CN105169972A - Hollow fiber nanofiltration membrane and preparation method for producing hollow fiber nanofiltration membrane - Google Patents
Hollow fiber nanofiltration membrane and preparation method for producing hollow fiber nanofiltration membrane Download PDFInfo
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- CN105169972A CN105169972A CN201510639479.8A CN201510639479A CN105169972A CN 105169972 A CN105169972 A CN 105169972A CN 201510639479 A CN201510639479 A CN 201510639479A CN 105169972 A CN105169972 A CN 105169972A
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Abstract
The invention relates to a hollow fiber nanofiltration membrane. The hollow fiber nanofiltration membrane comprises a supporting tube, a nano-fiber base layer and a nanofiltration separation layer. The invention further relates to a preparation method for producing the hollow fiber nanofiltration membrane. The preparation method comprises steps as follows: S1: the outer surface of the supporting tube is coated with the nano-fiber base layer; S2: the supporting tube is washed with ionized water and dried for standby use; S3: the treated supporting tube is soaked in a water-phase monomer solution and an organic phase monomer solution sequentially and then subjected to thermal treatment. The hollow fiber nanofiltration membrane has the benefits as follows: the hollow fiber nanofiltration membrane and the preparation method for producing the hollow fiber nanofiltration membrane are provided, the hollow fiber nanofiltration membrane has high mechanical performance, hydrophilia and water permeability, and the preparation method is simple in process and high in production efficiency.
Description
Technical field
The present invention relates to a kind of hollow fiber nanofiltration membrane and produce the preparation method of hollow fiber nanofiltration membrane.
Background technology
Nanofiltration-membrane technique is that recent domestic develops new membrane isolation technics faster.NF membrane is that one between milipore filter and reverse osmosis membrane is with pressure-actuated film.NF membrane has nano level membrane aperture, and in most cases with electric charge on film, so NF membrane operationally can retain the organic matter of divalence or multivalent ion and larger molecular weight, and allows monovalention to pass through.Therefore, based on the special performance of NF membrane, it is widely used in wastewater treatment, food industry, chemical and medicine industry industry and Drinking Water Industry etc.
Current most of business-like NF membrane is rolling NF membrane.Rolled film has poor, the more difficult cleaning of contamination resistance and to problems such as influent quality requirement are high.Compare rolling NF membrane, it is large that hollow fiber nanofiltration membrane has the process water yield, and the reference area of film is large, can carry out the advantages such as backwash.Thus effectively can improve the contamination resistance of film itself, and extend the service life of NF membrane.From the technology of preparing aspect of NF membrane, mainly containing phase inversion and composite algorithm, phase conversion method is at present that the NF membrane of preparation is comparatively simple, but the NF membrane of preparation has durability poor, the problems such as flux is lower.
The business-like NF membrane product of major part is all prepared by composite algorithm.The process of composite algorithm comprises the preparation of basement membrane and separating layer.Usually, basement membrane is preparation is by phase conversion method, and separating layer generally adopts interfacial polymerization to prepare.The basement membrane of preparation requires suitable aperture, pore-size distribution, porosity and chemical stability.General hollow fiber nanofiltration membrane is all adopt composite algorithm to be prepared, and make easily to peel off between supporting layer and separating layer, and overall flux is lower.
Summary of the invention
In view of the above-mentioned problems in the prior art, main purpose of the present invention is to address the deficiencies of the prior art, the invention provides a kind of hollow fiber nanofiltration membrane and produce the preparation method of hollow fiber nanofiltration membrane, this hollow fiber nanofiltration membrane has high mechanical property, hydrophily and water penetration, and this preparation method's technique is simple and production efficiency is high simultaneously.
The invention provides a kind of hollow fiber nanofiltration membrane, comprise stay pipe, nanofiber basic unit and nanofiltration separation layer, described nanometer dimension basic unit is arranged between described stay pipe and described nanofiltration separation layer, the external diameter of described stay pipe is 0.4 ~ 2.3mm, the wall thickness of described stay pipe is 0.1 ~ 0.7mm, and described stay pipe is inorganic or the stay pipe of organic polymer material braiding.
Optionally, the inorganic polymer material of described stay pipe is one or more in silk, copper wire, stainless steel wire, nickel foam, zirconia or alumina metals screen cloth.
