CN102806020A - Preparation method of high-flux tubular microfiltration membrane - Google Patents
Preparation method of high-flux tubular microfiltration membrane Download PDFInfo
- Publication number
- CN102806020A CN102806020A CN2012103134210A CN201210313421A CN102806020A CN 102806020 A CN102806020 A CN 102806020A CN 2012103134210 A CN2012103134210 A CN 2012103134210A CN 201210313421 A CN201210313421 A CN 201210313421A CN 102806020 A CN102806020 A CN 102806020A
- Authority
- CN
- China
- Prior art keywords
- tube type
- type filter
- membrane
- nonwoven
- preparation
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a preparation method of a high-flux tubular microfiltration membrane. The preparation method comprises preparing a membrane casting liquid and forming a membrane through phase inversion, and comprises the following specific steps of: mixing polyvinylidene fluoride, a pore-foaming agent, an additive and a solvent, heating to 30-80 DEG C, and stirring at the constant stirring speed of 100-1,000 revolutions per minute at a constant temperature for 10-48 hours to obtain a membrane casting liquid; standing the membrane casting liquid under the vacuum condition for defoaming for 10-48 hours, and winding a non-woven fabric into a non-woven fabric support pipe by using an integral tubular coating machine while completing membrane coating to obtain a tubular microfiltration basement membrane; and soaking the tubular microfiltration basement membrane into a coagulating bath, and performing phase inversion to obtain a finished tubular microfiltration membrane. The tubular microfiltration membrane has the characteristics of simple preparation process, high membrane flux, uniform pore diameter distribution, high mechanical strength, high chemical tolerance and the like.
Description
Technical field
The invention belongs to the polymeric membrane for separation technical field, particularly a kind of preparation method of high flux tube type filter membrance.
Background technology
Ultra/micro-filtration technology is as a kind of membrane separation technique; Mostly its film is the porous dissymmetrical structure; Filter process is to be mass transfer power with the both sides differential pressure of membrane, and a kind of separation process so that the mechanical grading principle is the basis has normal-temperature operation; Process does not have characteristics such as phase transformation, energy consumption are low, separation accuracy height, is used widely at aspects such as drink water purifying, water for industrial use processing, beverage, biology, food, medicine, environmental protection, chemical industry, metallurgy, oil at present.
Kynoar (PVDF) is a kind of crystalline polymer of function admirable; Mechanical strength, radiation hardness characteristic, resistance tocrocking and the hear resistance of its outstanding chemical stability, excellence; Make PVDF become a kind of material of desirable inversion of phases film forming, be widely used in preparing porous film material.
The scientific research personnel furthers investigate the PVDF film forming both at home and abroad in recent years, and great majority are confined to the research of doughnut and flat surpassing/micro-filtration membrane, and prepared film product is loose structure, even aperture distribution.Because the restriction of doughnut and dull and stereotyped membrane structure, runner is narrow but in actual use; Bad mechanical strength must have the preliminary treatment of strictness before filtering, and doughnut and the flat sheet membrane pressure loss are bigger; Should not handle that height contains admittedly, full-bodied feed liquid system; Pollute caudacoria cleaning, flux recovery difficulty, life cycle is short, and film is changed frequently.Mostly pvdf membrane is milipore filter in the market, and the aperture is little, and flux is low, is prone to pollute, and has greatly limited the commercial Application of pvdf membrane.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high flux tube type filter membrance; The tube type filter membrance flux of gained is high, applied range; Have favorable mechanical performance and chemical resistance, possess open runner, the runner scope is at 5 ~ 25mm; Antipollution is applicable to high viscosity, high solids content system.Said preparation method's technology is simple, membrane aperture is controlled, cost is low, be convenient to suitability for industrialized production.
The preparation method of high flux tube type filter membrance according to the invention is characterized in that comprising the steps:
A. prepare casting solution: with Kynoar, pore-foaming agent, additive and solvent, stirring is dissolved each component fully, obtains casting solution according to prescription;
Said casting solution is formulated by mass percentage by following component:
Kynoar 5 ~ 32%,
Pore-foaming agent 1 ~ 18%,
Additive 1 ~ 22%,
Solvent 28 ~ 93%;
The relative molecular weight of said Kynoar is 200,000 ~ 1,000,000.
