CN108722209A - A kind of processing technology of graphene hybridized film - Google Patents
A kind of processing technology of graphene hybridized film Download PDFInfo
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- CN108722209A CN108722209A CN201810604349.4A CN201810604349A CN108722209A CN 108722209 A CN108722209 A CN 108722209A CN 201810604349 A CN201810604349 A CN 201810604349A CN 108722209 A CN108722209 A CN 108722209A
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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
- B01D71/76—Macromolecular material not specifically provided for in a single one of groups B01D71/08 - B01D71/74
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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
- B01D67/0079—Manufacture of membranes comprising organic and inorganic components
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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
- B01D2323/30—Cross-linking
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- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention belongs to new material technology fields, more particularly to a kind of processing technology of graphene hybridized film, it is by crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, is uniformly mixed according to certain proportioning to dioxanone and deionized water, carrier film is put into modified solution under room temperature to take out after stir process and is cleaned up, for use, the carrier membrane material is aromatic polyimide；By it is graphene oxide-loaded on a carrier film；It by the carrier film solution coating of continuous phase in the carrier film for having loaded graphene oxide, then dries, removes solvent, then demoulding, obtain hybridized film.The present invention increases the crosslinking degree of carrier film functional layer, hence it is evident that the surface soundness for improving functional layer contributes to form homogeneous phase hybrid film system, improves the separation of hybridized film by the way that carrier film to be modified.
Description
Technical field
The present invention relates to new material technology fields, it particularly relates to a kind of processing technology of graphene hybridized film.
Background technology
Infiltration evaporation is the novel membrane technology detached for liquid mixture, is to drive using permeable pressure head between each component
Power dissolves in film by each component and diffusion rate difference reaches separation purpose.The outstanding advantages of the technology are low energy consumption,
Easy to operate, process is pollution-free.
Organic polymer films have many advantages, such as that flexibility good, good penetrability, density is low, cheap and good film-forming property,
But its solvent resistant, corrosion-resistant and heat resistance are all poor, and enough selectivity and permeation flux cannot be provided to some systems.
And inorganic film-strength is high, corrosion-resistant, solvent resistant and high temperature resistant, but inorganic material is crisp, and not easy to be processed, film forming is poor, at present price
It is also more expensive.In order to concentrate the advantage of organic film and inoranic membrane respectively, people to devise organic-inorganic hybrid membrane.This film
With good physical and chemical stability and separating property, and good film-forming property, it has also become macromolecule and material science, membrane material system
The standby research hotspot for waiting fields.According to the interaction type between organic and inorganic component, hybrid inorganic-organic materials can be divided into
Two major classes：One kind is tied with weak interaction-secondary bond (Van der Waals force, hydrogen bond or weak electrostatic interaction) between organic and inorganic component
The hybrid material of conjunction forms the composite material with embedding phase.Another kind of is between organic and inorganic component with strong interaction-change
Learn the hybrid material that key (such as covalent bond, ionic-covalent bonds and coordinate bond) combines.In this kind of hybridized film between organic and inorganic component
It combines closely to form the good hybrid material of compatibility by strong chemical bond, improves the performance of homogenous material.But it is existing
Hybridized film separation selectivity is relatively low, influences the practical performance of hybridized film.
Invention content
In view of this, the object of the present invention is to provide a kind of processing technologys of graphene hybridized film, to solve existing hydridization
UF membrane it is selectively relatively low and.
The present invention solves above-mentioned technical problem by the following technical programs：
A kind of processing technology of graphene hybridized film, includes the following steps：
（1）By crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, to dioxanone and deionized water according to
Certain proportioning is uniformly mixed, and modified solution is made；
（2）Carrier film is put into modified solution under room temperature to take out after 40 ~ 80min of stir process and is cleaned up, for use, the load
Body membrane material is aromatic polyimide；
（3）By graphene oxide-loaded in step（2）In carrier film that treated；
（4）It by the carrier film solution coating of continuous phase in the carrier film for having loaded graphene oxide, then dries, removes molten
Agent, then demoulding, obtain hybridized film.
The crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, to dioxanone and deionized water
Weight ratio is（1~2）：（120~180）：（40~60）：（250~350）：1000.
The method of the load is dip coating.
