CN105582822A - Preparation method of dopamine-modified polysulfone membrane - Google Patents

Preparation method of dopamine-modified polysulfone membrane Download PDF

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Publication number
CN105582822A
CN105582822A CN201610136497.9A CN201610136497A CN105582822A CN 105582822 A CN105582822 A CN 105582822A CN 201610136497 A CN201610136497 A CN 201610136497A CN 105582822 A CN105582822 A CN 105582822A
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China
Prior art keywords
membrane
dopamine
preparation
modification
powder
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Pending
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CN201610136497.9A
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Chinese (zh)
Inventor
武承林
杨健国
应安国
王庆丰
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Taizhou University
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Taizhou University
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Priority to CN201610136497.9A priority Critical patent/CN105582822A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D71/00Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
    • B01D71/06Organic material
    • B01D71/66Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
    • B01D71/68Polysulfones; Polyethersulfones
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • B01D67/0009Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
    • B01D67/0011Casting solutions therefor
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/02Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2325/00Details relating to properties of membranes
    • B01D2325/36Hydrophilic membranes

Abstract

The invention discloses modified polysulfone powder based on dopamine and a preparation method of a dopamine-modified polysulfone membrane. The preparation method of the dopamine-modified polysulfone powder comprises the steps that 1, autopolymerization of dopamine on the surface of polysulfone powder is conducted, and a generated polydopamine functional layer is adhered to the surface of the polysulfone powder; 2, the dopamine-modified polysulfone powder is prepared into the membrane through a solution phase-inversion membrane-forming method. The preparation method has the advantages that dopamine is adopted to modify membrane-forming material polysulfone, and then membrane forming is conducted so that the membrane structure can be flexibly and conveniently regulated and controlled according to the use demand; the prepared polysulfone membrane has the good hydrophilic property and anti-fouling performance and can be further subjected to functional modification; the membrane material is not damaged during modification, the physical and chemical properties of an original membrane are not sacrificed, the method is simple, the effect is good, energy conservation and environment friendliness are achieved, and the method is suitable for industrial production and application.