Said pore-foaming agent is the mixture of one or more arbitrary proportions in polyvinylpyrrolidone, polyethylene glycol, acetone, ethanol, ethylene glycol, diglycol, the water, and the relative molecular weight of said polyethylene glycol is 200 ~ 60000;
Said additive is the mixture of one or more arbitrary proportions in silica, calcium carbonate, titanium dioxide, alundum (Al, lithium chloride, ammonium chloride, the polyethylene, and the average grain diameter of additive is 0.01 ~ 5 μ m;
Said solvent is selected from N-methyl pyrrolidone, N, dinethylformamide, N, the mixed liquor of one or both arbitrary proportions in N-dimethylacetylamide, the dimethyl sulfoxide (DMSO);
B. above-mentioned casting solution is placed on the integral type tubular type film applicator with nonwoven leaving standstill under the vacuum condition to complete deaeration, accomplish when nonwoven is rolled into tubulose and film, obtain the tube type filter membrance basement membrane;
C. the tube type filter membrance basement membrane for preparing among the step B is left standstill 10 ~ 60 seconds to evaporate its surperficial partial solvent in air; Then immerse in the coagulating bath rapidly; Utilize phase inversion, the casting film liquid layer that nonwoven surface applies be separated formation diffusion barrier, i.e. tube type filter membrance finished product.
In the steps A, mixed each component water-bath is heated under 30 ~ 80 ℃ the condition, stirs and make it to dissolve fully.
In the steps A, be the mixing speed with 100 ~ 1000r/min, constant speed constant temperature stirred 10 ~ 48 hours, and each component is dissolved fully.
10 ~ 48 hours time that casting solution leaves standstill under vacuum condition among the step B.
Among the step B, the overlapping junction of the nonwoven of said nonwoven stay pipe adopts ultrasonic bonding to fix, and utilizes the mechanical vibrational energy of ultrasonic frequency to make the fusing of nonwoven overlapping generation high-temperature interface, thereby welds together.
The pipe diameter of said nonwoven stay pipe is 5 ~ 25mm.
Among the step B, said casting solution is coated in the inner surface or the outer surface of nonwoven stay pipe.
Existing any one nonwoven all is applicable to the present invention.
Said phase inversion is meant that the non-solvent of homogeneous casting solution and its polymer contacts, and said non-solvent can mix with arbitrary proportion with this casting solution solvent; Exchange through the solvent at interface and the diffusion of non-solvent, cause being separated of this casting film liquid layer, thereby produce supermicro filtration membrane.
The adding of said pore-foaming agent and additive, one side has changed the chemical potential of solvent, influences the solvability of solvent; Change the macromolecular dissolved state of Kynoar in the casting solution on the other hand, and then influenced the counterdiffusion speed between the solvent and water in the phase inversion process, thereby made film have good pore structure, helped the formation of large aperture membrane structure.
Coagulating bath among the step C is selected from a kind of in deionized water, distilled water, pure water, alcoholic solution, the solvent aqueous solution, and coagulation bath temperature is 0 ~ 50 ℃, and soak time is 2 ~ 10 days;
Alcohol in the said alcoholic solution is selected from a kind of in ethanol, propyl alcohol, the n-butanol, and the mass concentration of alcoholic solution is 10 ~ 80%;
Solvent in the said solvent aqueous solution is selected from N-methyl pyrrolidone, N, dinethylformamide, N, and a kind of in N-dimethylacetylamide, the dimethyl sulfoxide (DMSO), wherein the mass concentration of solvent is 10 ~ 80%.
High flux tube type filter membrance according to the invention is to do supporter with the nonwoven stay pipe, at the diffusion barrier of its surface-coated 0.1 ~ 0.25 μ m, this separating layer by the upper strata as thin as a wafer the open porous supporting layer of compacted zone and lower floor constitute.High pressure resistant, intensity is high, filter efficiency good, membrane flux is high and stable.
Said integral type tubular type film applicator comprises central shaft, casting film flow container, transmission rolling shaft; The casting film flow container is positioned at the central shaft top; Transmission rolling shaft is positioned at the both sides up and down of the right-hand member of central shaft, and is provided with the gap between the two; Nonwoven rotates automatic the winding with central shaft and is rolled into tubulose under the drive of transmission rolling shaft, form the nonwoven stay pipe, and the overlapping junction of its nonwoven adopts ultrasonic bonding to fix.When nonwoven is rolled into the nonwoven stay pipe, casting solution evenly is coated on nonwoven stay pipe surface, the tube type filter membrance basement membrane that obtains, tube type filter membrance basement membrane get into the coagulating tank transfer tube type filter membrance that coordinates.