Optionally, the organic polymer material of described stay pipe be that PETG, poly, PPTA, polyvinyl chloride, polyurethanes, polyamide, polypropylene are fine, one or more in polypropylene, polyethylene, polyvinyl formal.
Optionally, the material of described nanofiber basic unit be that polyamide, polyurethane, Merlon, polypropylene are fine, polyvinyl alcohol, PLA, polyoxyethylene, polymethyl methacrylate, polyester, polystyrene, polyvinyl chloride, polycaprolactone, cellulose acetate, collagen, polyphenyl miaow is frustrated, one or more in ammonium polyacrylate, polyvinylcarbazole or polyimides.
The present invention also provides a kind of method of producing hollow fiber nanofiltration membrane, comprises the following steps:
S1: prepare nanofiber basic unit by electrostatic spinning process at the outer surface of stay pipe;
S2: stay pipe outer surface being compounded with nanofiber basic unit carries out de-ionised water 20 ~ 40min, carries out drying process 6 ~ 10hrs, is positioned in hothouse for subsequent use after completing above-mentioned operation in the hothouse being placed on 40 ~ 80 DEG C afterwards;
S3: the stay pipe after step S2 process is immersed 60 ~ 480s in the aqueous phase monomers solution of 20 ~ 25 DEG C, top layer liquid is blotted after taking-up, then the organic phase monomer solution 60 ~ 300s of 25 DEG C is immersed, outer surface liquid is blotted after taking-up, then in the environment of 50 ~ 120 DEG C, heat-treat 1 ~ 30min, finally form hollow fiber nanofiltration membrane.
Optionally, prepare nanofiber basic unit by electrostatic spinning process in described step S1 specifically to comprise the following steps:
A1: selective polymer, by polymer melting or be dissolved in solvent, uniform stirring obtains melt or the solution of polymer.The concentration range of described melt or solution is: 5wt% ~ 100wt%;
A2: polymer spinning solution is injected in spinning syringe, adopt syringe needle electrospinning device to prepare layers of nanofibers, the operating voltage of described syringe needle electrospinning device is 10 ~ 100KV, and described syringe is 5 ~ 60cm to the distance of described collector;
A3: when using syringe needle electrospinning device, syringe needle is fixed and is evenly distributed on the outer ring of cylinder collector.Meanwhile, stay pipe is evenly arranged in the outer ring of cylinder type collector, and also press setting speed with rolling collector synchronous rotary and advance, and stay pipe tube body does not carry out spinning motion, nanofiber is wrapped in the outer surface of stay pipe uniformly.
Optionally, described solvent is the solvent dissolving close polymer, can be one or more in DMF, normal heptane, carrene, chloroform, cyclohexane, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide (DMSO), water, ethanol, glycerine, ethylene glycol, polyethylene glycol, dimethyl sulfoxide (DMSO), phenol, amide-type, triethanolamine, alcohol salt, urea, formic acid or acetic acid.
Optionally, described aqueous phase monomers solution is that a kind of in polynary amine is dissolved in the aqueous phase monomers solution formed in the aqueous solution, wherein polynary amine comprises aromatic series and aliphatic two class, described aromatic series comprises m-phenylene diamine (MPD), p-phenylenediamine (PPD), o-phenylenediamine, equal benzene three is pressed, 4-methylresorcinol diamines, m-phenylene diamine (MPD)-5-sulfonic acid, N, N-dimethyl-m-phenylenediamine and poly-m-aminophenyl ethene, described aliphatic comprises piperazine, 1,4-cyclohexanediamine, polyvinyl alcohol, shitosan, polyvinylamine and polyamines base polyoxyethylene.
Optionally, described organic phase monomer solution is that a kind of in acyl chlorides and isocyanates is dissolved in the organic phase monomer solution formed in alkane, wherein acyl chlorides and isocyanates include aromatic series and aliphatic two class, described aromatic series comprises paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, methylresorcinol vulcabond, 5-oxygen formyl chloride-isophthaloyl chlorine, 5-isocyanates-isophthaloyl chlorine and methylresorcinol vulcabond, described aliphatic comprises 1,3,5-cyclohexane three formyl chloride and 1,3,4-pentamethylene three acyl chlorides.
