CN115253698A - Preparation method of fiber-reinforced hollow fiber nanofiltration membrane - Google Patents
Preparation method of fiber-reinforced hollow fiber nanofiltration membrane Download PDFInfo
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- CN115253698A CN115253698A CN202110477631.2A CN202110477631A CN115253698A CN 115253698 A CN115253698 A CN 115253698A CN 202110477631 A CN202110477631 A CN 202110477631A CN 115253698 A CN115253698 A CN 115253698A
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- 239000012528 membrane Substances 0.000 title claims abstract description 34
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 24
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 22
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000012071 phase Substances 0.000 claims abstract description 22
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- 239000008346 aqueous phase Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000002791 soaking Methods 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000007664 blowing Methods 0.000 claims abstract description 5
- 239000011248 coating agent Substances 0.000 claims abstract description 5
- 238000000576 coating method Methods 0.000 claims abstract description 5
- 238000011033 desalting Methods 0.000 claims abstract description 5
- 239000002346 layers by function Substances 0.000 claims abstract description 5
- 238000004140 cleaning Methods 0.000 claims abstract description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 4
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 18
- 239000002585 base Substances 0.000 claims description 16
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 15
- 238000000034 method Methods 0.000 claims description 14
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 12
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 10
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 10
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 6
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 6
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002250 absorbent Substances 0.000 claims description 5
- 230000002745 absorbent Effects 0.000 claims description 5
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical compound ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 5
- 150000001875 compounds Chemical class 0.000 claims description 5
- 239000000835 fiber Substances 0.000 claims description 5
- 150000008282 halocarbons Chemical class 0.000 claims description 5
- 239000003960 organic solvent Substances 0.000 claims description 5
- 229920000768 polyamine Polymers 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 claims description 4
- RXYPXQSKLGGKOL-UHFFFAOYSA-N 1,4-dimethylpiperazine Chemical compound CN1CCN(C)CC1 RXYPXQSKLGGKOL-UHFFFAOYSA-N 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- IMNFDUFMRHMDMM-UHFFFAOYSA-N N-Heptane Chemical compound CCCCCCC IMNFDUFMRHMDMM-UHFFFAOYSA-N 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 4
- 150000001263 acyl chlorides Chemical class 0.000 claims description 4
- DIKBFYAXUHHXCS-UHFFFAOYSA-N bromoform Chemical compound BrC(Br)Br DIKBFYAXUHHXCS-UHFFFAOYSA-N 0.000 claims description 4
- NAQMVNRVTILPCV-UHFFFAOYSA-N hexane-1,6-diamine Chemical compound NCCCCCCN NAQMVNRVTILPCV-UHFFFAOYSA-N 0.000 claims description 4
- OKJPEAGHQZHRQV-UHFFFAOYSA-N iodoform Chemical compound IC(I)I OKJPEAGHQZHRQV-UHFFFAOYSA-N 0.000 claims description 4
- 229920002492 poly(sulfone) Polymers 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- IMNIMPAHZVJRPE-UHFFFAOYSA-N triethylenediamine Chemical compound C1CN2CCN1CC2 IMNIMPAHZVJRPE-UHFFFAOYSA-N 0.000 claims description 4
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 239000012752 auxiliary agent Substances 0.000 claims description 3
- VKIRRGRTJUUZHS-UHFFFAOYSA-N cyclohexane-1,4-diamine Chemical compound NC1CCC(N)CC1 VKIRRGRTJUUZHS-UHFFFAOYSA-N 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- -1 polyoxyethylene Polymers 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- FQUYSHZXSKYCSY-UHFFFAOYSA-N 1,4-diazepane Chemical compound C1CNCCNC1 FQUYSHZXSKYCSY-UHFFFAOYSA-N 0.000 claims description 2
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 claims description 2
- 229920000877 Melamine resin Polymers 0.000 claims description 2
- 239000002033 PVDF binder Substances 0.000 claims description 2
- 239000004695 Polyether sulfone Substances 0.000 claims description 2
- PWAXUOGZOSVGBO-UHFFFAOYSA-N adipoyl chloride Chemical compound ClC(=O)CCCCC(Cl)=O PWAXUOGZOSVGBO-UHFFFAOYSA-N 0.000 claims description 2
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 2
- 229950005228 bromoform Drugs 0.000 claims description 2