Description

A kind of dopamine modification PS membrane and preparation method thereof
Technical field
The present invention relates to a kind of dopamine modification PS membrane and preparation method thereof, be specially and adopt dopamine (PDA)Polysulfones filmogen is carried out to modification, then prepare film forming, belong to environmentally conscious materials field.
Background technology
Film separates and can under temperate condition, operate, there is no phase transformation, is one of important technology of chemical field. FilmThe core separating is film, and structure and the physicochemical properties of membrane material are most important to separating property. Commonly useMembrane material has Kynoar, polysulfones, polyether sulfone, polyacrylonitrile etc. These materials have excellent anti-purpleOutside line and ageing-resistant ability, and chemical stability is good, the corrosion such as acid and alkali, alkali under room temperature, simultaneously tool alsoHaving good heat endurance and mechanical strength, is the filmogen of function admirable. But, these material modificationsDifficulty, has greatly restricted the extensive use of corresponding membrane. In order to meet applied environment requirement, membrane material must be throughCross functional modification. At present, the modification of membrane material is divided into grafting and blending and modifying. Carry out on membrane body or surfaceGraft modification reaction condition is required harsh, cost is high, polymer and membrane structure may be suffered to a certain degreeDestruction; Although blending and modifying process is simple, between different materials, compatibility difference is large, and modification is inhomogeneous.
Researcher has found a kind of with Electrostatic Absorption, hydrogen bond, coordination in the process of exploring modified membraneKey and supermolecule interact as basic method of modifying. The method is simple and reliable, can be to having complex shapeThe film modifying surface of looks, prepares organic/organic and organic/inorganic film.
Dopamine is the main component of the secreted mussel adhesion protein of marine organisms mussel pedal gland cell, is leftRevolve the analog of 3,4-dihydroxyphenyl-L-alanine. Because dopamine contains catechol and amido functional group, itsCan there is oxidation polymerization, under room temperature wet environment can many inorganic and organic materials (comprise metal,Pottery, timber, quartz and polymer) surface forms one deck and has the poly-dopamine (PDA) of superpower adhesive forceComposite bed. This adhesion layer has good environmental stability, good biocompatibility, and excellent is hydrophilicProperty and be rich in the subsequent reactions platform of a large amount of-OH. Recent years, some seminars based on dopamine to multipleStudy on the modification has been carried out on film surface. Zhu seminar by PVDF, PE dopamine for film (XiZ-Y, XuY-Y,ZhuL-P, etal.JournalofMembraneScience, 2009,327 (1 – 2): 244-253 and JiangJ-H,ZhuL-P, ZhangH-T, etal.JournalofMembraneScience, 2014,457:73-81.) changeProperty, has improved hydrophily and the resistance tocrocking of membrane material. Cao etc. utilize dopamine to making by electrostatic spinningPVDF nano fibrous membrane carry out modification, be applied to, in lithium ion battery separator, make lithium ion batteryHave good cycle performance (CaoC, TanL, LiuW, etal.JournalofPowerSources, 2014,248:224-229.). Above modification only limits at existing membrane surface modification, and original film fenestra can reduce, and flux can reduce,Sacrificed original basement membrane partial properties, fenestra inter-modification is incomplete.
For the shortcoming and defect of prior art, the present invention adopts dopamine to carry out from film forming raw material polysulfones powderModification, and then by inversion of phases method film forming, obtain the PS membrane of fenestra and the modification simultaneously of film surface, gramTake and apply the defect that the former film properties that causes reduces after dopamine.
Summary of the invention
The object of this invention is to provide a kind of dopamine modification PS membrane and preparation method thereof, by polysulfones powderThe dopamine adhesion layer forming on end carries out modification to filmogen, then by forming film with phase transformation method, and preparationThe film of Stability Analysis of Structures, performance homogeneous, overcomes the defect that painting method causes after dopamine former film properties reduces.Preparation process of the present invention is simple, is easy to amplify, and is applicable to industrial applications.
The preparation method of dopamine Modified Membrane of the present invention is as follows:
(1) preparation tris solution, with salt acid for adjusting pH to 8.5, obtains Tris-HCl buffering moltenLiquid;
(2) continue under magnetic agitation in room temperature, to step (1), gained Tris-HCl adds polysulfones powder in cushioning liquid fastEnd and ethanol or isopropyl alcohol or glycerine;
(3) step (2) gained mixed liquor is stirred to 6~24h at 25 DEG C of lower magnetic forces;
(4) step (3) products therefrom is carried out to suction filtration, then, with deionized water washing-centrifugal 3 times, do not remove and do not adhere toPoly-dopamine and dopamine monomer, then product is placed in 40 DEG C of vacuum desiccators and dries to constant weight,Must gather the polysulfones powder of dopamine modification;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder, 2~5 parts of pore-foaming agents, 60~83 by mass fractionPart solvent, mixes, and stirs 2~6h and form homogeneous casting solution, vacuum defoamation 0.5~1.5h at 50~70 DEG CAfter, casting solution is poured on the glass plate of dried and clean, with scraping hymenotome knifing, be then positioned over pure water solidifyingGu obtain described dopamine modification PS membrane in bathing.
Pore-foaming agent of the present invention is polyethylene pyrrole network alkane ketone (PVP), polyvinyl alcohol (PEG), and oxirane-One in expoxy propane-oxirane (F127) triblock polymer.
Solvent of the present invention is DMF (DMF), DMA (DMAC),One in 1-METHYLPYRROLIDONE (NMP).
Polysulfones powder of the present invention, as modified object thing, adopts dopamine modification, then by turning mutuallyThe PS membrane that change legal system is standby and in the past preparation method relatively have following advantage:
(1) easy and simple to handle: modified condition gentleness, equipment requirement is low, can be used for industrialization structure stability strong, functionThe functional polysulfones film that groups density is high.