The present invention has the following advantages and beneficial effect: the invention provides a kind of hollow fiber nanofiltration membrane and produce the preparation method of hollow fiber nanofiltration membrane, this hollow fiber nanofiltration membrane adopts multi-layer supporting structure to prepare hollow fiber nanofiltration membrane, the inner high strength supporting tube structure that uses is as the inner standoff layer of hollow fiber nanofiltration membrane, at stay pipe superficies, pass through electrostatic spinning process, preparation layers of nanofibers is as the basic unit of hollow fiber nanofiltration membrane, finally interfacial polymerization method is adopted to prepare nanofiltration separation layer at the outermost layer of hollow fiber nanofiltration membrane, because layers of nanofibers is through Overheating Treatment and rolling technology, bonding strength between each layer obtains effective raising, this sandwich construction, greatly improving close-burning between each layer while, effectively can improve hydrophily and the permeable amount of film, owing to have employed electrostatic spinning process, the nanofiber basic unit of preparation has excellent porosity, permeable amount, the various problems that the composite nano fiber basic unit of simultaneously being prepared by electrostatic spinning process can effectively avoid ultrafiltration to produce as basement membrane, hollow fiber nanofiltration membrane function admirable provided by the invention, there is excellent hydrophily and contamination resistance simultaneously, flux can reach more than 40L/m2, is respectively >40% and >95% to the removal efficiency of monovalence and divalent salts, in addition, a kind of preparation method producing hollow fiber nanofiltration membrane provided by the invention, its technique is simple, is easy to operation, is applicable to industrial applications.
Accompanying drawing explanation
Fig. 1 is the structural representation of hollow fiber nanofiltration membrane provided by the invention;
Fig. 2 is the structural representation that surface provided by the invention is provided with the equipment of the production hollow fiber nanofiltration membrane of multiple stay pipe.
Detailed description of the invention
The present invention is further illustrated with specific embodiment below with reference to accompanying drawings.
As shown in Fig. 1 to 2: a kind of hollow fiber nanofiltration membrane of the embodiment of the present invention, comprises stay pipe 1, nanofiber basic unit 2 and nanofiltration separation layer 3, described nanometer dimension basic unit 2 is arranged between described stay pipe 1 and described nanofiltration separation layer 3, the external diameter of described stay pipe 1 is 0.4 ~ 2.3mm, the wall thickness of described stay pipe 1 is 0.1 ~ 0.7mm, described stay pipe 1 is inorganic or the stay pipe of organic polymer material braiding, and the inorganic polymer material of described stay pipe is silk, copper wire, stainless steel wire, nickel foam, one or more in zirconia or alumina metals screen cloth, the organic polymer material of described stay pipe is PETG, poly, PPTA, polyvinyl chloride, polyurethanes, polyamide, polypropylene is fine, polypropylene, polyethylene, one or more in polyvinyl formal, the material of described nanofiber basic unit is polyamide, polyurethane, Merlon, polypropylene is fine, polyvinyl alcohol, PLA, polyoxyethylene, polymethyl methacrylate, polyester, polystyrene, polyvinyl chloride, polycaprolactone, cellulose acetate, collagen, polyphenyl miaow are frustrated, ammonium polyacrylate, one or more in polyvinylcarbazole or polyimides, this hollow fiber nanofiltration membrane adopts multi-layer supporting structure to prepare hollow fiber nanofiltration membrane, the inner high strength supporting tube structure that uses is as the inner standoff layer of hollow fiber nanofiltration membrane, at stay pipe superficies, pass through electrostatic spinning process, preparation layers of nanofibers is as the basic unit of hollow fiber nanofiltration membrane, finally interfacial polymerization method is adopted to prepare nanofiltration separation layer at the outermost layer of hollow fiber nanofiltration membrane, because layers of nanofibers is through Overheating Treatment and rolling technology, the bonding strength between each layer obtains effective raising, this sandwich construction, greatly improving close-burning between each layer while, effectively can improve hydrophily and the permeable amount of film, owing to have employed electrostatic spinning process, the nanofiber basic unit of preparation has excellent porosity, permeable amount, the various problems that the composite nano fiber basic unit of simultaneously being prepared by electrostatic spinning process can effectively avoid ultrafiltration to produce as basement membrane, hollow fiber nanofiltration membrane function admirable provided by the invention, there is excellent hydrophily and contamination resistance simultaneously, flux can reach more than 40L/m2, is respectively >40% and >95% to the removal efficiency of monovalence and divalent salts.
