CN108479435A - A kind of preparation method of ceramic base polyvinyl acetate composite membrane - Google Patents
A kind of preparation method of ceramic base polyvinyl acetate composite membrane Download PDFInfo
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- CN108479435A CN108479435A CN201810339927.6A CN201810339927A CN108479435A CN 108479435 A CN108479435 A CN 108479435A CN 201810339927 A CN201810339927 A CN 201810339927A CN 108479435 A CN108479435 A CN 108479435A
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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
- 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
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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
- B01D2323/46—Impregnation
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Abstract
A kind of preparation method of ceramic base polyvinyl acetate composite membrane, belongs to technology of composite film preparation field.The method is:Ceramic pipe type film surface hydroxylating pre-processes:It after cleaning ceramic tubular membrane, is impregnated in hydrochloric acid, deionized water successively, is dried in vacuo, is subsequently placed in climatic chamber;Ceramic pipe type film intimal surface silanization:Ceramic pipe type film is placed in stainless steel component, shell side is pure dimethylbenzene, and tube side is silane coupler solution, after reaction, ceramic pipe type film is taken out from stainless steel membrane component, is dried in vacuo after cleaning;The ceramic pipe type film of vinyl acetate grafted silane:Ceramic pipe type film is placed in stainless steel component, shell side is full of pure ethyl acetate, configures polymer monomer solution, and heating circulates after initiator is added in tube side, after reaction, ceramic pipe type film is taken out from membrane module, is dried in vacuo after cleaning.Modified technique flow of the present invention is simple and convenient, modified condition is mild, expense is relatively low, is convenient for industrialization promotion.
Description
Technical field
The invention belongs to technology of composite film preparation fields, and in particular to a kind of system of ceramic base polyvinyl acetate composite membrane
Preparation Method.
Background technology
In face of the energy resource structure of China's " rich coal, oil-poor, few gas ", Chemical Industry is effectively converted into energy using coal resource
Source.But development Chemical Industry can bring pressure to ecology and environment, it includes high-concentration phenol to be primarily due to coal chemical industrial waste water
Substance and poisonous and harmful substance make it be difficult to by traditional bioanalysis degradation treatment.Pervaporation is as a kind of new membrane point
From technology, there are efficient simple, environmental-friendly, low power consumption and other advantages, it is a kind of " green technology " to be recognized.However, to current
Until, for commercial polymer film there are no being used widely in pervaporation technology, main cause is that organic film is easily swollen, and is led
The reduction of film properties is caused, or even loses the integrality of film.
Ceramic membrane has many advantages, such as good chemical stability, mechanical property, thermal stability, high temperature resistant, but poor selectivity,
Using the organic matter in inorganic film process waste water, it is clear that removal rate cannot reach maximization, therefore ceramic support composite membrane of polymer
As the development trend of pervaporation technology.Therefore, ceramic membrane is modified, by the rigid, heat-resisting, chemical steady of inorganic material
It is qualitative to be combined with the selectivity of polymer, so that mechanical strength, pore performance, the selection performance of the composite membrane of preparation is increased,
And then the selectivity and separating rate of UF membrane are improved, to achieve the purpose that efficiently to remove phenol for coal chemical industrial waste water, for industry
Large-scale application provides data and theories integration.
The method of current ceramics membrane modifying mainly has surface cladding process, the skills such as uv photo initiated grafting method and plasma grafting method
Art.Ai Siweier publishing houses periodical Journal of Membrane Science(2016,510,338-347)Describe one kind
The preparation method of ceramic base polyether block amide composite membrane.By will pre-process Ceramic Hollow Fiber immersion coating solution 1 ~
Then 5min is pulled out with the speed of about 3 ~ 6cm/s and is prepared ceramic base polyether block amide composite membrane.Composite membrane film 1-3 times,
Prepare the different composite membrane of film thickness.Composite membrane prepared by this physical method polymer in pervaporation technology is easy to fall off,
It is unfavorable for mass producing.In summary, ceramic membrane has good chemical stability, mechanical property, thermal stability, high temperature resistant
The advantages that, but poor selectivity, its application in technical field of membrane is limited, existing preparation method polymer coating is easy to fall off, locates
Manage complex process, energy consumption and it is costly the problems such as, it is difficult to carry out large-scale industrialization popularization and application.