- SSJXIUAHEKJCMH-UHFFFAOYSA-N cyclohexane-1,2-diamine Chemical compound NC1CCCCC1N SSJXIUAHEKJCMH-UHFFFAOYSA-N 0.000 claims description 2
- GEQHKFFSPGPGLN-UHFFFAOYSA-N cyclohexane-1,3-diamine Chemical compound NC1CCCC(N)C1 GEQHKFFSPGPGLN-UHFFFAOYSA-N 0.000 claims description 2
- WMPOZLHMGVKUEJ-UHFFFAOYSA-N decanedioyl dichloride Chemical compound ClC(=O)CCCCCCCCC(Cl)=O WMPOZLHMGVKUEJ-UHFFFAOYSA-N 0.000 claims description 2
- FJBFPHVGVWTDIP-UHFFFAOYSA-N dibromomethane Chemical compound BrCBr FJBFPHVGVWTDIP-UHFFFAOYSA-N 0.000 claims description 2
- NZZFYRREKKOMAT-UHFFFAOYSA-N diiodomethane Chemical compound ICI NZZFYRREKKOMAT-UHFFFAOYSA-N 0.000 claims description 2
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims description 2
- 229920006393 polyether sulfone Polymers 0.000 claims description 2
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 claims description 2
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- NGNBDVOYPDDBFK-UHFFFAOYSA-N 2-[2,4-di(pentan-2-yl)phenoxy]acetyl chloride Chemical compound CCCC(C)C1=CC=C(OCC(Cl)=O)C(C(C)CCC)=C1 NGNBDVOYPDDBFK-UHFFFAOYSA-N 0.000 claims 1
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims 1
- 229920000083 poly(allylamine) Polymers 0.000 claims 1
- 239000000243 solution Substances 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 7
- CSNNHWWHGAXBCP-UHFFFAOYSA-L Magnesium sulfate Chemical compound [Mg+2].[O-][S+2]([O-])([O-])[O-] CSNNHWWHGAXBCP-UHFFFAOYSA-L 0.000 description 4
- 230000004907 flux Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000007888 film coating Substances 0.000 description 2
- 238000009501 film coating Methods 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 2
- 235000019341 magnesium sulphate Nutrition 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000012527 feed solution Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229940018564 m-phenylenediamine Drugs 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- YPHQUSNPXDGUHL-UHFFFAOYSA-N n-methylprop-2-enamide Chemical compound CNC(=O)C=C YPHQUSNPXDGUHL-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920001451 polypropylene glycol Polymers 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 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
-
- 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
- B01D69/08—Hollow fibre membranes
-
- 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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to the field of membrane preparation, and particularly relates to a preparation method of a fiber-reinforced hollow fiber nanofiltration membrane, which comprises the following steps: 1) Coating a base film: soaking the braided tube component with a solvent which is the same as the feed liquid; after the material is completely discharged, the material liquid is pushed out of the braided tube component from top to bottom by using nitrogen; standing, immersing in deionized water for curing, cleaning to obtain a coated base film, and immersing in deionized water again for later use; 2) Preparing a desalting functional layer: soaking the coated base film in an aqueous phase solution for 5-60s from bottom to top, and then draining the aqueous phase; standing for 2min; then the oil phase solution is reacted for 1-20min from bottom to top to push out the soaked coated base film, and the oil phase is emptied; blowing with hot air at 80 deg.C for 10s to obtain product; the breaking strength of the fiber-reinforced hollow fiber nanofiltration membrane obtained by the preparation method of the fiber-reinforced hollow fiber nanofiltration membrane is remarkably improved. Greatly reduces the broken wire rate and obviously improves the pressure resistance.
Description
Technical Field
The invention belongs to the field of membrane preparation, and particularly relates to a preparation method of a fiber-reinforced hollow fiber nanofiltration membrane.
Background
The hollow fiber nanofiltration membrane is usually in a self-supporting structure, namely a base membrane is used for bearing pressure, and a desalination function layer is used for removing salts and small molecules. To achieve a certain pressure resistance, the base membrane needs to have a sufficient thickness, but the thicker the base membrane, the lower the water flux, and the membrane performance cannot be further improved. Meanwhile, in order to ensure the water yield, the tensile strength along the radial direction of the fiber is limited, so that the yarn breakage can be inevitable in the long-term use process.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a preparation method of a fiber-reinforced hollow fiber nanofiltration membrane.
