethyl propionate Chemical compound CCOC(=O)CC FKRCODPIKNYEAC-UHFFFAOYSA-N 0.000 description 1
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical group O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000008235 industrial water Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000015689 metaplastic ossification Effects 0.000 description 1
- 229920000069 polyphenylene sulfide Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0013—Casting processes
-
- 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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
-
- 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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0016—Coagulation
-
- 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
-
- 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
- B01D71/16—Cellulose acetate
-
- 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
- B01D71/20—Esters of inorganic acids, e.g. cellulose nitrate
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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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Abstract
The present invention relates to technical field of membrane, a kind of high temperature resistant accurate molecular cut off ultrafilter membrane and preparation method thereof, prepared by hygrometric state basement membrane, and combine hygrometric state basement membrane is modified solution modification process, and combine the raw material composition in hygrometric state basement membrane preparation process and bound of parameter is fixed, guarantee preparation hygrometric state basement membrane after follow-up modification, its performance is stablized, and can effectively improve its resistance to elevated temperatures；In combination with defining of the time during modification, temperature and processing mode, make ultrafilter membrane that in the rejection of 2,000 4000 scopes, molecular weight is reached more than 90%, effectively raise ultrafilter membrane low molecular weight substance is retained, improve the quality of filtering product.
Description
Technical field
The present invention relates to technical field of membrane, a kind of high temperature resistant accurate molecular cut off ultrafilter membrane and preparation side thereof
Method.
Background technology
Ultrafiltration Membrane is one of membrane separation technique of growing up in the sixties in 20th century.Currently for abroad,
Through ultrafiltration membrane technique is applied to technical field of drinking water treatment, and China is mainly used in Treatment of Industrial Water aspect, and
Along with the fast development of domestic industry level, it obtains in terms of the waste water process of the industrial circles such as chemical industry, smelting iron and steel, electric power
Be widely applied, and along with industrial development while, water pollutes the most increasingly severe, result in the short of Available water resources
Scarce problem highlights day by day；According to statistics, current former water has been detected by more than 2000 kinds of organic pollutions, most of organic contaminations
Thing uses conventional process technique and method to be difficult to remove so that the inferior quality of drinking water, is even difficult to reach drinking water
Standard, and hyperfiltration technique is due to its particularity, is widely used in this respect, and bring significant effect.
But, along with pharmaceuticals industry, the fast development of environmental protection industry (epi) so that kind and performance to ultrafilter membrane product propose
Higher requirement, especially increases day by day to the market demand of the ultrafilter membrane retaining low-molecular-weight.At biological engineering and medicine
Industrial circle, solable matter and the molecular weight of the needs a large amount of low-molecular-weights of process are the enzyme of thousand of left and right, virus, protein etc.
Polymer substance, and for the process of this type of material, the most commonly used is at NF membrane and inoranic membrane
Reason；But the preparation method of NF membrane is complicated, operation pressure ratio ultrafilter membrane is much higher, and the permeation flux of separation process is low, it is impossible to
Meet the market demand；The problem that inoranic membrane then exists difficult sealing；Simultaneously, abroad for the research of ultrafilter membrane, mainly concentrate
It is being several ten thousand ultrafilter membrane researchs arriving hundreds of thousands to molecular cut off, ultrafilter membrane is being retained to the report of research to low-molecular-weight
Relatively fewer.
To this end, this researcher combines long-term exploration and practice, ultrafilter membrane is retained process to low-molecular-weight and grinds
Study carefully, and the resistance to elevated temperatures of ultrafilter membrane is accounted for so that the ultrafilter membrane of acquisition can carry out essence to the material of small-molecular-weight
Close retain process, provide a kind of new approaches for ultrafiltration membrane technique field.
Summary of the invention
In order to solve above-mentioned technical problem present in prior art, the present invention provides a kind of high temperature resistant precision to retain molecule
Amount ultrafilter membrane and preparation method thereof.
It is achieved particular by techniques below scheme:
The preparation method of a kind of high temperature resistant accurate molecular cut off ultrafilter membrane, comprises the following steps:
(1) joining in organic solvent by polymer, pore former, wherein polymer volume is 10-by percentage to the quality
24%, pore former 1-10%, surplus is organic solvent；Adjust temperature and be 65-75 DEG C, stirring and dissolving 2-4h, it is filtered to remove impurity,
Carried out vacuum removal bubble again, it is thus achieved that casting solution, and casting solution is scraped on non-woven fabrics equably, and used at water-bath
Reason so that its solidification converts film forming, then uses the water of 79-81 DEG C to clean, it is thus achieved that hygrometric state basement membrane；
(2) hygrometric state basement membrane is soaked in modifier solution, immersion treatment 1-300min；The wherein temperature of modifier solution
For 80-90 DEG C, take out hygrometric state basement membrane, dry at 80-90 DEG C, it is thus achieved that.
