CN108452691A - Interface polymerization reaction device, hollow fiber compound nanofiltration membrane preparation facilities and method - Google Patents
Interface polymerization reaction device, hollow fiber compound nanofiltration membrane preparation facilities and method Download PDFInfo
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- CN108452691A CN108452691A CN201810172608.0A CN201810172608A CN108452691A CN 108452691 A CN108452691 A CN 108452691A CN 201810172608 A CN201810172608 A CN 201810172608A CN 108452691 A CN108452691 A CN 108452691A
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- groove body
- hollow fiber
- polymerization reaction
- membrane
- interface polymerization
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- 239000012528 membrane Substances 0.000 title claims abstract description 114
- 239000012510 hollow fiber Substances 0.000 title claims abstract description 82
- 238000006116 polymerization reaction Methods 0.000 title claims abstract description 46
- 150000001875 compounds Chemical class 0.000 title claims abstract description 38
- 238000001728 nano-filtration Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title abstract description 13
- 239000000178 monomer Substances 0.000 claims abstract description 91
- 239000008346 aqueous phase Substances 0.000 claims abstract description 53
- 239000012071 phase Substances 0.000 claims abstract description 46
- 239000002131 composite material Substances 0.000 claims abstract description 31
- 238000011068 loading method Methods 0.000 claims abstract description 9
- 230000008676 import Effects 0.000 claims abstract description 5
- 238000000108 ultra-filtration Methods 0.000 claims description 48
- 239000011248 coating agent Substances 0.000 claims description 32
- 238000000576 coating method Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 22
- -1 polyethylene Polymers 0.000 claims description 15
- 229920001223 polyethylene glycol Polymers 0.000 claims description 13
- 239000002202 Polyethylene glycol Substances 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000012544 monitoring process Methods 0.000 claims description 11
- 235000012489 doughnuts Nutrition 0.000 claims description 10
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 9
- 238000000137 annealing Methods 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 8
- GLUUGHFHXGJENI-UHFFFAOYSA-N Piperazine Chemical compound C1CNCCN1 GLUUGHFHXGJENI-UHFFFAOYSA-N 0.000 claims description 6
- 239000000835 fiber Substances 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 238000012695 Interfacial polymerization Methods 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- RUOKPLVTMFHRJE-UHFFFAOYSA-N benzene-1,2,3-triamine Chemical compound NC1=CC=CC(N)=C1N RUOKPLVTMFHRJE-UHFFFAOYSA-N 0.000 claims description 4
- UWCPYKQBIPYOLX-UHFFFAOYSA-N benzene-1,3,5-tricarbonyl chloride Chemical group ClC(=O)C1=CC(C(Cl)=O)=CC(C(Cl)=O)=C1 UWCPYKQBIPYOLX-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 229920006393 polyether sulfone Polymers 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 4
- OPPFIPBEHRZBOT-UHFFFAOYSA-N 1,1-bis(oxiran-2-ylmethoxy)propan-1-ol Chemical compound C1OC1COC(O)(CC)OCC1CO1 OPPFIPBEHRZBOT-UHFFFAOYSA-N 0.000 claims description 3
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 claims description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 239000004695 Polyether sulfone Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 150000001412 amines Chemical group 0.000 claims description 3
- FDQSRULYDNDXQB-UHFFFAOYSA-N benzene-1,3-dicarbonyl chloride Chemical compound ClC(=O)C1=CC=CC(C(Cl)=O)=C1 FDQSRULYDNDXQB-UHFFFAOYSA-N 0.000 claims description 3
- UKJLNMAFNRKWGR-UHFFFAOYSA-N cyclohexatrienamine Chemical group NC1=CC=C=C[CH]1 UKJLNMAFNRKWGR-UHFFFAOYSA-N 0.000 claims description 3
- 125000005442 diisocyanate group Chemical group 0.000 claims description 3
- 229920002492 poly(sulfone) Polymers 0.000 claims description 3
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 3
- 229920000728 polyester Polymers 0.000 claims description 3
- 229920001721 polyimide Polymers 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 2
- 239000004800 polyvinyl chloride Substances 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims 2
- HSRJKNPTNIJEKV-UHFFFAOYSA-N Guaifenesin Chemical compound COC1=CC=CC=C1OCC(O)CO HSRJKNPTNIJEKV-UHFFFAOYSA-N 0.000 claims 1
- CHBCHAGCVIMDKI-UHFFFAOYSA-N [F].C=C Chemical group [F].C=C CHBCHAGCVIMDKI-UHFFFAOYSA-N 0.000 claims 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims 1
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000010410 layer Substances 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 6
- 238000010924 continuous production Methods 0.000 description 6
- 239000006260 foam Substances 0.000 description 6
- 238000004804 winding Methods 0.000 description 6
- 230000004907 flux Effects 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 238000005491 wire drawing Methods 0.000 description 4
- 238000007605 air drying Methods 0.000 description 3
- 230000001276 controlling effect Effects 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000001112 coagulating effect Effects 0.000 description 2
- 238000000280 densification Methods 0.000 description 2
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 239000004088 foaming agent Substances 0.000 description 2
- 230000008595 infiltration Effects 0.000 description 2
- 238000001764 infiltration Methods 0.000 description 2
- 238000010406 interfacial reaction Methods 0.000 description 2
- WFKAJVHLWXSISD-UHFFFAOYSA-N isobutyramide Chemical class CC(C)C(N)=O WFKAJVHLWXSISD-UHFFFAOYSA-N 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L magnesium chloride Substances [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- 229910001629 magnesium chloride Inorganic materials 0.000 description 2
- 238000012797 qualification Methods 0.000 description 2
- 230000003014 reinforcing effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 239000004593 Epoxy Substances 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- PCIBVZXUNDZWRL-UHFFFAOYSA-N ethylene glycol monophosphate Chemical compound OCCOP(O)(O)=O PCIBVZXUNDZWRL-UHFFFAOYSA-N 0.000 description 1
- 238000007654 immersion Methods 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920001568 phenolic resin Polymers 0.000 description 1
- 239000005011 phenolic resin Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920006316 polyvinylpyrrolidine Polymers 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000002145 thermally induced phase separation Methods 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