(2) modifying process environmental protection: dopamine is in polysulfones powder modification process, and modification medium is water and a small amount of alcohol, nothingEnvironmental pollution.
(3) modifying process to material structure without destruction: the method just adheres to poly-dopamine at polysulfones powder surface, rightRaw-material structure and performance are without destruction.
(4) modified effect is good: utilize the prepared film of method of modifying of the present invention, functional group is simultaneously on film surfaceWith fenestra distribution homogeneous, density is high, effective.
(5) widely applicable: adopt first modification polysulfones film forming raw material, then film forming, is widely used in multi-form film systemStandby, can make according to actual needs flat sheet membrane, the hollow-fibre membrane of different pore size size, tubular membrane and quietElectrospinning cortina etc.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in further detail:
Embodiment 1
(1) 0.1815g trishydroxymethylaminomethane is dissolved in 300mL distilled water, uses salt acid for adjusting pH extremely8.5, obtain Tris-HCl cushioning liquid;
(2) under room temperature magnetic agitation, 0.3g Dopamine hydrochloride is dissolved in step (1) gained solution, add fast6.0g polysulfones powder and 10mL ethanol or isopropyl alcohol or glycerine;
(3) mixed liquor of step (2) gained is stirred to 6h at 25 DEG C of condition lower magnetic forces;
(4) step (3) products therefrom is carried out to suction filtration, then with deionized water washing-centrifugal 3 times, then by productBe placed in 40 DEG C of vacuum desiccators and dry to constant weight, obtain the polysulfones powder of dopamine modification;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder, 2~5 parts of PVP, 60~83 by mass fractionPart DMF, mixes, and stirs 2~6h and form homogeneous casting solution, then vacuum defoamation 0.5~1.5 at 50~70 DEG CAfter h, casting solution is poured on the glass plate of dried and clean, with scraping hymenotome knifing, is then positioned over pure water solidifyingGu obtain described dopamine modification PS membrane in bathing.
Embodiment 2
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) with embodiment 1;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder, 2~5 parts of PEG, 60~83 by mass fractionPart DMF, mixes, and stirs 2~6h and form homogeneous casting solution, then vacuum defoamation 0.5~1.5 at 50~70 DEG CAfter h, casting solution is poured on the glass plate of dried and clean, with scraping hymenotome knifing, is then positioned over pure water solidifyingGu obtain described dopamine modification PS membrane in bathing.
Embodiment 3
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) with embodiment 1;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder, 2~5 parts of F127,60~83 by mass fractionPart DMF, mixes, and stirs 2~6h and form homogeneous casting solution, then vacuum defoamation 0.5~1.5 at 50~70 DEG CAfter h, casting solution is poured on the glass plate of dried and clean, with scraping hymenotome knifing, is then positioned over pure water solidifyingGu obtain described dopamine modification PS membrane in bathing.
Embodiment 4
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) with embodiment 1;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder by mass fraction, 2~5 parts of pore-foaming agent PVP orPEG or F127,60~83 parts of solvent NMP, mix, and stir 2~6h and form homogeneous casting at 50~70 DEG CFilm liquid, then, after vacuum defoamation 0.5~1.5h, is poured into casting solution on the glass plate of dried and clean, with scrapingHymenotome knifing, is then positioned over and in pure water coagulating bath, obtains described dopamine modification PS membrane.
Embodiment 5
(1) with embodiment 1;
(2) with embodiment 1;
(3) with embodiment 1;
(4) with embodiment 1;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder by mass fraction, 2~5 parts of pore-foaming agent PVP orPEG or F127,60~83 parts of solvent DMAC, mix, and stir 2~6h and form homogeneous at 50~70 DEG CCasting solution, then, after vacuum defoamation 0.5~1.5h, is poured into casting solution on the glass plate of dried and clean, usesScrape hymenotome knifing, be then positioned over and in pure water coagulating bath, obtain described dopamine modification PS membrane.
Embodiment 6
(1) with embodiment 1;
(2) with embodiment 1;
(3) mixed liquor of step (2) gained is reacted to 10,14,18,24h under 25 DEG C of magnetic agitation;
(4) with embodiment 1;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder by mass fraction, 2~5 parts of pore-foaming agent PVP orPEG or F127,60~83 parts of solvent DMAC or DMF or NMP, mix, and at 50~70 DEG C, stirsMix 2~6h and form homogeneous casting solution, then, after vacuum defoamation 0.5~1.5h, casting solution is poured into dry cleanOn clean glass plate, with scraping hymenotome knifing, be then positioned over and in pure water coagulating bath, obtain described dopamine modificationPS membrane.
Embodiment 7
(1) 1.815g trishydroxymethylaminomethane is dissolved in 3000mL distilled water, uses salt acid for adjusting pH extremely8.5, obtain Tris-HCl cushioning liquid;
(2) continue, under the condition of magnetic agitation, 1.0,1.5,4.5,6.0g Dopamine hydrochloride to be dissolved in to step in room temperature(1), in gained solution, add fast 6.0g polysulfones powder and 100mL ethanol or isopropyl alcohol or glycerine;
(3) with embodiment 1;
(4) with embodiment 1;
(5) with embodiment 6.
Embodiment 8
(1) with embodiment 7;
(2) with embodiment 7;
(3) with embodiment 6;
(4) with embodiment 1;
(5) with embodiment 6.
After testing, dopamine modification PS membrane of the present invention, fenestra pore size is 50.0~200nm, filmPorosity is 85%-96%, and under 0.1Mpa, pure water flux is 300~1500Lm-2, there is good hydrophily,Film is loose structure, and bovine serum albumin and oil hydrosol are had to good separating property and contamination resistance;The polysulfones powder of dopamine modification and use PS membrane that these powder obtain containing a large amount of hydroxyl and amino officialsEnergy group, has very strong further modification ability. Film modification preparation process is simple, and be easy to industry and amplify,Modified layer has good stability.
The present invention propose one based on dopamine modification polysulfones filmogen and membrane preparation method thereof,Be described by embodiment, person skilled obviously can do not depart from of the present invention inIn appearance, spirit and scope, content as herein described changed or suitably change with combination and realizeThe present invention. Special needs to be pointed out is, all similar replacements and change are to art technology peopleMember is apparent obtaining, and they are deemed to be included in spirit of the present invention, scope and contentIn.