Described polymer be polyether sulfone, sulfonated polyether sulfone, novel poly (arylene ether nitrile) ketone, polyacrylonitrile, cellulose propionate,
Phthalazinone polyether sulfone, polysulfones, SPSF, Kynoar, polrvinyl chloride, cellulose acetate, polyvinyl alcohol, polyphenylene sulfide
Sulfone, celluloid, polyvinyl butyral resin, polymethyl methacrylate at least one.
Described pore former is Polyethylene Glycol 100, polyethylene glycol 200, PEG400, Macrogol 600, poly-second two
Alcohol 800, cetomacrogol 1000, Macrogol 2000, Macrogol 3000, Macrogol 4000, polyethylene glycol 6000, poly-second two
Alcohol 8000, PEG20000, PEG 20000, polyoxyethylene 50000, polyoxyethylene 100000, polyvinylpyrrolidine
Ketone K13, PVP K30, polyvinylpyrrolidone K40, polyvinylpyrrolidone K60, polyvinylpyrrolidone
K80, PVP K90, lithium chloride, polyvinyl alcohol, polyvinyl butyral resin, nano-aluminium oxide, nano-silica
SiClx, cesium chloride, lithium bromide, nano titanium oxide, nano zine oxide, zinc chloride, aluminum chloride, ferrous chloride, iron sesquioxide,
Magnesium hypochlorite, phosphoric acid, CNT, Graphene, acetone, glycerol, methanol, ethanol, ethylene glycol, the tert-butyl alcohol, dichloromethane, just
Hexane, isopropanol, normal propyl alcohol, ether, ethylene glycol monomethyl ether, diglycol, propanoic acid, methyl methacrylate, oxalic acid, sweet
One or both combination in any of oil, polysorbas20, polysorbate40, polysorbate60, Tween 80, hexadecanol
Described organic solvent is DMF, N,N-dimethylacetamide, dimethyl sulfoxide, N-methyl pyrrole
Pyrrolidone, dichloromethane, acetone, normal hexane, chloroform, oxolane, the one of acetonitrile.
High temperature resistant accurate molecular cut off ultrafilter membrane prepared by above-mentioned preparation method, its resistance to elevated temperatures is stable, it is possible to have
Effect molecular cut off is the material of 2000-4000.
The invention also provides for a kind of high temperature resistant accurate molecular cut off ultrafilter membrane modifier solution, its material composition
Be made up of cross-linking agent a and cross-linking agent b, solvent, wherein cross-linking agent a be Polyethylene Glycol 100, polyethylene glycol 200, PEG400,
Macrogol 600, polyethylene glycol-800, cetomacrogol 1000, Macrogol 2000, Macrogol 3000, Macrogol 4000,
Polyethylene glycol 6000, PEG 8000, PEG20000, PEG 20000, polyoxyethylene 50000, polyoxyethylene
100000, polyvinyl alcohol, ethylene glycol, methanol, ethanol, propanol, isopropanol, ethylenediamine, hexamethylene diamine, p-phenylenediamine, glucosan, Portugal
Grape sugar, chitosan, citric acid, piperazine, malic acid, polyacrylamide at least one, its consumption accounts for 0.05-3%；Cross-linking agent b
For Silane coupling agent KH550, silane coupler KH560, propanetriol-diglycidyl-ether, polyethyleneglycol diglycidylether, poly-third
Hexanediol diglycidyl ether, formaldehyde, Biformyl, glutaraldehyde, methacrylic acid, trimethylolpropane, petroleum ether, glycerol are at least
One, its consumption accounts for 1-10%；Remaining is solvent.
Described solvent is DMF, N,N-dimethylacetamide, dimethyl sulfoxide, N-crassitude
Ketone, dichloromethane, acetone, normal hexane, chloroform, oxolane, toluene, benzene, dimethylbenzene, chlorobenzene, water, acetonitrile at least one
Described modifying agent pH value is 4-6, and it adds acid in preparation process and is adjusted, and acid therein is high chlorine
Acid, concentrated sulphuric acid, concentrated nitric acid at least one.
Modifier solution preparation method, joins in solvent by cross-linking agent a and cross-linking agent b, adjusts temperature and is 45-55 DEG C,
Stirring and dissolving, and after being clarified, it is thus achieved that transparency liquid, regulation pH value is 4-6, it is thus achieved that.