- B01D69/1251—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction by interfacial polymerisation
-
- 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
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
-
- 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
- B01D71/26—Polyalkenes
-
- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—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
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/36—Polytetrafluoroethene
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/48—Polyesters
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/42—Details of membrane preparation apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
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- B01D67/0002—Organic membrane manufacture
- B01D67/0006—Organic membrane manufacture by chemical reactions
Abstract
A kind of interface polymerization reaction device, hollow fiber compound nanofiltration membrane preparation facilities and method, the device include applicator assembly, guidance set and dry component.Applicator assembly includes the first groove body for loading aqueous phase monomers and the second groove body for loading oil phase monomer, and the first groove body includes ontology, is connected to ontology and first and second opening up interconnecting part.Guidance set includes first and second guide part, first guide part is used for processed product out of, the first interconnecting part imports first groove body ontology, second guide part is used to from the second interconnecting part import processed product in the second groove body, so that with oil phase monomer in product surface interface polymerization reaction, which occurs, for the aqueous phase monomers coated on product forms composite membrane.Dry component is set between the second interconnecting part and the second groove body.The device and method can make the products such as hollow fiber compound nanofiltration membrane that can industrially realize extensive continuous high-efficient production.
Description
Technical field,
It is compound more particularly to a kind of interface polymerization reaction device, doughnut the present invention relates to separation technical field of membrane
Nanofiltration membrane preparation device and method.
Background technology
Membrane separation technique selects mixing liquid by membrane aperture size and surface compatibility using pressure as driving force
Property separation.Wherein, the composite nanometer filtering film that prepared by interfacial polymerization has larger permeation flux and salt rejection rate.Current is ground
From the point of view of studying carefully report and practical application, interfacial polymerization all has very important in NF membrane basic research and commercialization field
Position.It, can be by individually controlling the structure and property of supporting layer or fine and close composite layer this is because interfacial polymerization prepares NF membrane
It can be regulated and controled, prepare the composite nanometer filter of the different selectivity and different permeability of excellent, the resistance to densification of required mechanical strength
Film.
Composite nanometer filtering film product has plate film assembly and hollow fiber film assembly etc..But it is most of on the market compound to receive
Filter membrane is plate film assembly, and rarely has hollow fiber film assembly.This is primarily due to the hollow fibre used in hollow fiber film assembly
Dimension composite nanometer filtering film is usually used interface polymerization reaction and is made, and is prior to impregnating coating in aqueous phase monomers, taking out, then at oil
Coating is impregnated in phase monomer to be made, thus it is caused to be difficult industrially large-scale continuous production.Secondly, doughnut is compound to be received
Soaking time of the filter membrane in interface polymerization reaction needed for aqueous phase monomers coating is long, causes production efficiency relatively low.However hollow fibre
Tieing up membrane module has using more flexible, film wire loading density is high, treating nature water is simple, operation expense is low and application range
The advantages that more extensive, therefore be badly in need of providing a kind of interface polymerization reaction dress that can industrially realize large-scale continuous production
It sets, hollow fiber compound nanofiltration membrane preparation facilities and method.
Invention content
Based on this, it is necessary to provide a kind of interface polymerization reaction that can industrially realize extensive continuous high-efficient production
Device, hollow fiber compound nanofiltration membrane preparation facilities and method.
A kind of interface polymerization reaction device, including：
Applicator assembly, includes the first groove body for loading aqueous phase monomers and the second groove body for loading oil phase monomer,
First groove body includes ontology, the first interconnecting part and the second interconnecting part, first interconnecting part and second connected component
It is not connected to ontology and opening up setting；
Guidance set, including the first guide part and the second guide part, first guide part be used for by processed product from
First interconnecting part imports in the ontology of first groove body, and second guide part is used for the ontology of first groove body
The interior processed product coated with aqueous phase monomers is imported from second interconnecting part in second groove body, so as to be coated on product
Aqueous phase monomers and oil phase monomer interface polymerization reaction occur in product surface form composite membrane；And
Dry component is set between second interconnecting part and second groove body, and aqueous phase monomers are coated with for dry
Processed product.
Interfacial polymerization occurs for the surface that the interface polymerization reaction device can be applied to the products such as Hollow Fiber Ultrafiltration support membrane
Reaction forms composite membrane, and then hollow fiber compound nanofiltration membrane is made.So not only make the needs such as hollow fiber compound nanofiltration membrane
The product produced using interface polymerization reaction can industrially realize large-scale continuous production, and improve production efficiency, in addition
Also improve the stability of the products such as hollow fiber compound nanofiltration membrane.