The present invention also provides a kind of equipment producing hollow fiber nanofiltration membrane, comprise spinning syringe 200 and syringe needle electrospinning device 100, described spinning syringe 200 is arranged on the top of described syringe needle electrospinning device, described syringe needle electrospinning device comprises main shaft 10 and cylinder collector 20, described cylinder collector 20 is arranged on described main shaft 10, described main shaft is connected with external power source, the outside two ends of described cylinder collector be circumferentially provided with multiple equally distributed electrostatic spinning syringe needle 30, described main shaft is connected with outside motor, described cylinder collector along the circumferential direction rotates under the drive of main shaft, the exterior periphery direction of described cylinder collector 20 is evenly provided with multiple described stay pipe vertically, stay pipe completes spinning technique on cylinder collector 20, technique is simple and operating efficiency is high, improve the production efficiency of enterprise, further enhancing the competitiveness of enterprise.
The present invention also provides the present invention also to provide a kind of preparation method producing hollow fiber nanofiltration membrane, comprises the following steps: S1: prepare nanofiber basic unit at the outer surface of stay pipe by electrostatic spinning process; S2: stay pipe outer surface being compounded with nanofiber basic unit carries out de-ionised water 20 ~ 40min, carries out drying process 6 ~ 10hrs, is positioned in hothouse for subsequent use after completing above-mentioned operation in the hothouse being placed on 40 ~ 80 DEG C afterwards; S3: the stay pipe after step S2 process is immersed 60 ~ 480s in the aqueous phase monomers solution of 20 ~ 25 DEG C, top layer liquid is blotted after taking-up, then the organic phase monomer solution 60 ~ 300s of 25 DEG C is immersed, outer surface liquid is blotted after taking-up, then in the environment of 50 ~ 120 DEG C, heat-treat 1 ~ 30min, finally form hollow fiber nanofiltration membrane; Prepare nanofiber basic unit by electrostatic spinning process in described step S1 specifically to comprise the following steps: A1: selective polymer, by polymer melting or be dissolved in solvent, uniform stirring obtains melt or the solution of polymer.The concentration range of described melt or solution is: 5wt% ~ 100wt%, A2: polymer spinning solution is injected in spinning syringe, syringe needle electrospinning device is adopted to prepare layers of nanofibers, wherein: as shown in Figure 2, shown syringe needle electrospinning device 100 comprises main shaft 10 and cylinder receiver 20, described main shaft is connected with outside power supply, described cylinder receiver to be arranged on described main shaft 10 and along the circumferential direction to rotate under the drive of main shaft, described cylinder receiver 20 two ends be circumferentially provided with equally distributed electrostatic spinning syringe needle 30, the operating voltage of described syringe needle electrospinning device is 10 ~ 100KV, described spinning syringe is 5 ~ 60cm to the vertical range of described cylinder collector, A3: when using syringe needle electrospinning device, electrostatic spinning syringe needle is fixed and is evenly distributed on the outer ring of cylinder collector.Meanwhile, stay pipe is evenly arranged in the outer ring of cylinder type collector, and also press setting speed with rolling collector synchronous rotary and advance, and stay pipe self does not carry out spinning motion, nanofiber is wrapped in the outer surface of stay pipe uniformly; Described solvent is the solvent dissolving close polymer, can be one or more in DMF, normal heptane, carrene, chloroform, cyclohexane, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide (DMSO), water, ethanol, glycerine, ethylene glycol, polyethylene glycol, dimethyl sulfoxide (DMSO), phenol, amide-type, triethanolamine, alcohol salt, urea, formic acid or acetic acid; Described aqueous phase monomers solution is that a kind of in polynary amine is dissolved in the aqueous phase monomers solution formed in the aqueous solution, and wherein polynary amine comprises aromatic series and aliphatic two class, and described aromatic series comprises m-phenylene diamine (MPD), p-phenylenediamine (PPD), o-phenylenediamine, equal benzene three is pressed, 4-methylresorcinol diamines, m-phenylene diamine (MPD)-5-sulfonic acid, N, N-dimethyl-m-phenylenediamine and poly-m-aminophenyl ethene, described aliphatic comprises piperazine, Isosorbide-5-Nitrae-cyclohexanediamine, polyvinyl alcohol, shitosan, polyvinylamine and polyamines base polyoxyethylene; Described organic phase monomer solution is that a kind of in acyl chlorides and isocyanates is dissolved in the organic phase monomer solution formed in alkane, wherein acyl chlorides and isocyanates include aromatic series and aliphatic two class, described aromatic series comprises paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, methylresorcinol vulcabond, 5-oxygen formyl chloride-isophthaloyl chlorine, 5-isocyanates-isophthaloyl chlorine and methylresorcinol vulcabond, described aliphatic comprises 1,3,5-cyclohexane three formyl chloride and 1,3,4-pentamethylene three acyl chlorides; A kind of preparation method producing hollow fiber nanofiltration membrane provided by the invention, its technique is simple, is easy to operation, is applicable to industrial applications.