Compared with prior art, the technique effect of the present invention is embodied in:
Prepared by hygrometric state basement membrane, and combine and hygrometric state basement membrane is modified solution modification processes, and combine hygrometric state basement membrane
Raw material composition and bound of parameter in preparation process are fixed, it is ensured that the hygrometric state basement membrane of preparation after follow-up modification,
Its performance is stablized, and can effectively improve its resistance to elevated temperatures；In combination with the time during modification, temperature
Degree defines with processing mode so that ultrafilter membrane reaches more than 90% to molecular weight in the rejection of 2000-4000 scope, effectively
The ultrafilter membrane that improves low molecular weight substance is retained, improve the quality of filtering product.
In addition, the invention is by being bound the preparation of modified solution and proportioning raw materials so that modified molten
Liquid can improve the performance of hygrometric state basement membrane accurately to hygrometric state basement membrane effect, improve hygrometric state basement membrane and cut low molecular weight substance
Stay rate, improve the ultrafiltration effect of ultrafilter membrane.
The preparation technology of the high temperature resistant accurate molecular cut off ultrafilter membrane that the present invention provides is simple to operation, it is easy to accomplish work
Industry metaplasia is produced, and during use, resistance to elevated temperatures is stable.
Accompanying drawing explanation
Fig. 1 is the infrared figure of the high temperature resistant accurate molecular cut off ultrafilter membrane of the present invention.
Fig. 2 be the present invention high temperature resistant accurate molecular cut off ultrafilter membrane to the rejection of Macrogol 2000 and flux with
The change curve of operation time.Run under the hot environment of 70-90 DEG C.
Detailed description of the invention
Below in conjunction with specific embodiment, technical scheme is further limited, but claimed
Scope is not only limited to description.
In certain embodiments, the preparation method of high temperature resistant accurate molecular cut off ultrafilter membrane, comprise the following steps:
(1) joining in organic solvent by polymer, pore former, wherein polymer volume is 10-by percentage to the quality
24%, pore former 1-10%, surplus is organic solvent；Adjust temperature and be 65-75 DEG C, stirring and dissolving 2-4h, it is filtered to remove impurity,
Carried out vacuum removal bubble again, it is thus achieved that casting solution, and casting solution is scraped on non-woven fabrics equably, and used at water-bath
Reason so that its solidification converts film forming, then uses the water of 79-81 DEG C to clean, it is thus achieved that hygrometric state basement membrane；
(2) hygrometric state basement membrane is soaked in modifier solution, immersion treatment 1-300min；The wherein temperature of modifier solution
For 80-90 DEG C, take out hygrometric state basement membrane, dry at 80-90 DEG C, it is thus achieved that.
In certain embodiments, above-mentioned polymer is sulfonated polyether sulfone, novel poly (arylene ether nitrile) ketone, polyacrylonitrile, cellulose
Propionic ester, Phthalazinone polyether sulfone at least one.
In some other embodiment, above-mentioned pore former is PEG400, cetomacrogol 1000, Polyethylene Glycol
2000, Macrogol 4000, polyvinylpyrrolidone K13, PVP K30, polyvinylpyrrolidone K60, chlorination
Lithium, nano silicon, one or both combination in any of lithium bromide.
In certain embodiments, organic solvent is DMF (DMF), N,N-dimethylacetamide
(DMAC), dimethyl sulfoxide (DMSO), the one of N-Methyl pyrrolidone (NMP).
In the above-described embodiments, it is thus achieved that high temperature resistant accurate molecular cut off ultrafilter membrane, its resistance to elevated temperatures is stable, it is possible to
Effectively catching molecular weight is the material of 2000-4000, and under high temperature resistant environment, the rejection for low molecular weight substance reaches
More than 90%.
In certain embodiments, high temperature resistant accurate molecular cut off ultrafilter membrane modifier solution, its material composition is by handing over
Connection agent a and cross-linking agent b, solvent composition, wherein cross-linking agent a be Polyethylene Glycol, polyvinyl alcohol, chitosan, polyacrylamide extremely
Few one, its consumption accounts for 0.05-3%；Cross-linking agent b is that silane coupler, propanetriol-diglycidyl-ether, polyethylene glycol diglycidyl are sweet
Oil ether, Biformyl, methacrylic acid, trimethylolpropane at least one, its consumption accounts for 1-10%；Remaining is solvent.
In certain embodiments, the solvent of above-mentioned modified solution be acetone, toluene, water, oxolane, at least the one of acetonitrile
Kind.
