CN107149881A - A kind of dopamine modifying polymer film and preparation method thereof - Google Patents
A kind of dopamine modifying polymer film and preparation method thereof Download PDFInfo
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- CN107149881A CN107149881A CN201610114843.3A CN201610114843A CN107149881A CN 107149881 A CN107149881 A CN 107149881A CN 201610114843 A CN201610114843 A CN 201610114843A CN 107149881 A CN107149881 A CN 107149881A
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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
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- 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
- B01D67/0009—Organic membrane manufacture by phase separation, sol-gel transition, evaporation or solvent quenching
- B01D67/0011—Casting solutions therefor
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- 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
- B01D69/04—Tubular membranes
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- 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
- B01D69/06—Flat membranes
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- 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
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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
- B01D71/40—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
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
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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
- B01D2323/12—Specific ratios of components used
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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
- B01D2323/15—Use of additives
- B01D2323/18—Pore-control agents or pore formers
Abstract
The invention discloses one kind based on dopamine modifying polymer film and preparation method thereof, belong to environmentally conscious materials field.Dopamine modifying polymer film is made of following methods：(1) auto polymerization is carried out on polymer powder surface by dopamine, the poly-dopamine functional layer of generation is sticked into polymer powder surface；(2) dopamine modified polymer powders are prepared into film forming using solution conversion film build method.It is an advantage of the invention that be first modified with dopamine to filmogen, then film forming again can be flexibly and easily according to using needing membrane structure；Prepared film has good hydrophily and resistance tocrocking, can further carry out functional modification；Modification does not damage membrane material, and former film physical and chemical performance is not sacrificed, and method is simple, and effect is good, energy-conserving and environment-protective.Prepared film hydrophily and resistance tocrocking are good, it is adaptable to various UF membrane field applications.
Description
Technical field
The present invention relates to a kind of dopamine modifying polymer film and preparation method thereof, specially using dopamine (PDA) to polymer
Filmogen is modified, and then prepares film forming, belongs to environmentally conscious materials field.
Background technology
UF membrane can be operated, without phase transformation in a mild condition, be one of important technology of chemical field.The core of UF membrane is
Film, the structure and physicochemical properties of membrane material is most important to separating property.Conventional membrane material have Kynoar, polysulfones,
Polyether sulfone, polyacrylonitrile etc..These materials have excellent uvioresistant and ageing-resistant ability, and chemical stability is good, room
Do not corroded under temperature by acid, alkali etc., be the filmogen of function admirable while also having preferable heat endurance and mechanical strength.
However, these material modifications are difficult, the extensive use of corresponding membrane is greatly constrained.In order to meet application environment requirement, membrane material
Have to pass through functional modification.At present, the modification of membrane material is divided into grafting and blending and modifying.The grafting that membrane body or surface are carried out
Modified to require harsh to reaction condition, cost is high, and polymer and membrane structure may be by a certain degree of destructions；Though blending and modifying
Right process is simple, but compatibility difference is big between different materials, and modification is uneven.
Researcher is found that one kind with Electrostatic Absorption, hydrogen bond, coordinate bond and supermolecule phase during modified membrane is explored
Method of modifying based on interaction.This method is simple and reliable, and the film surface with complex topography can be modified, and prepares
Organic/organic and organic/inorganic film.
Dopamine is the main component of the mussel adhesion protein secreted by marine organisms mussel pedal gland cell, is left-handed 3,4- dihydroxy
The analog of phenylalanine.Because dopamine contains catechol and amido functional group, it can occur oxidation polymerization, in room
Can be on many inorganic and organic material (including metal, ceramics, timber, quartz and polymer) surface under warm wet environment
Form one layer of poly-dopamine (PDA) composite bed with superpower adhesive force.This adhesion layer has excellent environmental stability, good
Good biocompatibility, excellent hydrophily and the subsequent reactions platform rich in a large amount of-OH.Recent years, some seminar's bases
Study on the modification has been carried out to multiple film surface in dopamine.Zhu seminars by PVDF, PE film with dopamine (Xi Z-Y, Xu Y-Y,
Zhu L-P, et al.Journal of Membrane Science, 2009,327 (1-2)：244-253 and Jiang J-H, Zhu L-P, Zhang
H-T, et al.Journal of Membrane Science, 2014,457：73-81.) be modified, improve membrane material hydrophily and
Resistance tocrocking.Cao etc. is modified using dopamine to the PVDF nano fibrous membranes being made up of electrostatic spinning, is applied
In lithium ion battery separator, lithium ion battery is set there are preferable cycle performance (Cao C, Tan L, Liu W, et al.Journal of
Power Sources, 2014,248：224-229.).Modification is only limitted in existing membrane surface modification above, and original film fenestra can reduce,
Flux can be reduced, and sacrifice original Base film portion performance, and fenestra inter-modification is incomplete.