The detection method of film pure water flux is among the present invention:
With electrical conductivity less than 10 μ mcm
-1, turbidity injects head tank less than the pure water of 0.1NTU, water temperature remains on 25 ℃.Start water pump, make pure water pass through tubular membrane, regulate transmembrane pressure 0.1MPa, stablize area, the interior pure water flux of unit interval of the tubular membrane of determinator behind the 15min.By formula calculate:
F=Q/A×1000
In the formula:
The pure water flux of F---film, L/m
2H
The pure water transit dose of the film of Q---unit interval, m
3/ h
A---effective film area, m
2
The present invention has following advantage:
A. the present invention is a kind of micro-filtration membrane preparation method based on phase inversion, and prepared tube type filter membrance has even aperture distribution, high, the applied range of membrane flux, characteristics such as favorable mechanical performance and chemical resistance.
B. compare with flat sheet membrane with hollow-fibre membrane, its open wide runner of tubular membrane can significantly improve the tube type filter membrance antifouling property, makes it be applicable to that more high viscosity, height contain system admittedly.
C. the present invention compares with other preparation methods, has that preparation technology is simple, membrane aperture is controlled, cost is low, be convenient to characteristics such as suitability for industrialized production.
D. the present invention is that the research and development of large aperture, high flux tube type filter membrance provide a kind of new thinking.
Description of drawings: Fig. 1 high flux tube type filter membrance electromicroscopic photograph.
Fig. 2 integral type tubular type film applicator structural representation;
Wherein 1 is central shaft, the 2nd, and nonwoven, the 3rd, casting film liquid bath, the 4th, transmission rolling shaft, the 5th, tube type filter membrance basement membrane, the 6th, coagulating tank, 7 wave welding head of ultrasonic wave.
The specific embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1:
Mass percent is consisted of 5% Kynoar, 8% polyvinylpyrrolidone, 2% calcium carbonate places there-necked flask; Add 85% N again; Dinethylformamide mixes each component, and water-bath is heated to 60 ℃, stirs 12 hours with the mixing speed constant speed constant temperature of 400r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 25 ℃ the pure water coagulating bath and soaked 3 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 939L/m
2H.
Embodiment 2:
Mass percent is consisted of 10% Kynoar, 6% polyvinylpyrrolidone, 5% ethylene glycol; 2% water, 2% silica places there-necked flask, adds 75% N again; The N-dimethylacetylamide mixes each component, and water-bath is heated to 60 ℃, stirs 18 hours with the mixing speed constant speed constant temperature of 300r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 25 ℃ the pure water coagulating bath and soaked 5 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 815L/m
2H.
Embodiment 3:
Mass percent is consisted of 12% Kynoar, 10% polyvinylpyrrolidone, 5% acetone; 2% ammonium chloride places there-necked flask, adds 71% N again, and the N-dimethylacetylamide mixes each component; Water-bath is heated to 50 ℃; Mixing speed constant speed constant temperature with 300r/min stirred 16 hours, and each component is fully mixed, and obtained casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 25 ℃ the distilled water coagulating bath and soaked 4 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 886L/m
2H.
Embodiment 4:
Mass percent is consisted of 18% Kynoar, 3% diglycol, 4% acetone; 2% alundum (Al places there-necked flask; Add 73% N-methyl pyrrolidone again each component is mixed, water-bath is heated to 65 ℃, stirs 22 hours with the mixing speed constant speed constant temperature of 200r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; Surface coating outside when nonwoven is rolled into tubulose, the overlapping junction of its nonwoven obtains the tube type filter membrance basement membrane through ultrasonic bonding; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 25 ℃ the 30%N-methyl pyrrolidone aqueous coagulation bath and soaked 2 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 694L/m
2H.
Embodiment 5:
Mass percent is consisted of 22% Kynoar, 3% polyvinylpyrrolidone, 10% Macrogol 600; 2% ammonium chloride places there-necked flask, adds 63% N again, and the N-dimethylacetylamide mixes each component; Water-bath is heated to 50 ℃; Mixing speed constant speed constant temperature with 600r/min stirred 12 hours, and each component is fully mixed, and obtained casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be 25 ℃ 30%N, soaked 5 days in the N-dimethylacetylamide aqueous coagulation bath, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 759L/m
2H.