In order to realize the purpose, the invention adopts the technical scheme that:
a preparation method of a fiber-reinforced hollow fiber nanofiltration membrane comprises the following steps:
1) Coating a base film: soaking the braided tube component with a solvent which is the same as the feed liquid; after the material is completely discharged, the material liquid is pushed out of the braided tube assembly from top to bottom by using nitrogen; standing, immersing in deionized water for curing, cleaning to obtain a coated base film, and immersing in deionized water again for later use;
the feed liquid comprises the following components in parts by mass: 18-33 parts of main material, 0-5 parts of forming auxiliary agent and 100 parts of solvent; preferably, the molding auxiliary comprises 25 parts by mass of a main material, 3 parts by mass of a molding auxiliary and 100 parts by mass of a solvent;
2) Preparing a desalting functional layer: soaking the coated base film in an aqueous phase solution from bottom to top for 5-60s, preferably, soaking for 20s, and draining the aqueous phase; standing for 2min; then the oil phase solution is reacted for 1-20min from bottom to top, the soaked coating base membrane is pushed out, and the oil phase is emptied; blowing with hot air at 80 deg.C for 10s to obtain product;
the aqueous phase solution comprises the following components in parts by mass: 0.1-16 parts of polyamine compound, 0.01-5 parts of proton absorbent, 0.01-3 parts of polymerization accelerator and 100 parts of deionized water; the oil phase solution comprises 0.01-4 parts by mass of polyfunctional acyl chloride, 0.01-5 parts by mass of halogenated hydrocarbon and 100 parts by mass of organic solvent.
Preferably, the aqueous phase solution comprises the following components in parts by mass: 2-4 parts of polyamine compound, 0.1-0.5 part of proton absorbent, 0.2 part of polymerization accelerator and 100 parts of deionized water; the oil phase solution contains 0.4 part by mass of polyfunctional acyl chloride, 0.8 part by mass of halogenated hydrocarbon and 100 parts by mass of organic solvent.
The main material is one of polysulfone, polyethersulfone and polyvinylidene fluoride.
The forming auxiliary agent is one of lithium chloride, polyoxyethylene 400, glycol and polyvinylpyrrolidone.
The solvent is one of Dimethylacetamide (DMAC), dimethylformamide (DMF) or N-methylpyrrolidone (NMP).
The polyamine compound is one or a mixture of more of phenylenediamine, piperazine, homopiperazine, ethylenediamine, hexamethylenediamine, melamine, 1, 2-cyclohexanediamine, aminoethyl piperazine, o-phenylenediamine, p-phenylenediamine, 1, 3-cyclohexanediamine, 1, 4-cyclohexanediamine and 4,4' -diphenyldiamine.
The polymerization accelerator is one of polyvinylpyrrolidone, poly (methyl) acrylamide, polyhydroxyethyl methacrylate and polypropylene glycol.
The proton absorbent is one of triethylamine, triethylene diamine, trimethylamine, N, N' -dimethyl piperazine, sodium hydroxide, potassium hydroxide, sodium phosphate and sodium carbonate.
The polyfunctional acyl chloride is one of trimesoyl chloride, adipoyl chloride and sebacoyl chloride.
The organic solvent is one of isoparaffin, normal hexane, cyclohexane and heptane.
The halogenated hydrocarbon is one of chloroform, dichloromethane, bromoform, dibromomethane, iodoform and diiodomethane.
Compared with the prior art, the invention has the beneficial effects that:
the breaking strength of the fiber-reinforced hollow fiber nanofiltration membrane obtained by the preparation method of the fiber-reinforced hollow fiber nanofiltration membrane is remarkably improved. Greatly reduces the broken wire rate and obviously improves the pressure resistance.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the preferred embodiments.
Example 1: the feed liquid formula is as follows: 25 parts by mass of polysulfone, 3 parts by mass of lithium chloride and 100 parts by mass of dimethylacetamide. Stirred at 60 ℃ for 24 hours and then left to stand for 24 hours.