In view of the shortcomings of the prior art and not enough, the present invention is modified using dopamine from film forming raw material polymer powder, then
Again by phase conversion method film forming, the simultaneously modified film in fenestra and film surface is obtained, the former film for coating and causing after dopamine is overcome
The defect that can be reduced.
The content of the invention
It is an object of the invention to provide a kind of dopamine modifying polymer film and preparation method thereof, by being formed on polymer powder
Dopamine adhesion layer polymer film-forming material is modified, then by forming film with phase transformation method, preparation structure is stable, performance
Homogeneous film, the defect for overcoming the former film properties that painting method is caused after dopamine to reduce.Preparation process of the present invention is simple, it is easy to
Amplification, is adapted to industrial applications.
The preparation method of dopamine Modified Membrane of the present invention is as follows：
(1) Tris-HCl cushioning liquid is prepared, trishydroxymethylaminomethane is dissolved in distilled water, with salt acid for adjusting pH to 8.5, obtained
To Tris-HCl cushioning liquid；
(2) under the stirring of room temperature continuing magnetic force, polymer powder and ethanol are rapidly joined into Tris-HCl cushioning liquid obtained by step (1)
Or isopropanol or glycerine；
(3) by mixed liquor 6~24h of magnetic agitation at 25 DEG C obtained by step (2)；
(4) step (3) products therefrom is subjected to suction filtration, is then washed with deionized-centrifuges 3 times, remove nonadherent poly-dopamine with
And DOPA amine monomers, then product is placed in 40 DEG C of vacuum desiccators and dried to constant weight, the polymer powder of dopamine modification is produced；
(5) 15~35 parts of step (4) resulting polymers powder are weighed respectively by mass fraction, 2~5 parts of pore-foaming agents, 60~83 parts of solvents,
Mixing, 2~6h of stirring is formed after homogeneous casting solution, 0.5~1.5h of vacuum defoamation at 50~70 DEG C, casting solution is poured into dry
On dry clean glass plate, with hymenotome knifing is scraped, it is then placed into obtaining the dopamine modifying polymer film in pure water coagulating bath.
Polymer powder of the present invention is Kynoar (PVDF), polysulfones (PSU), polyether sulfone (PES) or polyacrylonitrile
(PAN) one kind in.
Pore-foaming agent of the present invention is polyethylene pyrrole network alkanone (PVP), polyvinyl alcohol (PEG), epoxy ethane-epoxy propane-epoxy
One kind in ethane (F127) triblock polymer.
Solvent of the present invention is DMF (DMF), DMA (DMAC), N- methylpyrroles
One kind in alkanone (NMP).
Polymer powder of the present invention is modified as modified object thing using dopamine, is then prepared by phase inversion
Polymer film is compared with conventional preparation method to be had the advantage that：
(1) it is easy to operate：It is modified suitable for any polymeric film material, modified condition is gentle, and equipment requirement is low, available for industrializing
Build stability strong, the high functional polymer film of Functional group density.
(2) modifying process environmental protection：Dopamine is in polymer powder modifying process, modification medium is water and a small amount of alcohol, non-environmental-pollution.
(3) modifying process to material structure without destruction：The method is simply in polymer powder surface adhesion poly-dopamine, to raw material
Structure is with performance without destruction.
(4) modified effect is good：Using the film prepared by method of modifying of the present invention, functional group is distributed on film surface and fenestra simultaneously
Homogeneous, density is high, and effect is good.
(5) it is widely applicable：Using first polymer-modified film forming raw material, then film forming, be widely used in different polymeric film materials be modified and
Film preparation, Flat Membrane, the hollow-fibre membrane of different pore size size, tubular membrane and static spinning membrane can be made according to actual needs
Deng.