Embodiment 6:
Mass percent is consisted of 18% Kynoar, 8% polyvinylpyrrolidone, 6% ethanol; 2% lithium chloride places there-necked flask, adds 66% N again, and dinethylformamide mixes each component; Water-bath is heated to 60 ℃; Mixing speed constant speed constant temperature with 400r/min stirred 24 hours, and each component is fully mixed, and obtained casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 45 ℃ the 20% ethanolic solution coagulating bath and soaked 4 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 706L/m
2H.
Embodiment 7:
Mass percent is consisted of 14% Kynoar, 7% polyvinylpyrrolidone, 6% Macrogol 2000; 4% water, 2% ammonium chloride places there-necked flask, adds 67% N again; Dinethylformamide mixes each component, and water-bath is heated to 60 ℃, stirs 24 hours with the mixing speed constant speed constant temperature of 300r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 18 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 25 ℃ the pure water coagulating bath and soaked 5 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 1082L/m
2H.
Embodiment 8:
Mass percent is consisted of 24% Kynoar, 6% diglycol, 2% titanium dioxide places there-necked flask; Add 68% N again; Dinethylformamide mixes each component, and water-bath is heated to 60 ℃, stirs 16 hours with the mixing speed constant speed constant temperature of 500r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be 25 ℃ 60%N, soaked 4 days in the dinethylformamide aqueous coagulation bath, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 919L/m
2H.
Embodiment 9:
Mass percent is consisted of 22% Kynoar, 8% polyvinylpyrrolidone, 6% PEG400; 2% silica places there-necked flask; Add 62% dimethyl sulfoxide (DMSO) again each component is mixed, water-bath is heated to 60 ℃, stirs 18 hours with the mixing speed constant speed constant temperature of 400r/min; Each component is fully mixed, obtain casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 5 ℃ the pure water coagulating bath and soaked 2 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 648L/m
2H.
Embodiment 10:
Mass percent is consisted of 32% Kynoar, 12% acetone, 6% Macrogol 2000; 2% silica places there-necked flask, adds 48% N again, and dinethylformamide mixes each component; Water-bath is heated to 40 ℃; Mixing speed constant speed constant temperature with 400r/min stirred 22 hours, and each component is fully mixed, and obtained casting solution; Casting solution was left standstill 24 hours at the vacuum condition lower seal; Place on the integral type tubular type film applicator with nonwoven after the deaeration fully; At inner surface coating, the overlapping junction of its nonwoven obtained the tube type filter membrance basement membrane through ultrasonic bonding when nonwoven was rolled into tubulose; After subsequently the tube type filter membrance basement membrane being left standstill 10 ~ 60 seconds in air, immerse temperature rapidly and be in 40 ℃ the distilled water coagulating bath and soaked 2 days, phase inversion forms the tube type filter membrance finished product.
According to conventional film properties evaluation method, be that 0.1MPa, temperature are under 25 ℃ at pressure, the pure water flux of this film is 624L/m
2H.
Claims (8)
1. the preparation method of a high flux tube type filter membrance is characterized in that comprising the steps:
A. prepare casting solution: with Kynoar, pore-foaming agent, additive and solvent, stirring is dissolved each component fully, obtains casting solution;
Said casting solution is formulated by mass percentage by following component:
Kynoar 5 ~ 32%,
Pore-foaming agent 1 ~ 18%,
Additive 1 ~ 22%,
Solvent 28 ~ 93%;
The relative molecular weight of said Kynoar is 200,000 ~ 1,000,000;
Said pore-foaming agent is the mixture of one or more arbitrary proportions in polyvinylpyrrolidone, polyethylene glycol, acetone, ethanol, ethylene glycol, diglycol, the water, and the relative molecular weight of said polyethylene glycol is 200 ~ 60000;
Said additive is the mixture of one or more arbitrary proportions in silica, calcium carbonate, titanium dioxide, alundum (Al, lithium chloride, ammonium chloride, the polyethylene, and the average grain diameter of additive is 0.01 ~ 5 μ m;
Said solvent is selected from N-methyl pyrrolidone, N, dinethylformamide, N, the mixed liquor of one or both arbitrary proportions in N-dimethylacetylamide, the dimethyl sulfoxide (DMSO);
B. above-mentioned casting solution is placed on the integral type tubular type film applicator with nonwoven leaving standstill under the vacuum condition to complete deaeration, accomplish when nonwoven is rolled into the nonwoven stay pipe and film, obtain the tube type filter membrance basement membrane;
C. the tube type filter membrance basement membrane for preparing among the step B is left standstill 10 ~ 60 seconds to evaporate its surperficial partial solvent in air; Then immerse in the coagulating bath rapidly; Utilize phase inversion, the casting film liquid layer that nonwoven surface applies be separated formation diffusion barrier, i.e. tube type filter membrance finished product.