The method of the load is：Graphene oxide is scattered in ethyl alcohol, the dispersion of 0.8 ~ 4wt% is made, super
Ultrasonic disperse handles 1 ~ 2h under conditions of acoustic frequency is 20 ~ 100KHz；With the dispersion impregnate carrier film, temperature be 60 ~
80 DEG C, supersonic frequency be 10 ~ 18KHz under conditions of after 30 ~ 50min of infiltration, drying is taken out, repeatedly after 1 ~ 5 time, i.e., by oxygen
Graphite alkene is supported on carrier film surface.
The carrier coating solution of the continuous phase is hexamethylene, a concentration of 15 ~ 30wt% of hexamethylene.
The temperature of the drying process is 60 ~ 80 DEG C, and the time is 20 ~ 40min.
The step of demoulding is：Carrier film with carrier film and graphene oxide is subjected to hot place at 120 ~ 200 DEG C
Manage 20 ~ 30min, you can demoulding.
The thickness of the hybridized film is 40 ~ 70 μm.
The form of the carrier film is plate and frame, rolling, tubular type or hollow fiber form.
The size of the graphene oxide particle is 5 ~ 20 μm.
The crosslinking agent is polyacrylamide.
The beneficial effects of the present invention are：The present invention increases the friendship of carrier film functional layer by the way that carrier film to be modified
Connection degree is crosslinked one layer of modification " healing " thin layer, hence it is evident that improve the surface soundness of functional layer again on carrier layer so that carries
Body film surface is more smooth and closely knit, can effectively inhibit the phase separation of hybrid organic-inorganic film, contributes to form homogeneous miscellaneous
Change film system, improves the separation of hybridized film.
Specific implementation mode
In order to facilitate the understanding of those skilled in the art, below in conjunction with embodiment, the present invention will be further described.
Embodiment is only to the invention for example, not being limitation of the invention, the step of not illustrated in embodiment
It is prior art, is not described in detail herein.
Embodiment one
A kind of preparation method of hybridized film, includes the following steps：
（1）By crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, to dioxanone and deionized water with 1：
120：40：250：1000 weight ratio is uniformly mixed and is configured to modified solution, for use；
（2）After carrier film is put into modified solution stir process 40min at normal temperatures, carrier film taking-up is cleaned with clear water and is done
Only it and drains, for use, the carrier membrane material is aromatic polyimide；
（3）Graphene oxide is scattered in ethyl alcohol, the dispersion of a concentration of 0.8wt% is made, by the dispersion in ultrasound
Ultrasonic disperse handles 1h under conditions of frequency is 20KHz；Carrier film is impregnated with the dispersion, is 60 DEG C, supersonic frequency in temperature
Under conditions of rate is 10KHz after infiltration 30min, takes out carrier film and it is dried 20min at a temperature of 60 DEG C, so
Repeatedly after 1 time, i.e., by graphene oxide-loaded in carrier film surface；
（4）By the carrier film solution coating of continuous phase in the carrier film for having loaded graphene oxide, then carrier film is at 60 DEG C
At a temperature of be dried 20min, rotary evaporation removes solvent, by the carrier film with carrier film and graphene oxide 120
DEG C carry out heat treatment 20min, you can demoulding obtains hybridized film.
The carrier coating solution of the continuous phase is hexamethylene, a concentration of 15wt% of hexamethylene.
The thickness of the hybridized film is 40 μm.
The form of the carrier film is plate and frame, rolling, tubular type or hollow fiber form.
The size of the graphene oxide particle is 5 μm.
The crosslinking agent is polyacrylamide.
Embodiment two
A kind of preparation method of hybridized film, includes the following steps：
（1）By crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, to dioxanone and deionized water with 2：
180：60：350：1000 weight ratio is uniformly mixed and is configured to modified solution, for use；
（2）After carrier film is put into modified solution stir process 80min at normal temperatures, carrier film taking-up is cleaned with clear water and is done
Only it and drains, for use, the carrier membrane material is aromatic polyimide；
（3）Graphene oxide is scattered in ethyl alcohol, the dispersion of a concentration of 4wt% is made, by the dispersion in supersonic frequency
Ultrasonic disperse handles 2h under conditions of rate is 100KHz；Carrier film is impregnated with the dispersion, is 80 DEG C, supersonic frequency in temperature
After infiltrating 50min under conditions of 18KHz, takes out carrier film and it is dried 40min at a temperature of 80 DEG C, it is so anti-
After 5 times multiple, i.e., by graphene oxide-loaded in carrier film surface；
（4）By the carrier film solution coating of continuous phase in the carrier film for having loaded graphene oxide, then carrier film is at 80 DEG C
At a temperature of be dried 40min, rotary evaporation removes solvent, by the carrier film with carrier film and graphene oxide 200
DEG C carry out heat treatment 30min, you can demoulding obtains hybridized film.