Further include for heating first heating component of the first groove body and/or for adding in one of the embodiments,
Heat second heating component of the second groove body.
The applicator assembly further includes adjusting control for the first groove body inner aqueous phase monomer temperature in one of the embodiments,
First temperature control part of system and/or the second temperature control part for oil phase monomer temperature adjusting control in the second groove body.
The applicator assembly further includes being waited for for monitoring the intrinsic of the first groove body in one of the embodiments,
The first pressure of the hydraulic pressure of liquid level residing for converted products monitors part and/or for monitoring the processed product in second groove body
The second pressure of the hydraulic pressure of residing liquid level monitors part.
First groove body is U-shaped structure in one of the embodiments,.
First groove body is formed by the pipeline of multistage both ends open by flanged joint in one of the embodiments,.
The dry component includes power source and air-dries pipe in one of the embodiments, and the power source is used for institute
It states air-dried pipe and compressed gas is provided, the air-dried pipe is set between second interconnecting part and second groove body, described to air-dry
The tube wall of pipe is hollow structure, and the tube wall has the ventilation inner cavity for being connected to the power source, and the tube wall is interior
Surface be equipped with exhaust vent, in the pore to the air-dried pipe by processed product air-dry.
A kind of preparation facilities of hollow fiber compound nanofiltration membrane, including annealing device and above-mentioned interface polymerization reaction dress
It sets, the interface polymerization reaction device is used to carry out interface polymerization reaction on the surface of Hollow Fiber Ultrafiltration support membrane multiple to be formed
UF membrane layer is closed, the Hollow Fiber Ultrafiltration support membrane that the annealing device is used to be formed with composite membrane separating layer carries out hot place
Reason, the hollow fiber compound nanofiltration membrane is made.
A kind of preparation method of hollow fiber compound nanofiltration membrane is filled using the preparation of above-mentioned hollow fiber compound nanofiltration membrane
It sets, the preparation method comprises the following steps：
Hollow Fiber Ultrafiltration support membrane is sequentially passed through described by first guide part and second guide part
One interconnecting part, the ontology, second interconnecting part, the dry component and second groove body, the Hollow Fiber Ultrafiltration
Support membrane coats aqueous phase monomers in first groove body, is dried through the dry component, then at the second groove body coating oil
Phase monomer, and make the aqueous phase monomers that interface occur on the surface of the Hollow Fiber Ultrafiltration support membrane with the oil phase monomer and gather
It closes reaction and forms composite membrane separating layer；It is heat-treated then at the annealing device, obtains the doughnut composite nanometer filter
Film.
In one of the embodiments, the material of the Hollow Fiber Ultrafiltration support membrane be polysulfones, polyether sulfone, polyethylene,
Polypropylene, polyvinyl chloride, polyimides, polyacrylonitrile, Kynoar, polytetrafluoroethylene (PTFE) or polyester；
The aqueous phase monomers are piperazine, triaminobenzene, p-aminophenyl, m-aminophenyl, polyethylene glycol sulfuric ester, polyethylene glycol
The aqueous solution of at least one of phosphate, quaternary amine polyethylene glycol and polyethylene glycol polyampholyte；The aqueous solution
Mass fraction is 0.5%~5%；
The oil phase monomer be trimesoyl chloride, terephthalyl chloride, isophthaloyl chloride, diisocyanate, epoxychloropropane,
The mixed liquor of at least one of diglycidyl ether and propanetriol-diglycidyl-ether and organic solvent；The organic solvent is just
At least one of hexane and toluene；
The liquid level of first groove body is 0.5~5m, and the coating time of the aqueous phase monomers is 0.5~5 minute, the oil
The coating time of phase monomer is 10~60 seconds.
Description of the drawings
Fig. 1 is the structure chart of the interface polymerization reaction device of an embodiment.
Specific implementation mode
To facilitate the understanding of the present invention, below will to invention is more fully described, and give the present invention compared with
Good embodiment.But the present invention can realize in many different forms, however it is not limited to embodiment described herein.Phase
Instead, purpose of providing these embodiments is makes the disclosure of the present invention more thorough and comprehensive.
Unless otherwise defined, all of technologies and scientific terms used here by the article and belong to the technical field of the present invention
The normally understood meaning of technical staff is identical.Used term is intended merely to description tool in the description of the invention herein
The purpose of the embodiment of body, it is not intended that in the limitation present invention.Term as used herein "and/or" includes one or more phases
Any and all combinations of the Listed Items of pass.
Referring to Fig.1, the interface polymerization reaction device 10 of an embodiment includes applicator assembly, guidance set and dry component
14。
Applicator assembly includes the first groove body 11 for loading aqueous phase monomers and the second groove body for loading oil phase monomer
12.First groove body 11 includes ontology 111, the first interconnecting part 112 and the second interconnecting part 113, the connection of the first interconnecting part 112 and second
Portion 113 is connected to respectively with ontology 111 and opening up setting.