In certain embodiments, modifying agent pH value is 4-6, and it adds acid in preparation process and is adjusted, wherein
Acid be perchloric acid, concentrated sulphuric acid, concentrated nitric acid at least one.
In certain embodiments, modifier solution preparation method, is to join in solvent by cross-linking agent a and cross-linking agent b, adjusts
Whole temperature is 45-55 DEG C, stirring and dissolving, and after being clarified, it is thus achieved that transparency liquid, regulation pH value is 4-6, it is thus achieved that.
Embodiment 1
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 10%, and pore former is 1%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds molten by the cross-linking agent b accounting for the cross-linking agent a and 10% of modified solution gross mass 3%
In agent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Embodiment 2
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 15%, and pore former is 3%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds the cross-linking agent b accounting for the cross-linking agent a and 8% of modified solution gross mass 1.75%
In solvent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Embodiment 3
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 18%, and pore former is 5%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds the cross-linking agent b accounting for the cross-linking agent a and 6% of modified solution gross mass 1.25%
In solvent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Embodiment 4
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 18%, and pore former is 3%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds the cross-linking agent b accounting for the cross-linking agent a and 5% of modified solution gross mass 0.75%
In solvent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Embodiment 5
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 20%, and pore former is 8%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds the cross-linking agent b accounting for the cross-linking agent a and 3% of modified solution gross mass 0.2%
In solvent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Embodiment 6
(1) preparation of hygrometric state ultrafiltration membranes, adds in organic solvent by membrane material polymer and pore former, wherein membrane material
Polymer is 24%, and pore former is 10%, remaining as organic solvent, dissolves 2～4h about 70 DEG C mechanical agitation, is filtered to remove
After residual impurities, and vacuum removal bubble, obtain limpid transparent casting solution, casting solution is scraped the most equably smooth, dry
On dry non-woven fabrics, then inversion of phases film forming in pure water coagulating bath, then cleaned by the high temperature pure water of 80 DEG C；
(2) preparation of modified solution, adds the cross-linking agent b accounting for the cross-linking agent a and 1% of modified solution gross mass 0.05%
In solvent, dissolve in about 50 DEG C mechanical agitation and obtain clear transparent solutions, and to add acid-conditioning solution pH value be 5；
(3) the composite modified film forming of membrane surface, immerses step (2) by hygrometric state basement membrane prepared in step (1) and is prepared
85 DEG C of modified solutions in, make cross-linking agent a and cross-linking agent b be grafted on ultrafiltration membranes surface by crosslinked action, then take out
In about 85 DEG C drying.
Be necessary at this explanation, above example be only limitted to technical scheme is further explained and
Illustrating, not further limited technical scheme, those skilled in the art make non-protruding on this basis
Essential characteristics and the improvement of non-significant progress, belong to the protection category of the present invention.
Claims (9)
1. the preparation method of a high temperature resistant accurate molecular cut off ultrafilter membrane, it is characterised in that comprise the following steps:
(1) joining in organic solvent by polymer, pore former, wherein polymer volume is 10-24% by percentage to the quality,
Pore former 1-10%, surplus is organic solvent；Adjust temperature and be 65-75 DEG C, stirring and dissolving 2-4h, it is filtered to remove impurity, then will
It carries out vacuum removal bubble, it is thus achieved that casting solution, and is scraped on non-woven fabrics equably by casting solution, and uses water bath processing, makes
Obtain its solidification and convert film forming, then use the water of 79-81 DEG C to clean, it is thus achieved that hygrometric state basement membrane；
(2) hygrometric state basement membrane is soaked in modifier solution, immersion treatment 1-300min；Wherein the temperature of modifier solution is
80-90 DEG C, take out hygrometric state basement membrane, dry at 80-90 DEG C, it is thus achieved that.
The preparation method of high temperature resistant accurate molecular cut off ultrafilter membrane the most as claimed in claim 1, it is characterised in that described
Polymer is polyether sulfone, sulfonated polyether sulfone, novel poly (arylene ether nitrile) ketone, polyacrylonitrile, cellulose propionate, Phthalazinone polyethers
Sulfone, polysulfones, SPSF, Kynoar, polrvinyl chloride, cellulose acetate, polyvinyl alcohol, PPSS, cellulose nitrate
Element, polyvinyl butyral resin, polymethyl methacrylate at least one.