2. the preparation method of high flux tube type filter membrance according to claim 1 is characterized in that in the steps A, mixed each component water-bath is heated under 30 ~ 80 ℃ the condition, stirs to make it to dissolve fully.
3. the preparation method of high flux tube type filter membrance according to claim 1 and 2 is characterized in that in the steps A, stirs 10 ~ 48 hours with the mixing speed constant speed constant temperature of 100 ~ 1000r/min, and each component is dissolved fully.
4. the preparation method of high flux tube type filter membrance according to claim 1 is characterized in that 10 ~ 48 hours time that casting solution leaves standstill among the step B under vacuum condition.
5. the preparation method of high flux tube type filter membrance according to claim 1 is characterized in that the overlapping junction of nonwoven of nonwoven stay pipe among the step B adopts ultrasonic bonding to fix.
6. according to the preparation method of claim 1 or 5 described high flux tube type filter membrances, the diameter that it is characterized in that said nonwoven stay pipe is 5 ~ 25mm.
7. according to the preparation method of claim 1,5 or 6 described high flux tube type filter membrances, it is characterized in that among the step B that said casting solution is coated in the inner surface or the outer surface of nonwoven stay pipe.
8. the preparation method of high flux tube type filter membrance according to claim 1; It is characterized in that coagulating bath among the step C is selected from a kind of in deionized water, distilled water, pure water, alcoholic solution, the solvent aqueous solution; Coagulation bath temperature is 4 ~ 50 ℃, and soak time is 2 ~ 10 days;
Alcohol in the said alcoholic solution is selected from a kind of in ethanol, propyl alcohol, the n-butanol, and the mass concentration of alcoholic solution is 10-80%;
Solvent in the said solvent aqueous solution is selected from N-methyl pyrrolidone, N, dinethylformamide, N, and a kind of in N-dimethylacetylamide, the dimethyl sulfoxide (DMSO), wherein the mass concentration of solvent is 10 ~ 80%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103134210A CN102806020A (en) | 2012-08-30 | 2012-08-30 | Preparation method of high-flux tubular microfiltration membrane |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103134210A CN102806020A (en) | 2012-08-30 | 2012-08-30 | Preparation method of high-flux tubular microfiltration membrane |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102806020A true CN102806020A (en) | 2012-12-05 |
Family
ID=47229995
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2012103134210A Pending CN102806020A (en) | 2012-08-30 | 2012-08-30 | Preparation method of high-flux tubular microfiltration membrane |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102806020A (en) |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028108A (en) * | 2014-06-24 | 2014-09-10 | 江苏凯米膜科技股份有限公司 | Method for preparing tubular micro-porous filter membrane |
| CN104404726A (en) * | 2014-10-28 | 2015-03-11 | 北京碧水源膜科技有限公司 | Porous detachable RF (Reinforced polyvinylidene fluoride filtration) film silk coating device and coating machine comprising coating device |
| CN104923090A (en) * | 2015-07-06 | 2015-09-23 | 翟锦树 | Method for preparing internal pressure macromolecule tubular microfiltration membrane |
| CN105439888A (en) * | 2015-12-14 | 2016-03-30 | 广东创源节能环保有限公司 | Method and device for solving obstruction problems of distillation column and rectifying tower in synthetic leather DMF waste liquid recovery |
| CN106268327A (en) * | 2016-09-21 | 2017-01-04 | 苏州凯虹高分子科技有限公司 | A kind of preparation method of high temperature resistant tube type filter membrance |
| CN106731328A (en) * | 2016-11-25 | 2017-05-31 | 浙江绿净环保科技有限公司 | A kind of two-layer compound air-filtering membrane and its preparation technology |
| CN106890571A (en) * | 2017-03-06 | 2017-06-27 | 江苏凯米膜科技股份有限公司 | A kind of preparation method of organic tubular nanofiltration membrane |
| CN108261931A (en) * | 2018-03-26 | 2018-07-10 | 四川美富特水务有限责任公司 | A kind of preparation method of polyvinylidene fluoride microporous filtering film |