Claims (7)

1. dopamine modification PS membrane and preparation method thereof, is characterized in that this film step system by the following methodStandby obtaining:
(1) preparation tris solution, with salt acid for adjusting pH to 8.5, obtains Tris-HCl slowDissolved liquid;
(2) continue under the condition of magnetic agitation in room temperature, fast in the Tris-HCl cushioning liquid of step (1) gainedSpeed adds polysulfones powder and ethanol or isopropyl alcohol or glycerine;
(3) mixed liquor of step (2) gained is stirred to 6~24h at 25 DEG C of lower magnetic forces;
(4) by step, (product of 3 gained carries out suction filtration, then with deionized water washing-centrifugal 3 times, by instituteProduct is placed in 40 DEG C of vacuum desiccators and dries to constant weight, obtain the polysulfones powder of dopamine modification;
(5) take respectively 15~35 parts of steps (4) gained polysulfones powder by mass fraction, 2~5 parts of pore-foaming agents,60~83 parts of solvents, mix, and stir 2~6h and form homogeneous casting solution, vacuum defoamation 0.5~1.5 at 50~70 DEG CAfter h, casting solution is poured on the glass plate of dried and clean, with scraping hymenotome knifing, is then positioned over pure water solidifyingGu obtain described dopamine modification PS membrane in bathing; Described solvent is DMF (DMF), N, N-Dimethylacetylamide (DMAC), the one in 1-METHYLPYRROLIDONE (NMP); Described pore-foaming agent is polyethylenePyrrole network alkane ketone (PVP), polyvinyl alcohol (PEG), epoxy ethane-epoxy propane-oxirane (F127) three blocksOne in polymer.
2. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that instituteThe form of the film of stating is flat sheet membrane.
3. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that film isPerforated membrane, fenestra size is 20.0~250nm, and membrane porosity is 90%-99%, and under 0.1Mpa, pure water flux is200~2000L·m-2
4. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that gainedFilm good hydrophilic property, has good separating property and contamination resistance to bovine serum albumin and oil hydrosol.
5. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that manyCling to the polysulfones powder of amine modification and use the film that these powder obtain to contain a large amount of hydroxyl and amino-functional basesGroup, has very strong further functionalization ability.
6. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that changingProperty be to adhere to poly-dopamine layer at polysulfones powder surface, to former polysulfones structure and performance without destruction.
7. a kind of dopamine modification PS membrane and preparation method thereof according to claim 1, is characterized in that systemStandby technique is simple, modified effect excellence, and energy-conserving and environment-protective, can industrialization build that stability is strong, form is variousHydrophilic polysulfone membrane, is applicable to suitability for industrialized production and application.
CN201610136497.9A 2016-03-10 2016-03-10 Preparation method of dopamine-modified polysulfone membrane Pending CN105582822A (en)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106139917A (en) * 2016-08-19 2016-11-23 杭州易膜环保科技有限公司 A kind of method of biomimetic modification polyvinylidene fluoride film hydrophilically
CN106474546A (en) * 2016-09-09 2017-03-08 华南理工大学 A kind of electric polypyrrole/poly-dopamine nanofiber and preparation method and application
CN106669468A (en) * 2016-12-20 2017-05-17 济南大学 Metal doped g-C3N4 based visible light catalysis flat plate type ultra-filtration membrane and preparation method
CN106757789A (en) * 2017-01-11 2017-05-31 西南交通大学 A kind of preparation method of super hydrophilic polyvinylidene fluoride/poly-dopamine laminated film
CN107486037A (en) * 2017-09-15 2017-12-19 福州大学 A kind of PVDF/PDA composite membranes with super hydrophilicity
CN108144559A (en) * 2018-02-24 2018-06-12 清华大学 A kind of catalytic film reactor based on nuclear track membrane and preparation method thereof
CN108772106A (en) * 2018-03-29 2018-11-09 天津工业大学 The preparation method and its functional method of fiber reinforcement type hollow Nano fiber in use film
CN111420559A (en) * 2020-01-13 2020-07-17 天津科技大学 Surface modification method of polymeric membrane based on dopamine