Embodiment 1
The first step passes through Advance in Manufacture of Nano-fibers by Electrospinning basic unit 2 at stay pipe 1 outer surface:
1,10g polyvinylpyrrolidone is dissolved in 100ml ethanol, obtains the polyvinylpyrrolidone homogeneous solution of 10%.Solution is joined in syringe, it is 9 μ l/min that described syringe setting pushes away speed, syringe is apart from golden Rotation of receiver cylinder 10cm, under 20V DC voltage, hydrophilic fiber is received on the stay pipe that is longitudinally travelled uniformly, the speed that is longitudinally travelled of woven tube is 10cm/min, and stay pipe body is without carrying out spinning motion;
2, the surface recombination obtained is had the stay pipe 1 of nanofiber basic unit 2 with by deionized water rinsing 20mins, 6hrs in the hothouse being positioned over 40 DEG C afterwards, is positioned in hothouse stand-by after completing above-mentioned operation.
Second step forms nanofiltration separation layer 3 at nanofiber basic unit 2 outer surface:
1, aqueous phase and organic phase solution is configured: 10g m-phenylene diamine (MPD) and 2g NaOH are dissolved in 150g water tank and configure aqueous phase solution, configure organic phase solution by 10 m-phthaloyl chloride solution 190g normal octanes;
2, carry out interfacial reaction at nanofiber basic unit 2 outer surface and prepare nanofiltration separation layer 3: the above-mentioned obtained stay pipe with nanofiber basic unit to be entered in the aqueous phase solution of 25 DEG C 60 seconds, then stay pipe surface is purged, the aqueous phase solution of removing excess surface, then the organic phase solution 60 seconds of 25 DEG C is immersed, taking-up purges, and removes the organic phase solution of excess surface.Enter the thermal treatment tunnel process 1 minute of 100 DEG C afterwards, link with amido link between described nanofiber basic unit 2 and nanofiltration separation layer 3.
Last it is noted that above-described each embodiment is only for illustration of technical scheme of the present invention, be not intended to limit; Although with reference to previous embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that: it still can be modified to the technical scheme described in previous embodiment, or to wherein partly or entirely technical characteristic carry out equivalent replacement; And these amendments or replacement, do not make the essence of appropriate technical solution depart from the scope of various embodiments of the present invention technical scheme.
Claims (9)
1. a hollow fiber nanofiltration membrane, it is characterized in that: comprise stay pipe, nanofiber basic unit and nanofiltration separation layer, described nanometer dimension basic unit is arranged between described stay pipe and described nanofiltration separation layer, the external diameter of described stay pipe is 0.4 ~ 2.3mm, the wall thickness of described stay pipe is 0.1 ~ 0.7mm, and described stay pipe is inorganic or the stay pipe of organic polymer material braiding.
2. hollow fiber nanofiltration membrane according to claim 1, is characterized in that, the inorganic polymer material of described stay pipe is one or more in silk, copper wire, stainless steel wire, nickel foam, zirconia or alumina metals screen cloth.
3. hollow fiber nanofiltration membrane according to claim 1, it is characterized in that, the organic polymer material of described stay pipe is that PETG, poly, PPTA, polyvinyl chloride, polyurethanes, polyamide, polypropylene are fine, one or more in polypropylene, polyethylene, polyvinyl formal.
4. hollow fiber nanofiltration membrane according to claim 1, it is characterized in that, the material of described nanofiber basic unit is that polyamide, polyurethane, Merlon, polypropylene are fine, polyvinyl alcohol, PLA, polyoxyethylene, polymethyl methacrylate, polyester, polystyrene, polyvinyl chloride, polycaprolactone, cellulose acetate, collagen, polyphenyl miaow is frustrated, one or more in ammonium polyacrylate, polyvinylcarbazole or polyimides.