Embodiment
The present invention is described in further detail with reference to embodiment：
Embodiment 1
(1) 0.1815g trishydroxymethylaminomethanes are dissolved in 300mL distilled water, with salt acid for adjusting pH to 8.5, obtained
Tris-HCl cushioning liquid；
(2) under room temperature magnetic agitation, 0.3g Dopamine hydrochlorides is dissolved in step (1) resulting solution, 6.0g PVDF are rapidly joined
Powder and 10mL ethanol or isopropanol or glycerine；
(3) by the mixed liquor obtained by step (2) under the conditions of 25 DEG C magnetic agitation 6h；
(4) step (3) products therefrom is subjected to suction filtration, is then washed with deionized-centrifuges 3 times, product is then placed in 40 DEG C of vacuum
Dried to constant weight in drier, produce the PVDF powder of dopamine modification；
(5) 15~35 parts of step (4) resulting polymers powder are weighed respectively by mass fraction, 2~5 parts of PVP, 60~83 parts of DMF,
Mixing, 2~6h of stirring forms homogeneous casting solution at 50~70 DEG C, and then after 0.5~1.5h of vacuum defoamation, casting solution is toppled over
In on the glass plate of dried and clean, with hymenotome knifing is scraped, it is then placed into obtaining the dopamine modified poly in pure water coagulating bath
Thing film.
Embodiment 2
(1) be the same as Example 1；
(2) be the same as Example 1；
(3) be the same as Example 1；
(4) be the same as Example 1；
(5) 15~35 parts of step (4) resulting polymers powder are weighed respectively by mass fraction, 2~5 parts of PEG, 60~83 parts of DMF,
Mixing, 2~6h of stirring forms homogeneous casting solution at 50~70 DEG C, and then after 0.5~1.5h of vacuum defoamation, casting solution is toppled over
In on the glass plate of dried and clean, with hymenotome knifing is scraped, it is then placed into obtaining the dopamine modified poly in pure water coagulating bath
Thing film.
Embodiment 3
(1) be the same as Example 1；
(2) be the same as Example 1；
(3) be the same as Example 1；
(4) be the same as Example 1；
(5) 15~35 parts of step (4) resulting polymers powder are weighed respectively by mass fraction, 2~5 parts of F127,60~83 parts of DMF,
Mixing, 2~6h of stirring forms homogeneous casting solution at 50~70 DEG C, and then after 0.5~1.5h of vacuum defoamation, casting solution is toppled over
In on the glass plate of dried and clean, with hymenotome knifing is scraped, it is then placed into obtaining the dopamine modified poly in pure water coagulating bath
Thing film.
Embodiment 4
(1) be the same as Example 1；
(2) be the same as Example 1；
(3) be the same as Example 1；
(4) be the same as Example 1；
(5) weigh 15~35 parts of step (4) resulting polymers powder respectively by mass fraction, 2~5 parts of pore-foaming agent PVP or PEG or
F127,60~83 parts of solvent NMP, mixing, 2~6h of stirring forms homogeneous casting solution at 50~70 DEG C, then vacuum defoamation
After 0.5~1.5h, casting solution is poured on the glass plate of dried and clean, with hymenotome knifing is scraped, pure water coagulating bath is then placed into
In obtain the dopamine modifying polymer film.
Embodiment 5
(1) be the same as Example 1；
(2) be the same as Example 1；
(3) be the same as Example 1；
(4) be the same as Example 1；
(5) weigh 15~35 parts of step (4) resulting polymers powder respectively by mass fraction, 2~5 parts of pore-foaming agent PVP or PEG or
F127,60~83 parts of solvent DMAC, mixing, 2~6h of stirring forms homogeneous casting solution at 50~70 DEG C, and then vacuum takes off
Steep after 0.5~1.5h, casting solution is poured on the glass plate of dried and clean, with hymenotome knifing is scraped, be then placed into pure water solidification
The dopamine modifying polymer film is obtained in bath.
Embodiment 6
(1) be the same as Example 1；
(2) be the same as Example 1；
(3) mixed liquor obtained by step (2) is reacted 10,14,18,24h under 25 DEG C of magnetic agitations；
(4) be the same as Example 1；
(5) weigh 15~35 parts of step (4) resulting polymers powder respectively by mass fraction, 2~5 parts of pore-foaming agent PVP or PEG or
F127,60~83 parts of solvent DMAC or DMF or NMP, mixing, 2~6h of stirring forms homogeneous casting film at 50~70 DEG C
Liquid, then after 0.5~1.5h of vacuum defoamation, casting solution is poured on the glass plate of dried and clean, with hymenotome knifing is scraped, then
It is positioned in pure water coagulating bath and obtains the dopamine modifying polymer film.