Guidance set includes the first guide part 131 and the second guide part 132.First guide part 131 is used for production to be processed
Product are out of, the first interconnecting part 112 imports the first groove body 11 ontology 111.Second guide part 132 is used for the sheet of the first groove body 11
The processed product coated with aqueous phase monomers is imported from the second interconnecting part 113 in the second groove body 12 in body 111, so as to be applied on product
The aqueous phase monomers covered occur interface polymerization reaction in product surface with oil phase monomer and form composite membrane.
Dry component 14 is set between the second interconnecting part 113 and the second groove body 12, for drying coated with aqueous phase monomers
Processed product, removes the moisture of its excess surface, and control enters the degree of drying of film wire waiting converted products before oil phase monomer.
When above-mentioned interface polymerization reaction device 10 works, water phase list is loaded respectively in the first groove body 11 and the second groove body 12
Body and oil phase monomer, and other processed products such as Hollow Fiber Ultrafiltration support membrane are led set on the first guide part 131 and second
To on part 132, and sequentially pass through the first interconnecting part 112, ontology 111, the second interconnecting part 113, dry component 14 and the second groove body
12, it is formed so that with oil phase monomer on the surface of the products such as Hollow Fiber Ultrafiltration support membrane interface polymerization reaction occurs for aqueous phase monomers
Composite membrane.The aqueous phase monomers and oil phase monomer activity of interface polymerization reaction are very high, once contact forms net in product surface quickly
The ultra-thin dense skin of shape, i.e. composite membrane.Finally by being thermally treated resulting in hollow fiber compound nanofiltration membrane.
Above-mentioned interface polymerization reaction device 10 is coated aqueous phase monomers coating and oil phase monomer continuously using guidance set
Change, the moisture of the processed product excess surface coated with aqueous phase monomers is removed using dry component 14, overcomes doughnut
The problem of product of the cortinas shape such as ultrafiltration support membrane equally brushes away extra liquid without image of Buddha flat support layer by brush, avoids
Surplus liquid and coating are uneven to cause composite membrane to form " pin hole " defect, and then influences the infiltration of hollow fiber compound nanofiltration membrane
The problem of cutoff performance.And by the unique design of the first groove body 11, it can control the first interconnecting part 112 and the second interconnecting part 113
Liquid level, the liquid level residing for the products such as Hollow Fiber Ultrafiltration support membrane in ontology 111 to control the first groove body 11, Jin Ertong
Cross higher liquid level and increase Hollow Fiber Ultrafiltration support membrane pressure suffered in water phase coating procedure, with accelerate aqueous phase monomers with
The infiltration rate of adsorption of the products such as Hollow Fiber Ultrafiltration support membrane, and then shorten the soaking time needed for water phase coating, to contract
Soaking time needed for short aqueous phase monomers coating, and then reduce the immersion needed for aqueous phase monomers coating and oil phase monomer coating
Time difference further reduces the production time on the basis of continuous production, improves production efficiency.
Therefore the application of the interface polymerization reaction device 10 not only makes hollow fiber compound nanofiltration membrane etc. need to use interface
The product of polymerisation production can industrially realize large-scale continuous production, and improve production efficiency, also improve in addition
The stability of the products such as hollow fiber compound nanofiltration membrane.
Specifically, traditional preparation methods, the coating times of aqueous phase monomers be at least want 5 the time acted on aqueous phase monomers~
20 minutes, and the coating time of aqueous phase monomers can be foreshortened to 0.5~5 minute using above-mentioned interfacial reaction device.
It is understood that can be used for one or more Hollow Fiber Ultrafiltration support membrane etc. to be added for above-mentioned interface polymerization reaction device 10
Chemical product is carried out at the same time interface polymerization reaction, it may also be used for film surface chemical modification.Specifically, in order to avoid more doughnuts
Ultrafiltration support membrane influences each other, and can be suitably modified to guidance set, and groove or baffle is arranged.It is prepared by interface polymerization reaction
Method have the advantages that the structure in dense layer thickness and aperture is regulatable, to which the separation film water for breaking through conventional process preparation is logical
Amount and the shifting restriction of rejection, the composite membrane of preparation go out permeation flux and rejection while improving.
Further, which further includes the first heating component (not shown).First heating component
For heating the first groove body 11.Further, which further includes the second heating component (not shown).The
Two heating components are for heating the second groove body 12.The first heating component of temperature setting needed for can so being coated according to aqueous phase monomers
Heating temperature.The heating temperature of the second heating component of temperature setting needed for being coated according to oil phase monomer.
Further, applicator assembly further includes the first temperature control part 114.First temperature control part 114 is used for the first slot of adjusting control
The temperature of 11 inner aqueous phase monomer of body.Further, applicator assembly further includes the second temperature control part (not shown).Second temperature control part is used for
The temperature of oil phase monomer in the second groove body of adjusting control 12.
Further, applicator assembly further includes first pressure monitoring part 115.First pressure monitors part 115 for monitoring the
The hydraulic pressure of liquid level residing for processed product in the ontology 111 of one groove body 11.Further, applicator assembly further includes second pressure
Monitor part (not shown).Second pressure monitoring part is used to monitor the hydraulic pressure of liquid level residing for the processed product in the second groove body 12.
It is pressure gauge that first pressure, which monitors part and second pressure monitoring part,.
Specifically, the first groove body 11 is U-shaped structure.First groove body 11 of U-shaped structure can reduce the usage amount of aqueous phase monomers.