The preparation method of high temperature resistant accurate molecular cut off ultrafilter membrane the most as claimed in claim 1, it is characterised in that described
Pore former is Polyethylene Glycol 100, polyethylene glycol 200, PEG400, Macrogol 600, polyethylene glycol-800, Polyethylene Glycol
1000, Macrogol 2000, Macrogol 3000, Macrogol 4000, polyethylene glycol 6000, PEG 8000, poly-second two
Alcohol 10000, PEG 20000, polyoxyethylene 50000, polyoxyethylene 100000, polyvinylpyrrolidone K13, polyethylene pyrrole
Pyrrolidone K30, polyvinylpyrrolidone K40, polyvinylpyrrolidone K60, polyvinylpyrrolidone K80, polyvinylpyrrolidine
Ketone K90, lithium chloride, polyvinyl alcohol, polyvinyl butyral resin, nano-aluminium oxide, nano silicon, cesium chloride, bromination
Lithium, nano titanium oxide, nano zine oxide, zinc chloride, aluminum chloride, ferrous chloride, iron sesquioxide, magnesium hypochlorite, phosphoric acid, carbon
Nanotube, Graphene, acetone, glycerol, methanol, ethanol, ethylene glycol, the tert-butyl alcohol, dichloromethane, normal hexane, isopropanol, positive third
Alcohol, ether, ethylene glycol monomethyl ether, diglycol, propanoic acid, methyl methacrylate, oxalic acid, glycerol, polysorbas20, polysorbate40,
One or both combination in any of polysorbate60, Tween 80, hexadecanol.
The preparation method of high temperature resistant accurate molecular cut off ultrafilter membrane the most as claimed in claim 1, it is characterised in that described
Organic solvent is DMF, N,N-dimethylacetamide, dimethyl sulfoxide, N-Methyl pyrrolidone, dichloromethane
Alkane, acetone, normal hexane, chloroform, oxolane, the one of acetonitrile.
5. the resistance to height that prepared by the preparation method of the high temperature resistant accurate molecular cut off ultrafilter membrane as described in any one of claim 1-4
The accurate molecular cut off ultrafilter membrane of temperature, its resistance to elevated temperatures is stable, it is possible to effectively catching molecular weight is the material of 2000-4000.
6. a high temperature resistant accurate molecular cut off ultrafilter membrane modifier solution, it is characterised in that its material composition is by cross-linking
Agent a and cross-linking agent b, solvent form, and wherein cross-linking agent a is Polyethylene Glycol 100, polyethylene glycol 200, PEG400, poly-second two
Alcohol 600, polyethylene glycol-800, cetomacrogol 1000, Macrogol 2000, Macrogol 3000, Macrogol 4000, poly-second two
Alcohol 6000, PEG 8000, PEG20000, PEG 20000, polyoxyethylene 50000, polyoxyethylene 100000,
Polyvinyl alcohol, ethylene glycol, methanol, ethanol, propanol, isopropanol, ethylenediamine, hexamethylene diamine, p-phenylenediamine, glucosan, glucose, shell
Polysaccharide, citric acid, piperazine, malic acid, polyacrylamide at least one, its consumption accounts for 0.05-3%；Cross-linking agent b is that silane is even
Connection agent KH550, silane coupler KH560, propanetriol-diglycidyl-ether, polyethyleneglycol diglycidylether, polypropylene glycol two contract
Water glycerin ether, formaldehyde, Biformyl, glutaraldehyde, methacrylic acid, trimethylolpropane, petroleum ether, glycerol, at least one, its
Consumption accounts for 1-10%；Remaining is solvent.
High temperature resistant accurate molecular cut off ultrafilter membrane modifier solution the most as claimed in claim 6, it is characterised in that described
Solvent be DMF, N,N-dimethylacetamide, dimethyl sulfoxide, N-Methyl pyrrolidone, dichloromethane,
Acetone, normal hexane, chloroform, oxolane, toluene, benzene, dimethylbenzene, chlorobenzene, water, acetonitrile at least one.
High temperature resistant accurate molecular cut off ultrafilter membrane modifier solution the most as claimed in claim 6, it is characterised in that described
Modifying agent pH value be 4-6, it adds acid in preparation process and is adjusted, and acid therein is perchloric acid, concentrated sulphuric acid, dense
At least one of nitric acid.
9. the preparation side of the high temperature resistant accurate molecular cut off ultrafilter membrane modifier solution as described in any one of claim 6-8
Method, it is characterised in that join in solvent by cross-linking agent a and cross-linking agent b, adjusts temperature and is 45-55 DEG C, stirring and dissolving, and will
After its clarification, it is thus achieved that transparency liquid, regulation pH value is 4-6, it is thus achieved that.
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| CN111467979B (en) * | 2020-04-29 | 2021-08-20 | 高浩然 | Preparation method of polysulfone photocatalytic ultrafiltration membrane material for wastewater treatment |
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