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CN104466063A (en) * 2014-12-09 2015-03-25 吉林省聚科高新材料有限公司 Polydopamine surface modified polyether sulfone nanofiber composite diaphragm and preparation method and applications
CN105013336A (en) * 2015-06-30 2015-11-04 天津大学 Preparation method of nano silver/poly dopamine composite membrane
CN107149882A (en) * 2016-03-02 2017-09-12 天津工业大学 A kind of Kynoar pollution-resistant membrane and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104466063A (en) * 2014-12-09 2015-03-25 吉林省聚科高新材料有限公司 Polydopamine surface modified polyether sulfone nanofiber composite diaphragm and preparation method and applications
CN105013336A (en) * 2015-06-30 2015-11-04 天津大学 Preparation method of nano silver/poly dopamine composite membrane
CN107149882A (en) * 2016-03-02 2017-09-12 天津工业大学 A kind of Kynoar pollution-resistant membrane and preparation method thereof

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106139917A (en) * 2016-08-19 2016-11-23 杭州易膜环保科技有限公司 A kind of method of biomimetic modification polyvinylidene fluoride film hydrophilically
CN106474546A (en) * 2016-09-09 2017-03-08 华南理工大学 A kind of electric polypyrrole/poly-dopamine nanofiber and preparation method and application
CN106474546B (en) * 2016-09-09 2019-10-18 华南理工大学 A kind of electric polypyrrole/poly-dopamine nanofiber and the preparation method and application thereof
CN106669468A (en) * 2016-12-20 2017-05-17 济南大学 Metal doped g-C3N4 based visible light catalysis flat plate type ultra-filtration membrane and preparation method
CN106669468B (en) * 2016-12-20 2019-10-25 济南大学 Based on metal-doped g-C3N4Visible light catalytic flat-plate ultrafiltration membrane and preparation method
CN106757789A (en) * 2017-01-11 2017-05-31 西南交通大学 A kind of preparation method of super hydrophilic polyvinylidene fluoride/poly-dopamine laminated film
CN107486037A (en) * 2017-09-15 2017-12-19 福州大学 A kind of PVDF/PDA composite membranes with super hydrophilicity
CN108144559A (en) * 2018-02-24 2018-06-12 清华大学 A kind of catalytic film reactor based on nuclear track membrane and preparation method thereof
CN108772106A (en) * 2018-03-29 2018-11-09 天津工业大学 The preparation method and its functional method of fiber reinforcement type hollow Nano fiber in use film
CN111420559A (en) * 2020-01-13 2020-07-17 天津科技大学 Surface modification method of polymeric membrane based on dopamine

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