That is U-shaped structure is collectively formed in the ontology 111 of the first groove body 11, the first interconnecting part 112 and the second interconnecting part 113.Specifically
Ground, the first groove body 11 are formed by the pipeline of multistage both ends open by flanged joint.The setting of such first groove body 11 is very clever
Living, the height of the first interconnecting part 112 and the second interconnecting part 113 also can be flexibly arranged as needed.Specifically, pipeline is steel pipe.
Specifically, the bottom of the ontology 111 of the first groove body 11 is equipped with the first leakage fluid dram (not shown).The bottom of second groove body 12
Portion is equipped with the second leakage fluid dram (not shown).
Further, dry component 14 includes power source (not shown) and air-dried pipe (figure is not marked).Power source is used for wind
Main pipe provides compressed gas, air-dries pipe and is set between the second interconnecting part 113 and the second groove body 12.
Specifically, power source is air compressor.Specifically, the tube wall for air-drying pipe is hollow structure, have for it is dynamic
The ventilation inner cavity of power source connection.Tube wall is connected to power source, and the inner surface of tube wall is equipped with exhaust vent, with to air-drying inside pipe
Product is uniformly air-dried, and it is controllable to air-dry degree.More specifically, the quantity of exhaust vent can be multiple.Specifically, ventilation inner cavity
So that compressed air tiny air draught formed therein that, so that compressed gas is uniform from exhaust vent by small air runner
Outflow, is uniformly air-dried towards processed products.More specifically, exhaust vent is evenly distributed on the inner surface of air-dried pipe, with right
Processed product carries out 360 degree and air-dries.
Specifically, dry component 14 further includes heating temperature-controlled member, and heating temperature-controlled member can carry out the gas flowed through
Accurate heated for controlling temperature.
Specifically, dry component 14 further includes third pressure monitoring regulating part (not shown), is set to and air-dries pipe and power source
For adjusting and detect wind velocity on the pipeline of connection.Third pressure monitoring regulating part is pressure gauge.
More specifically, the interface polymerization reaction device 10 further includes first support 15 and second support 16.First support 15
It is separately connected with the first interconnecting part 112, ontology 111, the second interconnecting part 113 of the first groove body 11 to ensure its stability.Second
Holder 16 is connect with the second groove body 12, for supporting the second groove body 12.
Specifically, the first guide part 131 is connected to the opening in first support 15 and positioned at the first interconnecting part 112.Tool
Body, air-dried pipe is connected in first support 15 and the opening of the second interconnecting part of face 113 is arranged.Specifically, the second guide part
132 are connected to first support 15 and positioned at the opening for air-drying separate first interconnecting part 112 of pipe.
Specifically, first support 15 is rectangular frame structure, and the first groove body 11 is located in first support 15 and the first connection
Portion 112, ontology 111, the second interconnecting part 113 are connect with first support 15 respectively.Specifically, second support 16 is set to first support
15 side.More specifically, first support 15 and second support 16 are located in a plane.
Specifically, it is additionally provided with reinforcing rib in first support 15.Reinforcing rib is horizontally disposed to lead with the first guide part 131 and second
It is arranged in parallel to 132 junction of part.
More specifically, first support 15 and second support 16 are connected with each other, to enhance the monolithic stability of interfacial reaction device
Property.
Specifically, guidance set further includes third guide part 133, and third guide part 133 is set in first support 15, and is used
A breeze way is provided before entering the second groove body 12 in the processed product come out to air-dried pipe.Specifically, third is oriented to
The quantity of part 133 is multiple, and multiple intervals of third guide part 133 are set in first support 15, and two neighboring third guide part
The 133 distance setting apart from first support 15 differs, to further increase breeze way.
Specifically, each guide part is directive wheel.The surface of each guide part be equipped with sponge foam, with reduce product surface by
To the abrasion of guide part.Specifically, sponge foam is high molecular polymer software sponge foam.More specifically, sponge foam by
Polyurethane, at least one of polyethylene, phenolic resin, polyethers, polyvinyl alcohol and natural emulsion material are made.
Further, which further includes unreeling component.It unreels component and is set to the first interconnecting part 112
Opening, and for product to be coated to be unwound.Specifically, unreeling component has unreeling wheel, the surface of unreeling wheel
Also above-mentioned sponge foam can be equipped with.It is understood that in one embodiment, 131 alternative unreeling wheel of the first guide part, while playing and moving back
Around the effect with guiding.
Further, which further includes winding component 17.It winds component 17 and is set to the second groove body
12 side, and for winding the product after progress interface polymerization reaction.Specifically, winding component 17 has winding
Wheel, the surface of winding wheel can also be equipped with above-mentioned sponge foam.Winding wheel is connected in second support 16.
The present invention also provides the preparation facilities of the hollow fiber compound nanofiltration membrane of an embodiment.It includes heat treatment dress
It sets and above-mentioned interface polymerization reaction device 10.
Interface polymerization reaction device 10 is used to carry out interface polymerization reaction on the surface of Hollow Fiber Ultrafiltration support membrane with shape
At composite membrane separating layer.
Annealing device is for the hollow-fibre membrane for being formed with composite membrane separating layer to be heat-treated, so that composite membrane point
The further cross-linked polymeric of absciss layer makes the micropore on surface layer further shrink densification, obtains hollow fiber compound nanofiltration membrane.