Embodiment 7
(1) be the same as Example 1；
(2) under conditions of the stirring of room temperature continuing magnetic force, 0.3g Dopamine hydrochlorides is dissolved in step (1) resulting solution, rapidly joined
6.0g polysulfones (PSU) or polyether sulfone (PES), polyacrylonitrile (PAN) powder and 10mL ethanol or isopropanol or glycerine；
(3) be the same as Example 6；
(4) product obtained by step (3) is subjected to suction filtration, is then washed with deionized-centrifuges 3 times, product is placed in into 40 DEG C of vacuum does
Dried to constant weight in dry device, produce the polysulfones (PSU) or polyether sulfone (PES), polyacrylonitrile (PAN) powder of dopamine modification；
(5) be the same as Example 6.
Embodiment 8
(1) be the same as Example 1；
(2) under conditions of the stirring of room temperature continuing magnetic force, 0.6g Dopamine hydrochlorides is dissolved in step (1) resulting solution, 6.0 are rapidly joined
G Kynoar ethene or polysulfones (PSU), polyether sulfone (PES), polyacrylonitrile (PAN) powder and 10mL ethanol or isopropanol
Or glycerine；
(3) be the same as Example 1；
(4) product obtained by step (3) is subjected to suction filtration, is then washed with deionized-centrifuges 3 times, product is placed in into 40 DEG C of vacuum does
Dried to constant weight in dry device, produce the Kynoar or polysulfones (PSU), polyether sulfone (PES), polyacrylonitrile (PAN) of dopamine modification
Powder；
(5) be the same as Example 6.
Embodiment 9
(1) be the same as Example 1；
(2) be the same as Example 8；
(3) be the same as Example 6；
(4) be the same as Example 8；
(5) be the same as Example 6.
Embodiment 10
(1) 1.815g trishydroxymethylaminomethanes are dissolved in 3000mL distilled water, with salt acid for adjusting pH to 8.5, obtained
Tris-HCl cushioning liquid；
(2) under conditions of the stirring of room temperature continuing magnetic force, 1.0,1.5,4.5,6.0g Dopamine hydrochlorides are dissolved in step (1) resulting solution
In, rapidly join 6.0g Kynoar or polysulfones (PSU), polyether sulfone (PES), polyacrylonitrile (PAN) powder and 100mL
Ethanol or isopropanol or glycerine；
(3) be the same as Example 1；
(4) be the same as Example 8；
(5) be the same as Example 6.
Embodiment 11
(1) be the same as Example 10；
(2) be the same as Example 10；
(3) be the same as Example 6；
(4) be the same as Example 8；
(5) be the same as Example 6.
After testing, dopamine modifying polymer film of the present invention, fenestra pore size is 20.0~250nm, and membrane porosity is
Pure water flux is 200~2000L.m under 90%-99%, 0.1Mpa-2, with good hydrophily, film is loose structure, to ox
Haemocyanin and oil hydrosol have good separating property and contamination resistance；Polymer powder and use that dopamine is modified
The film film surface and fenestra that these powder are obtained contain substantial amounts of hydroxyl and amino-functional group, with very strong further modification power.
Membrane modifying preparation process is simple, it is easy to which industry amplification, modified layer has preferable stability.
It is proposed by the present invention a kind of based on the polymer-modified filmogen of dopamine and its membrane preparation method, carried out by embodiment
Description, person skilled can substantially not depart from present disclosure, content as described herein carried out in spirit and scope
Change or suitably change with combining to realize the present invention.In particular, all similar replacements and change are to ability
It is apparent for field technique personnel, they are considered as being included in spirit, scope and the content of the present invention.