| CN109078502A (en) * | 2018-08-15 | 2018-12-25 | 新疆水处理工程技术研究中心有限公司 | A kind of production method of casting solution, casting film liquor manufacture method and tubular membrane |
| CN110898668A (en) * | 2019-11-22 | 2020-03-24 | 江苏凯米膜科技股份有限公司 | Method for preparing organic tubular nanofiltration membrane by phase inversion method and nanofiltration membrane |
| CN111760471A (en) * | 2020-07-03 | 2020-10-13 | 江苏峰科达科技有限公司 | Alkali-resistant backwashing tubular membrane element and tubular membrane assembly thereof |
| CN111905572A (en) * | 2020-07-14 | 2020-11-10 | 江苏千里膜业科技有限公司 | Preparation method of MBR (membrane bioreactor) flat dry film for domestic sewage treatment |
| CN112316736A (en) * | 2020-10-26 | 2021-02-05 | 武汉工程大学 | Method for preparing tubular composite membrane by limited space phase inversion, external coating device, internal coating device and composite membrane |
| CN115010214A (en) * | 2022-06-30 | 2022-09-06 | 成都美富特膜环保科技有限公司 | Sewage treatment membrane, preparation method of sewage treatment membrane and membrane separation equipment |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2996304B2 (en) * | 1989-07-12 | 1999-12-27 | 東レ株式会社 | Manufacturing method of separation membrane |
| CN101279211A (en) * | 2008-01-11 | 2008-10-08 | 北京工业大学 | Preparation of polyvinylidene fluoride dewatering microporous film |
| EP2145675A1 (en) * | 2007-03-23 | 2010-01-20 | Kureha Corporation | Vinylidene fluoride resin hollow-fiber porous membrane and process for production of the same |
| CN102527247A (en) * | 2011-12-08 | 2012-07-04 | 江苏凯米膜科技股份有限公司 | Strong acid and strong alkali resistance organic tubular membrane and preparation method thereof, and membrane casting liquid |
-
2012
- 2012-08-30 CN CN2012103134210A patent/CN102806020A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2996304B2 (en) * | 1989-07-12 | 1999-12-27 | 東レ株式会社 | Manufacturing method of separation membrane |
| EP2145675A1 (en) * | 2007-03-23 | 2010-01-20 | Kureha Corporation | Vinylidene fluoride resin hollow-fiber porous membrane and process for production of the same |
| CN101279211A (en) * | 2008-01-11 | 2008-10-08 | 北京工业大学 | Preparation of polyvinylidene fluoride dewatering microporous film |
| CN102527247A (en) * | 2011-12-08 | 2012-07-04 | 江苏凯米膜科技股份有限公司 | Strong acid and strong alkali resistance organic tubular membrane and preparation method thereof, and membrane casting liquid |
Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104028108A (en) * | 2014-06-24 | 2014-09-10 | 江苏凯米膜科技股份有限公司 | Method for preparing tubular micro-porous filter membrane |
| CN104028108B (en) * | 2014-06-24 | 2016-02-17 | 江苏凯米膜科技股份有限公司 | A kind of preparation method of tube-type micropore filter membrane |
| CN104404726A (en) * | 2014-10-28 | 2015-03-11 | 北京碧水源膜科技有限公司 | Porous detachable RF (Reinforced polyvinylidene fluoride filtration) film silk coating device and coating machine comprising coating device |
| CN104923090A (en) * | 2015-07-06 | 2015-09-23 | 翟锦树 | Method for preparing internal pressure macromolecule tubular microfiltration membrane |
| CN105439888A (en) * | 2015-12-14 | 2016-03-30 | 广东创源节能环保有限公司 | Method and device for solving obstruction problems of distillation column and rectifying tower in synthetic leather DMF waste liquid recovery |
| CN106268327A (en) * | 2016-09-21 | 2017-01-04 | 苏州凯虹高分子科技有限公司 | A kind of preparation method of high temperature resistant tube type filter membrance |
| CN106731328A (en) * | 2016-11-25 | 2017-05-31 | 浙江绿净环保科技有限公司 | A kind of two-layer compound air-filtering membrane and its preparation technology |
| CN106890571A (en) * | 2017-03-06 | 2017-06-27 | 江苏凯米膜科技股份有限公司 | A kind of preparation method of organic tubular nanofiltration membrane |
| CN108261931A (en) * | 2018-03-26 | 2018-07-10 | 四川美富特水务有限责任公司 | A kind of preparation method of polyvinylidene fluoride microporous filtering film |
| CN109078502A (en) * | 2018-08-15 | 2018-12-25 | 新疆水处理工程技术研究中心有限公司 | A kind of production method of casting solution, casting film liquor manufacture method and tubular membrane |