Specifically, annealing device is that heat-treating apparatus may be implemented in baking oven etc..
The preparation facilities of above-mentioned hollow fiber compound nanofiltration membrane can be used for large-scale continuous production doughnut composite nanometer filter
Film, and there is higher production efficiency and properties of product stability.
Hollow fiber compound nanofiltration membrane obtained is using Hollow Fiber Ultrafiltration support membrane as middle support layer, composite membrane separating layer
It is closely uniformly combined on the outer surface of Hollow Fiber Ultrafiltration support membrane for fine and close compound-split layer.
The present invention also provides the preparation methods of the hollow fiber compound nanofiltration membrane of an embodiment, use above-mentioned hollow fibre
Tie up the preparation facilities of composite nanometer filtering film.The preparation method includes the following steps：
By Hollow Fiber Ultrafiltration support membrane by sequentially passing through the first interconnecting part, sheet on the first guide part and the second guide part
Body, the second interconnecting part, dry component and the second groove body.Hollow Fiber Ultrafiltration support membrane coats aqueous phase monomers in the first groove body,
It is dried through dry component, oil phase monomer is coated then at the second groove body, and make aqueous phase monomers with oil phase monomer in Hollow Fiber Ultrafiltration
The surface of support membrane occurs interface polymerization reaction and forms composite membrane；It is heat-treated then at annealing device, obtains doughnut
Composite nanometer filtering film.
The preparation method of above-mentioned hollow fiber compound nanofiltration membrane is simple, at low cost, can realize that serialization efficiently produces, and
The stability of hollow fiber compound nanofiltration membrane obtained is high.
Further, the material of Hollow Fiber Ultrafiltration support membrane is polysulfones, polyether sulfone, polyethylene, polypropylene, polychlorostyrene second
Alkene, polyimides, polyacrylonitrile, Kynoar, polytetrafluoroethylene (PTFE) or polyester.
Specifically, hollow fiber ultrafiltration membrane supporting layer can directly be bought or by thermally induced phase separation, phase separation
Method, hot-drawing method are prepared.
Further, aqueous phase monomers are piperazine, triaminobenzene, p-aminophenyl, m-aminophenyl, polyethylene glycol sulfuric ester, gather
The aqueous solution of at least one of ethylene glycol phosphate, quaternary amine polyethylene glycol and polyethylene glycol polyampholyte；Aqueous solution
Mass fraction be 0.5%~5%.
Further, oil phase monomer is trimesoyl chloride, terephthalyl chloride, isophthaloyl chloride, diisocyanate, epoxy chlorine
The mixed liquor of at least one of propane, diglycidyl ether and propanetriol-diglycidyl-ether and organic solvent, organic solvent are
At least one of n-hexane and toluene.
In the present embodiment, the coating time of oil phase monomer, that is, the Hollow Fiber Ultrafiltration branch coated with aqueous phase monomers
It is 10~60 seconds that film, which is supportted, by the time of the second groove body.Therefore it is produced to further realize continuous high-efficient, the painting of aqueous phase monomers
It is close as much as possible to cover the time.The liquid level of the first groove body is 0.5~5m, i.e. the first slot in one of the embodiments,
Liquid level residing for the intrinsic Hollow Fiber Ultrafiltration support membrane of body is 0.5~5m.By controlling Hollow Fiber Ultrafiltration support membrane
Distance and guidance set through aqueous phase monomers transmission speed, can control Hollow Fiber Ultrafiltration support membrane by the first groove body
Aqueous phase monomers time be 0.5~5 minute, i.e., the coating time of aqueous phase monomers be 0.5~5 minute.Preferably, tune can be passed through
The transmission speed of section liquid level and guidance set keeps the coating time of aqueous phase monomers suitable with the coating time of oil phase monomer.
Specifically, the condition of heat treatment is to be heat-treated 10~50 minutes at 70~100 DEG C.
It is specific embodiment below.Following embodiment is all made of interface polymerization reaction device 10 shown in FIG. 1 and is made.
Embodiment 1
Prepare Hollow Fiber Ultrafiltration support membrane.The material based on the Kynoar of 17wt%, with the poly- second of 12wt% two
Alcohol 200,8wt% PEG 20000s be pore-foaming agent, 63wt% dimethylacetylamides be solvent, water be core liquid and outer coagulating bath,
Hollow Fiber Ultrafiltration support membrane is spinned on hollow fiber spinning machine.
After the Hollow Fiber Ultrafiltration support membrane wash clean spinned dries, removed together with wire drawing wheel anti-mounted on interface
On the unreeling wheel for unreeling component for answering device.By a pull-out of Hollow Fiber Ultrafiltration support membrane.Ensure that film wire is run in equipment
After smooth, the triaminobenzene aqueous solution of the mass fraction 2wt% as aqueous phase monomers is added to the first groove body, until in ontology
Hollow Fiber Ultrafiltration support membrane residing for liquid level at 3.5 meters.Using the trimesoyl chloride hexane solution of 0.1wt% as oil phase list
Body is added to the second groove body.Starting device adjusts wire feed rolls rate and wire drawing wheel rate, opens blowing-dry apparatus, passes through guiding
Component sequentially passes through the first interconnecting part, ontology, the second interconnecting part, dry component and the second groove body, starts in Hollow Fiber Ultrafiltration
The outer surface of support membrane is continuously applied coated with formation composite membrane separating layer.The coating time of oil phase monomer is 60 seconds, aqueous phase monomers
Coating time is 1 minute.