Claims (6)
1. a kind of dopamine modifying polymer film and preparation method thereof, it is characterized in that step is prepared the film by the following method：
(1) Tris-HCl cushioning liquid is prepared：Trishydroxymethylaminomethane is dissolved in distilled water, with salt acid for adjusting pH to 8.5,
Obtain Tris-HCl cushioning liquid；
(2) under conditions of the stirring of room temperature continuing magnetic force, polymerization is rapidly joined in the Tris-HCl cushioning liquid obtained by step (1)
Thing powder and ethanol or isopropanol or glycerine, the polymer powder are Kynoar (PVDF), polysulfones (PSU), gathered
One kind in ether sulfone (PES), polyacrylonitrile (PAN)；
(3) by the mixed liquor obtained by step (2) at 25 DEG C 6~24h of magnetic agitation；
(4) by step, (product of 3 gained carries out suction filtration, is then washed with deionized-centrifuges 3 times, products therefrom is placed in into 40 DEG C
Dried to constant weight in vacuum desiccator, obtain the polymer powder of dopamine modification；
(5) 15~35 parts of step (4) resulting polymers powder are weighed respectively by mass fraction, 2~5 parts of pore-foaming agents, 60~83 parts are molten
Agent, mixing, 2~6h of stirring is formed after homogeneous casting solution, 0.5~1.5h of vacuum defoamation at 50~70 DEG C, and casting solution is toppled over
In on the glass plate of dried and clean, with hymenotome knifing is scraped, it is then placed into obtaining the dopamine modified poly in pure water coagulating bath
Thing film；The solvent is DMF (DMF), DMA (DMAC), 1-METHYLPYRROLIDONE
(NMP) one kind in；The pore-foaming agent is polyethylene pyrrole network alkanone (PVP), polyvinyl alcohol (PEG), epoxy ethane-epoxy propane
One kind in-oxirane (F127) triblock polymer.
2. a kind of dopamine modifying polymer film and preparation method thereof according to claim 1, it is characterized in that the form of the film
It is Flat Membrane.
3. a kind of dopamine modifying polymer film and preparation method thereof according to claim 1, it is characterized in that the film is porous
Film, fenestra size is 20.0~250nm, and membrane porosity is that pure water flux is 200~2000Lm under 90%-99%, 0.1Mpa-2。
4. a kind of dopamine modifying polymer film and preparation method thereof according to claim 1, it is characterized in that the film hydrophily
It is good, there is good separating property to bovine serum albumin and oil hydrosol.
5. a kind of dopamine modifying polymer film and preparation method thereof according to claim 1, it is characterized in that the film surface and
Fenestra contains substantial amounts of hydroxyl and amino-functional group, with very strong further functionalization ability.
6. a kind of dopamine modifying polymer film and preparation method thereof according to claim 1, it is characterized in that the film have it is good
Good antifouling property.
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| CN107486037A (en) * | 2017-09-15 | 2017-12-19 | 福州大学 | A kind of PVDF/PDA composite membranes with super hydrophilicity |
| CN108905647A (en) * | 2018-06-19 | 2018-11-30 | 杭州安诺过滤器材有限公司 | A kind of preparation method of hydrophily polyvinylidene fluoride microfiltration membranes |
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| CN111001307A (en) * | 2019-12-03 | 2020-04-14 | 广西大学 | Preparation method of composite film with replaceable active layer |
| CN111001307B (en) * | 2019-12-03 | 2022-04-05 | 广西大学 | Preparation method of composite film with replaceable active layer |
| CN115051107A (en) * | 2022-06-02 | 2022-09-13 | 哈尔滨工业大学 | Composite diaphragm modified by core-shell nanotube type structural material and preparation method and application thereof |
| CN115051107B (en) * | 2022-06-02 | 2023-08-22 | 哈尔滨工业大学 | Composite diaphragm modified by core-shell nano-tube type structural material and preparation method and application thereof |
| CN115337790A (en) * | 2022-07-15 | 2022-11-15 | 上海工程技术大学 | Preparation method of super-hydrophilic polyether sulfone separation membrane and separation membrane prepared by same |
| CN115337790B (en) * | 2022-07-15 | 2023-10-20 | 上海工程技术大学 | Preparation method of super-hydrophilic polyethersulfone separation membrane and separation membrane prepared by same |
| CN115178097A (en) * | 2022-08-15 | 2022-10-14 | 无锡零界净化设备股份有限公司 | PVDF (polyvinylidene fluoride) microporous filter membrane and preparation process thereof |
| CN115178097B (en) * | 2022-08-15 | 2024-02-23 | 无锡零界净化设备股份有限公司 | PVDF microporous filter membrane and preparation process thereof |
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