| CN110898668A (en) * | 2019-11-22 | 2020-03-24 | 江苏凯米膜科技股份有限公司 | Method for preparing organic tubular nanofiltration membrane by phase inversion method and nanofiltration membrane |
| CN111760471A (en) * | 2020-07-03 | 2020-10-13 | 江苏峰科达科技有限公司 | Alkali-resistant backwashing tubular membrane element and tubular membrane assembly thereof |
| CN111905572A (en) * | 2020-07-14 | 2020-11-10 | 江苏千里膜业科技有限公司 | Preparation method of MBR (membrane bioreactor) flat dry film for domestic sewage treatment |
| CN112316736A (en) * | 2020-10-26 | 2021-02-05 | 武汉工程大学 | Method for preparing tubular composite membrane by limited space phase inversion, external coating device, internal coating device and composite membrane |
| CN115010214A (en) * | 2022-06-30 | 2022-09-06 | 成都美富特膜环保科技有限公司 | Sewage treatment membrane, preparation method of sewage treatment membrane and membrane separation equipment |
| CN115010214B (en) * | 2022-06-30 | 2024-03-29 | 成都美富特膜环保科技有限公司 | Sewage treatment membrane, preparation method of sewage treatment membrane and membrane separation equipment |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102806020A (en) | Preparation method of high-flux tubular microfiltration membrane | |
| CN102698614B (en) | Tubular nanofiltration membrane with multi-layer structure and preparation method thereof | |
| CN104492284B (en) | A kind of two-sided dissymmetrical structure flat support film and its preparation method and application | |
| CN104474919B (en) | A kind of high performance flat formula cellulose acetate/Graphene is blended forward osmosis membrane | |
| CN105709619B (en) | A kind of positively charged nanofiltration membranes and preparation method thereof | |
| CN103223302B (en) | Preparation method of self-assembly covalent cross-linked sodium filter membrane | |
| CN107020020A (en) | A kind of preparation method of new MOFs PVDF composite membranes | |
| CN103657449B (en) | The preparation method of Novel hydrophilic hollow fiber membrane | |
| CN110523281A (en) | A kind of polyamide doughnut receives the preparation method of permeable membrane | |
| CN104437124B (en) | A kind of self-cleaning type polyvinylidene fluoride microporous film and preparation method thereof | |
| CN105617875A (en) | High-throughput hollow fiber composite nanofiltration membrane, and preparation method thereof | |
| CN106474942B (en) | The preparation method of hollow fiber ultrafiltration membrane | |
| JP2009536573A (en) | Porous composite membrane material and its application | |
| CN104147943A (en) | Preparation method and application of high-molecular forward osmosis membrane | |
| CN102824859B (en) | Method for preparing hollow fiber nanofiltration membrane by using thermally induced phase separation/interface cross linking synchronization method | |
| CN105597552A (en) | Forward osmosis membrane with high water flux and high salt rejection rate and method for preparing forward osmosis membrane with one-step method | |
| CN102389722A (en) | Method for preparing nano composite ultrafiltration membrane by using polyaniline nano material | |
| CN102343225A (en) | Preparation method of polyaniline (PANI) composite ultrafiltration membrane | |
| CN104923086A (en) | Semi-aromatic polyamide compound reverse osmosis membrane and preparation method thereof | |
| CN108704482A (en) | A kind of antipollution hollow fiber ultrafiltration membrane | |
| CN104492285B (en) | Antipollution, high-flux ultra-filtration membrane and preparation method thereof and casting solution used | |
| CN101733023A (en) | Method for manufacturing polyvinylidene fluoride hollow fiber membrane | |
| Tang et al. | A novel positively charged asymmetry membranes from poly (2, 6-dimethyl-1, 4-phenylene oxide) by benzyl bromination and in situ amination: membrane preparation and characterization | |
| CN103495348A (en) | Polyvinyl chloride hollow fiber ultrafiltration membrane and preparation method thereof | |
| CN101422706A (en) | Preparation method of co-mixing polyvinylidene fluoride hollow fiber membrane with improved hydrophilicity |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20121205 |