It waits for that the coating of entire volume film wire finishes, removes entire volume film wire and carry out heat treatment 30 minutes in 85 DEG C, you can obtain that there is cause
The hollow fiber compound nanofiltration membrane of close compound-split layer.
Embodiment 2
Prepare Hollow Fiber Ultrafiltration support membrane.The material based on 19wt% polyether sulfones, with 10wt% polyvinylpyrrolidines
Ketone, 8wt% normal propyl alcohols are pore-foaming agent, and 63wt% dimethylacetylamides are solvent, and water is core liquid and outer coagulating bath, in doughnut
Hollow Fiber Ultrafiltration support membrane is spinned on spinning-drawing machine.
After the Hollow Fiber Ultrafiltration support membrane wash clean spinned dries, removed together with wire drawing wheel anti-mounted on interface
On the unreeling wheel for unreeling component for answering device.By a pull-out of Hollow Fiber Ultrafiltration support membrane.Ensure that film wire is run in equipment
After smooth, the quaternary ammoniated Aqueous Solutions of Polyethylene Glycol of the mass fraction 1.5wt% as aqueous phase monomers is added to the first groove body, directly
To liquid level residing for intrinsic Hollow Fiber Ultrafiltration support membrane at 2 meters.Using the epoxychloropropane hexane solution of 0.1wt% as
Oil phase monomer is added to the second groove body.Starting device adjusts wire feed rolls rate and wire drawing wheel rate, opens blowing-dry apparatus, leads to
It crosses guidance set and sequentially passes through the first interconnecting part, ontology, the second interconnecting part, dry component and the second groove body, start in hollow fibre
The outer surface for tieing up ultrafiltration support membrane is continuously applied coated with formation composite membrane separating layer.The coating time of oil phase monomer is 60 seconds, water phase
The coating time of monomer is 1.5 minutes.
It waits for that the coating of entire volume film wire finishes, removes entire volume film wire and carry out heat treatment 12 minutes in 100 DEG C, you can obtain that there is cause
The hollow fiber compound nanofiltration membrane of close compound-split layer.
Embodiment 3
The preparation method of embodiment 3 is substantially the same manner as Example 1, the difference is that, intrinsic Hollow Fiber Ultrafiltration
For liquid level residing for support membrane at 5 meters, the coating time of oil phase monomer is 30 seconds, and the coating time of aqueous phase monomers is 0.5 minute, at heat
The condition of reason is to be heat-treated 50 minutes at 70 DEG C.
Comparative example 1
Hollow Fiber Ultrafiltration support membrane, aqueous phase monomers, oil phase monomer and heat treatment condition are same as Example 1.
Hollow Fiber Ultrafiltration support membrane is placed in aqueous phase monomers and is impregnated 10 minutes, is taken out after spontaneously drying.It is placed in oil phase
60s carries out interface polymerization reaction in monomer, to form composite membrane separating layer in the outer surface of Hollow Fiber Ultrafiltration support membrane, takes out
It is cleaned and dried, then is heat-treated, obtain hollow fiber compound nanofiltration membrane.
Obviously learn that the production efficiency of comparative example 1 is relatively low compared to the production efficiency of Examples 1 to 3 by actual production.And
Hollow fiber compound nanofiltration membrane made from comparative example 1 and Examples 1 to 3 is subjected to yield analysis, the qualification rate of comparative example 1 is
80%, the qualification rate of Examples 1 to 3 is up to 90%.The coating of comparative example 1 is owed uniformly and coating procedure and coating time are difficult to essence
Really control, causes its reproducibility poor.
In addition, at 0.2 mpa by the certified products of hollow fiber compound nanofiltration membrane made from comparative example 1 and Examples 1 to 3
Test the Na of its pure water flux, a concentration of 1000ppm2SO4Rejection and a concentration of 1000ppm MgCl2Rejection, obtain
Pure water flux average value, the Na arrived2SO4Rejection average value and MgCl2Rejection average value, the results are shown in table below.It can
See, separative efficiency also can be improved in this preparation method.
Each technical characteristic of embodiment described above can be combined arbitrarily, to keep description succinct, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, it is all considered to be the range of this specification record.
Several embodiments of the invention above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of interface polymerization reaction device, which is characterized in that including：
Applicator assembly, includes the first groove body for loading aqueous phase monomers and the second groove body for loading oil phase monomer, described
First groove body includes ontology, the first interconnecting part and the second interconnecting part, first interconnecting part and second interconnecting part respectively with
Ontology is connected to and opening up setting；
Guidance set, including the first guide part and the second guide part, first guide part are used for processed product from described
First interconnecting part imports in the ontology of first groove body, and second guide part in the ontology of first groove body for will apply
The processed product for being covered with aqueous phase monomers is imported from second interconnecting part in second groove body, so that the water coated on product
Phase monomer occurs interface polymerization reaction in product surface with oil phase monomer and forms composite membrane；And
Dry component is set between second interconnecting part and second groove body, is waited for coated with aqueous phase monomers for dry
Converted products.