Coating a base film: the braided tube assembly was first soaked with the same solvent as the feed solution for 5min. After purging, the feed liquid is pushed out of the module from top to bottom under a certain pressure using nitrogen. Standing for 60s, soaking in deionized water, curing for 10min, cleaning, and soaking in deionized water again for use.
The water phase formula comprises: comprises 2 parts by mass of piperazine, 0.5 part by mass of triethylamine, 0.2 part by mass of polyvinylpyrrolidone and 100 parts by mass of deionized water.
The oil phase formula comprises: comprises 0.4 part by mass of trimesoyl chloride, 0.5 part by mass of dichloromethane and 100 parts by mass of n-hexane.
Preparing a desalting functional layer: soaking the coated base film obtained in the step 1) for 20 seconds from bottom to top by using an aqueous phase solution, and then draining the aqueous phase. Standing for 2min. And pushing the soaked coated base membrane in an oil phase solution from bottom to top, reacting for 2min, and then emptying the oil phase. Blowing with hot air at 80 deg.C for 10s to obtain the final product.
Example 2: the feed liquid formula is as follows: 25 parts by mass of polysulfone, 400,3 parts by mass of polyoxyethylene and 100 parts by mass of dimethylacetamide. The rest was the same as in example 1.
Example 3: the water phase formula comprises: comprises 2 parts by mass of m-phenylenediamine, 0.5 part by mass of triethylamine, 0.2 part by mass of polyvinylpyrrolidone and 100 parts by mass of deionized water. The rest is the same as in example 1.
Example 4: the water phase formula comprises: comprises 2 parts by mass of 1, 4-cyclohexanediamine, 0.5 part by mass of triethylamine, 0.2 part by mass of polyvinylpyrrolidone and 100 parts by mass of deionized water. The rest is the same as in example 1.
Example 5: the water phase formula comprises: comprises piperazine 2 weight portions, sodium hydroxide 0.1 weight portions, polyvinylpyrrolidone 0.2 weight portions and deionized water 100 weight portions. The rest was the same as in example 1.
Example 6: the water phase formula comprises: comprises 2 parts by mass of piperazine, 0.5 part by mass of sodium phosphate, 0.2 part by mass of polyvinylpyrrolidone and 100 parts by mass of deionized water. The rest is the same as in example 1.
Example 7: the water phase formula comprises: comprises 4 parts by mass of piperazine, 0.5 part by mass of triethylamine, 0.2 part by mass of polyvinylpyrrolidone and 100 parts by mass of deionized water. The rest was the same as in example 1.
Example 8: the oil phase formula comprises: comprises 0.8 mass part of trimesoyl chloride, 0.5 mass part of dichloromethane and 100 mass parts of normal hexane. The rest is the same as in example 1.
Example 9: the oil phase formula comprises: comprises 0.4 parts by mass of trimesoyl chloride, 0.5 parts by mass of dichloromethane and 100 parts by mass of isoparaffin. The rest is the same as in example 1.
Example 10: preparing a desalting functional layer: the aqueous solution was allowed to soak for 20 seconds from the bottom up, and then the aqueous phase was drained. Standing for 2min. Then the oil phase solution is reacted for 2min from bottom to top, and the oil phase is emptied. The rest was the same as in example 1.
Comparative example 1 the base film coating process was not wet out and the rest was the same as in example 1.
Comparative example 2 the base film coating process was not left to stand, and the rest was the same as in example 1.
Comparative example 3 the desalination function layer was prepared without hot air blowing, and the procedure was otherwise the same as in example 1.
Nanofiltration membrane separation performance test method
Testing liquid: the test was carried out using a 2000mg/L magnesium sulfate solution.
The operating parameters are as follows: a nanofiltration membrane evaluator is adopted for testing, the pressure is 0.5MPa, the temperature is 25 ℃, the pH =7.0, and the recovery rate is 15%.
Calculating the formula:
the retention rate R = (CI-CO)/CI x 100%, wherein CI is water inlet conductance, and CO is water outlet conductance;
flux F = V/(a × T), where V is water production volume, a is membrane area, and T is measurement time.
Table 1 shows the results of the runs of the different examples and comparative examples.