Claims (9)
1. a kind of processing technology of graphene hybridized film, it is characterised in that include the following steps：
（1）By crosslinking agent, trisiloxanes polyether ester, alkyl polyoxyethylene ether, to dioxanone and deionized water according to
Certain proportioning is uniformly mixed, and modified solution is made；
（2）Carrier film is put into modified solution under room temperature to take out after 40 ~ 80min of stir process and is cleaned up, for use, the load
Body membrane material is aromatic polyimide；
（3）By graphene oxide-loaded in step（2）In carrier film that treated；
（4）It by the carrier film solution coating of continuous phase in the carrier film for having loaded graphene oxide, then dries, removes molten
Agent, then demoulding, obtain hybridized film.
2. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The crosslinking agent, trisiloxanes
Polyether ester, alkyl polyoxyethylene ether are to the weight ratio of dioxanone and deionized water（1~2）：（120~180）：（40
~60）：（250~350）：1000.
3. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The method of the load is：It will
Graphene oxide is scattered in ethyl alcohol, and the dispersion of 0.8 ~ 4wt% is made, super under conditions of supersonic frequency is 20 ~ 100KHz
1 ~ 2h of sound decentralized processing；Carrier film is impregnated with the dispersion, in the item that temperature is 60 ~ 80 DEG C, supersonic frequency is 10 ~ 18KHz
After infiltrating 30 ~ 50min under part, drying is taken out, repeatedly after 1 ~ 5 time, i.e., by graphene oxide-loaded in carrier film surface.
4. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The carrier film of the continuous phase is molten
Liquid is hexamethylene, a concentration of 15 ~ 30wt% of hexamethylene.
5. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The temperature of the drying process is
60 ~ 80 DEG C, the time is 20 ~ 40min.
6. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The step of demoulding is：It will
Carrier film with carrier film and graphene oxide carries out 20 ~ 30min of heat treatment at 120 ~ 200 DEG C, you can demoulding.
7. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The thickness of the hybridized film is 40
~70μm。
8. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The graphene oxide particle
Size is 5 ~ 20 μm.
9. the processing technology of graphene hybridized film as described in claim 1, it is characterised in that：The crosslinking agent is polyacrylamide
Amine.
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| JP2013000633A (en) * | 2011-06-14 | 2013-01-07 | Sekisui Chem Co Ltd | Method for manufacturing porous membrane |
| CN103894074A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | Novel hybrid membrane as well as preparation method and application thereof |
| KR20150101039A (en) * | 2014-02-25 | 2015-09-03 | 코오롱패션머티리얼 (주) | Porous support, method for manufacturing the same, and reinforced membrane comprising the same |
| CN106268348A (en) * | 2016-08-08 | 2017-01-04 | 太原市晋华恒远科技有限公司 | A kind of preparation method of super-hydrophobic polyphenylene sulfide film |
| CN106582318A (en) * | 2016-12-20 | 2017-04-26 | 南京工业大学 | Graphene oxide-modified organic solvent-resistant nanofiltration membrane, preparation method and application |
| CN106752318A (en) * | 2015-11-25 | 2017-05-31 | 重庆伟恒包装有限公司 | It is applied to the printing-ink on ITO base materials |
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2018
- 2018-06-13 CN CN201810604349.4A patent/CN108722209A/en active Pending
Patent Citations (7)
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|---|---|---|---|---|
| CN101234298A (en) * | 2007-01-29 | 2008-08-06 | 北京联合大学应用文理学院 | Porous filter membrane prepared by plant base raw material |
| JP2013000633A (en) * | 2011-06-14 | 2013-01-07 | Sekisui Chem Co Ltd | Method for manufacturing porous membrane |
| CN103894074A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | Novel hybrid membrane as well as preparation method and application thereof |
| KR20150101039A (en) * | 2014-02-25 | 2015-09-03 | 코오롱패션머티리얼 (주) | Porous support, method for manufacturing the same, and reinforced membrane comprising the same |
| CN106752318A (en) * | 2015-11-25 | 2017-05-31 | 重庆伟恒包装有限公司 | It is applied to the printing-ink on ITO base materials |
| CN106268348A (en) * | 2016-08-08 | 2017-01-04 | 太原市晋华恒远科技有限公司 | A kind of preparation method of super-hydrophobic polyphenylene sulfide film |
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