2. interface polymerization reaction device as described in claim 1, which is characterized in that further include for heating first groove body
The first heating component and/or the second heating component for heating second groove body.
3. interface polymerization reaction device as claimed in claim 2, which is characterized in that the applicator assembly further includes being used for first
First temperature control part of groove body inner aqueous phase monomer temperature adjusting control and/or adjust control for oil phase monomer temperature in the second groove body
Second temperature control part of system.
4. interface polymerization reaction device as claimed in claim 2, which is characterized in that the applicator assembly further includes for monitoring
The first pressure of the hydraulic pressure of liquid level residing for the intrinsic processed product of first groove body monitors part and/or for monitoring
State the second pressure monitoring part of the hydraulic pressure of liquid level residing for the processed product in the second groove body.
5. interface polymerization reaction device as described in claim 1, which is characterized in that first groove body is U-shaped structure.
6. interface polymerization reaction device as claimed in claim 5, which is characterized in that first groove body is by multistage both ends open
Pipeline formed by flanged joint.
7. such as claim 1~6 any one of them interface polymerization reaction device, which is characterized in that the dry component includes
Power source and air-dried pipe, the power source are used to provide compressed gas to the air-dried pipe, and the air-dried pipe is set to described second
Between interconnecting part and second groove body, the tube wall of the air-dried pipe is hollow structure, and the tube wall has for being moved with described
Power source connection ventilation inner cavity, and the inner surface of the tube wall be equipped with exhaust vent, in the pore to the air-dried pipe by
Processed product is air-dried.
8. a kind of preparation facilities of hollow fiber compound nanofiltration membrane, which is characterized in that including annealing device and such as claim 1
~7 any one of them interface polymerization reaction devices, the interface polymerization reaction device are used in Hollow Fiber Ultrafiltration support membrane
Surface carry out interface polymerization reaction to form composite membrane separating layer, the annealing device will be for that will be formed with compound UF membrane
The hollow-fibre membrane of layer is heat-treated, the hollow fiber compound nanofiltration membrane is made.
9. a kind of preparation method of hollow fiber compound nanofiltration membrane, which is characterized in that use the doughnut as described in wanting 8 such as right
The preparation facilities of composite nanometer filtering film, the preparation method comprises the following steps：
Hollow Fiber Ultrafiltration support membrane is sequentially passed through described first by first guide part and second guide part to connect
Logical portion, the ontology, second interconnecting part, the dry component and second groove body, the Hollow Fiber Ultrafiltration support
Film coats aqueous phase monomers in first groove body, is dried through the dry component, and oil phase list is coated then at second groove body
Body, and keep the aqueous phase monomers anti-in the generation interfacial polymerization of the surface of the Hollow Fiber Ultrafiltration support membrane with the oil phase monomer
Composite membrane separating layer should be formed；It is heat-treated then at the annealing device, obtains the hollow fiber compound nanofiltration membrane.
10. the preparation method of hollow fiber compound nanofiltration membrane as claimed in claim 9, which is characterized in that the doughnut
The material of ultrafiltration support membrane is polysulfones, polyether sulfone, polyethylene, polypropylene, polyvinyl chloride, polyimides, polyacrylonitrile, gathers inclined fluorine
Ethylene, polytetrafluoroethylene (PTFE) or polyester；
The aqueous phase monomers are piperazine, triaminobenzene, p-aminophenyl, m-aminophenyl, polyethylene glycol sulfuric ester, polyethylene glycol phosphoric acid
The aqueous solution of at least one of ester, quaternary amine polyethylene glycol and polyethylene glycol polyampholyte；The quality of the aqueous solution
Score is 0.5%~5%；
The oil phase monomer is trimesoyl chloride, terephthalyl chloride, isophthaloyl chloride, diisocyanate, epoxychloropropane, two contractings
The mixed liquor of at least one of water glycerin ether and propanetriol-diglycidyl-ether and organic solvent；The organic solvent is n-hexane
At least one of with toluene；
The liquid level of first groove body is 0.5~5m, and the coating time of the aqueous phase monomers is 0.5~5 minute, the oil phase list
The coating time of body is 10~60 seconds.
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| CN201810172608.0A CN108452691B (en) | 2018-03-01 | 2018-03-01 | Interfacial polymerization reaction device, and device and method for preparing hollow fiber composite nanofiltration membrane |
| PCT/CN2018/081413 WO2019165664A1 (en) | 2018-03-01 | 2018-03-30 | Interfacial polymerization reaction device, and hollow fiber composite nanofiltration membrane preparation device and method |
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| CN110772999A (en) * | 2019-10-28 | 2020-02-11 | 德蓝水技术股份有限公司 | Preparation method of special membrane for preparing health water |
| CN110917909A (en) * | 2019-12-27 | 2020-03-27 | 白银图微新材料科技有限公司 | Method for preparing separation membrane by using poly (amino) sulfate polymer and modified polymer thereof as membrane preparation material |
| WO2022252484A1 (en) * | 2021-06-01 | 2022-12-08 | 浙江大学 | Polymer self-supporting nanofilm, continuous and macro-scale preparation method therefor and application thereof |
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Also Published As
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| CN108452691B (en) | 2020-01-14 |
| WO2019165664A1 (en) | 2019-09-06 |
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