TABLE 1
| Magnesium sulfate,% | Water flux, L/(m)2*h) | |
| Example 1 | 97 | 46 |
| Example 2 | 98 | 42 |
| Example 3 | 97 | 45 |
| Example 4 | 97 | 43 |
| Example 5 | 96 | 47 |
| Example 6 | 97 | 41 |
| Example 7 | 95 | 40 |
| Example 8 | 98 | 38 |
| Example 9 | 96 | 39 |
| Example 10 | 97 | 44 |
| Comparative example 1 | 35 | 62 |
| Comparative example 2 | 92 | 8 |
| Comparative example 3 | 88 | 27 |
From the data, it can be seen that the membrane material with good performance can be obtained by adopting the fiber reinforced hollow fiber nanofiltration membrane.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and amendments can be made without departing from the principle of the present invention, and these modifications and amendments should also be considered as the protection scope of the present invention.
Claims (10)
1. A preparation method of a fiber-reinforced hollow fiber nanofiltration membrane is characterized by comprising the following steps:
1) Coating a base film: soaking the braided tube component with a solvent which is the same as the feed liquid; after the material is completely discharged, the material liquid is pushed out of the braided tube assembly from top to bottom by using nitrogen; standing, immersing in deionized water for curing, cleaning to obtain a coated base film, and immersing in deionized water again for later use;
the feed liquid comprises the following components in parts by mass: 18-33 parts of main material, 0-5 parts of forming auxiliary agent and 100 parts of solvent;
2) Preparing a desalting functional layer: soaking the coated base film in an aqueous phase solution for 5-60s from bottom to top, and then draining the aqueous phase; standing for 2min, reacting the oil phase solution from bottom to top for 1-20min, pushing out the soaked coated base film, and draining the oil phase; blowing with hot air at 80 deg.C for 10s to obtain product;
the aqueous phase solution comprises the following components in parts by mass: 0.1-16 parts of polyamine compound, 0.01-5 parts of proton absorbent, 0.01-3 parts of polymerization accelerator and 100 parts of deionized water; the oil phase solution comprises 0.01-4 parts by mass of polyfunctional acyl chloride, 0.01-5 parts by mass of halogenated hydrocarbon and 100 parts by mass of organic solvent.
2. The method for preparing the fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the main material is one of polysulfone, polyethersulfone and polyvinylidene fluoride.
3. The method for preparing the fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the molding aid is one of lithium chloride, polyoxyethylene 400, ethylene glycol and polyvinylpyrrolidone.
4. The method for preparing the fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the solvent is one of Dimethylacetamide (DMAC), dimethylformamide (DMF) or N-methylpyrrolidone (NMP).
5. The method for preparing a fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the polyamine compound is one or more of phenylenediamine, piperazine, homopiperazine, ethylenediamine, hexamethylenediamine, melamine, 1, 2-cyclohexanediamine, aminoethylpiperazine, o-phenylenediamine, p-phenylenediamine, 1, 3-cyclohexanediamine, 1, 4-cyclohexanediamine, and 4,4' -diphenyldiamine.
6. The method for preparing the fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the polymerization accelerator is one of polyvinylpyrrolidone, poly (meth) acrylamide, polyhydroxyethyl methacrylate, and polyallylamine.
7. The method for preparing a fiber-enhanced hollow fiber nanofiltration membrane according to claim 1, wherein the proton absorbent is one of triethylamine, triethylene diamine, trimethylamine, N, N' -dimethylpiperazine, sodium hydroxide, potassium hydroxide, sodium phosphate and sodium carbonate.
8. The method for preparing a fiber-enhanced hollow fiber nanofiltration membrane according to claim 1, wherein the polyfunctional acid chloride is one of trimesoyl chloride, adipoyl chloride and sebacoyl chloride.
9. The method for preparing the fiber-enhanced hollow fiber nanofiltration membrane according to claim 1, wherein the organic solvent is one of isoparaffin, n-hexane, cyclohexane and heptane.
10. The method for preparing the fiber-reinforced hollow fiber nanofiltration membrane according to claim 1, wherein the halogenated hydrocarbon is one of chloroform, dichloromethane, bromoform, dibromomethane, iodoform and diiodomethane.
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