5. produce a preparation method for hollow fiber nanofiltration membrane, it is characterized in that, comprise the following steps:
S1: the nanofiber basic unit of being prepared by electrostatic spinning process at the outer surface of stay pipe;
S2: stay pipe outer surface being compounded with nanofiber basic unit carries out de-ionised water 20 ~ 40min, carries out drying process 6 ~ 10hrs, is positioned in hothouse for subsequent use after completing above-mentioned operation in the hothouse being placed on 40 ~ 80 DEG C afterwards;
S3: the stay pipe after step S2 process is immersed 60 ~ 480s in the aqueous phase monomers solution of 20 ~ 25 DEG C, top layer liquid is blotted after taking-up, then the organic phase monomer solution 60 ~ 300s of 25 DEG C is immersed, outer surface liquid is blotted after taking-up, then in the environment of 50 ~ 120 DEG C, heat-treat 1 ~ 30min, finally form hollow fiber nanofiltration membrane.
6. the preparation method of production hollow fiber nanofiltration membrane according to claim 5, is characterized in that, prepares nanofiber basic unit specifically comprise the following steps in described step S1 by electrostatic spinning process:
A1: selective polymer, by polymer melting or be dissolved in solvent, uniform stirring obtains melt or the solution of polymer, and the concentration range of described melt or solution is: 5wt% ~ 100wt%;
A2: polymer spinning solution is injected in spinning syringe, adopt syringe needle electrospinning device to prepare layers of nanofibers, the operating voltage of described syringe needle electrospinning device is 10 ~ 100KV, and described syringe is 5 ~ 60cm to the distance of described cylinder collector;
A3: when using syringe needle electrospinning device, syringe needle is fixed and is evenly distributed on the outer ring of cylinder collector.Meanwhile, stay pipe is evenly arranged in the outer ring of cylinder type collector, and also press setting speed with rolling collector synchronous rotary and advance, and stay pipe tube body does not carry out spinning motion, nanofiber is wrapped in the outer surface of stay pipe uniformly.
7. the preparation method of production hollow fiber nanofiltration membrane according to claim 6, it is characterized in that, described solvent is the solvent dissolving close polymer, can be one or more in DMF, normal heptane, carrene, chloroform, cyclohexane, trifluoroacetic acid, toluene, oxolane, acetone, dimethyl sulfoxide (DMSO), water, ethanol, glycerine, ethylene glycol, polyethylene glycol, dimethyl sulfoxide (DMSO), phenol, amide-type, triethanolamine, alcohol salt, urea, formic acid or acetic acid.
8. the method for production hollow fiber nanofiltration membrane according to claim 5, it is characterized in that, described aqueous phase monomers solution is that a kind of in polynary amine is dissolved in the aqueous phase monomers solution formed in the aqueous solution, wherein polynary amine comprises aromatic series and aliphatic two class, described aromatic series comprises m-phenylene diamine (MPD), p-phenylenediamine (PPD), o-phenylenediamine, equal benzene three is pressed, 4-methylresorcinol diamines, m-phenylene diamine (MPD)-5-sulfonic acid, N, N-dimethyl-m-phenylenediamine and poly-m-aminophenyl ethene, described aliphatic comprises piperazine, 1, 4-cyclohexanediamine, polyvinyl alcohol, shitosan, polyvinylamine and polyamines base polyoxyethylene.
9. the preparation method of production hollow fiber nanofiltration membrane according to claim 5, it is characterized in that, described organic phase monomer solution is that a kind of in acyl chlorides and isocyanates is dissolved in the organic phase monomer solution formed in alkane, wherein acyl chlorides and isocyanates include aromatic series and aliphatic two class, described aromatic series comprises paraphthaloyl chloride, m-phthaloyl chloride, o-phthaloyl chloride, pyromellitic trimethylsilyl chloride, methylresorcinol vulcabond, 5-oxygen formyl chloride-isophthaloyl chlorine, 5-isocyanates-isophthaloyl chlorine and methylresorcinol vulcabond, described aliphatic comprises 1, 3, 5-cyclohexane three formyl chloride and 1, 3, 4-pentamethylene three acyl chlorides.
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