Invention content
The purpose of the present invention is to solve ceramic membrane poor selectivity, the compound membrane preparation methods of existing ceramic-base
There is a problem of polymer coating easy to fall off, complex treatment process, energy consumption with it is costly, a kind of poly- acetic acid second of ceramic base is provided
The preparation method of enester composite membrane, the compound Membrane pore property of preparation, selection performance increase, and then improve the choosing of UF membrane
Selecting property and separating rate.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of ceramic base polyvinyl acetate composite membrane, steps are as follows for the method:
Step 1:Ceramic pipe type film surface hydroxylating pre-processes:Ceramic pipe type film is cleaned by ultrasonic 5 in acetone, ethyl alcohol, water successively
Ceramic pipe type film after cleaning in the hydrochloric acid of 1wt.% is impregnated 30 ~ 180min, then gone by ~ 30min, ultrasonic power 250w
10 ~ 30min is impregnated in ionized water, is taken out film and is dried in vacuo 24 h at a temperature of 110 DEG C, then by ceramic pipe type film in deionization
30min is submerged in water, dries 1h at room temperature, is subsequently placed in the climatic chamber that humidity is 35 ~ 65%, 24 are balanced at 20 ~ 28 DEG C
H obtains the ceramic pipe type film of surface hydroxylation;
Step 2:Ceramic pipe type film intimal surface silanization:The ceramic pipe type film that step 1 pre-processes is placed in homemade
In stainless steel membrane component, the shell side of stainless steel membrane component is full of pure dimethylbenzene, and shell side sealing configures 5 ~ 15wt.% silane coupling agents
Xylene solution, and place it in 1L opening three-necked flask reactor in, which is connected with 70 ~ 75 DEG C of condenser,
Reaction solution is warming up to 138 DEG C in oil bath pan, is circulated in the tube side of stainless steel membrane component under the promotion of peristaltic pump, fortune
2 ~ 7 h of row time takes out ceramic pipe type film from stainless steel membrane component, 3 ceramic tubes is cleaned with pure dimethylbenzene after reaction
Then formula film dries 24 h in 140 DEG C of vacuum drying chamber;
Step 3:The ceramic pipe type film of vinyl acetate grafted silane:The ceramic pipe type film of step 2 silanization is placed in not
It becomes rusty in steel component, stainless steel membrane component shell side is full of pure ethyl acetate or water, and shell side sealing configures 5 ~ 50 wt.% polymer lists
The ethyl acetate solution of body is placed in the reaction vessel of nitrogen atmosphere, reaction temperature be increased to 30 ~ 70 DEG C after be added 0 ~
0.05mol/L initiators circulate under the promotion of peristaltic pump in the tube side of stainless steel membrane component, 1 ~ 6 h of run time,
After reaction, ceramic pipe type film is taken out from stainless steel membrane component, is cleaned 3 ceramic pipe type films with ethyl acetate, is then existed
Dry 24 h in 110 DEG C of vacuum drying chamber.
The advantageous effect of the present invention compared with the existing technology is:The present invention is using vinyltrimethoxysilane as silane
Coupling agent carries out silanization, two kinds of different chemical functional groups that silane both ends are contained, one end energy and ceramic membrane to ceramic membrane surface
The hydroxyl reaction on surface generates covalent bond;The other end can generate covalent bond with vinyl acetate, to make two kinds of nature differences very
Big material " coupling " gets up, and plays the role of improving composite property, entire modified technique flow is simple and convenient, is modified item
Part is mild, expense is relatively low, is convenient for industrialization promotion.
Specific implementation mode
Technical scheme of the present invention is further described with reference to embodiment, however, it is not limited to this, every right
Technical solution of the present invention is modified or equivalent replacement, without departing from the spirit of the technical scheme of the invention range, should all cover
Among protection scope of the present invention.
Specific implementation mode one:What present embodiment was recorded is a kind of preparation side of ceramic base polyvinyl acetate composite membrane
Method, steps are as follows for the method:
Step 1:Ceramic pipe type film surface hydroxylating pre-processes:Ceramic pipe type film is cleaned by ultrasonic 5 in acetone, ethyl alcohol, water successively
~ 30min, ultrasonic power are that the ceramic pipe type film after cleaning is impregnated 30 ~ 180min by 250w in the hydrochloric acid of 1wt.%, then is being gone
10 ~ 30min is impregnated in ionized water, is taken out film and is dried in vacuo 24 h at a temperature of 110 DEG C, then by ceramic pipe type film in deionization
30min is submerged in water, dries 1h at room temperature, is subsequently placed in the climatic chamber that humidity is 35 ~ 65%, 24 are balanced at 20 ~ 28 DEG C
H obtains the ceramic pipe type film of surface hydroxylation;
Step 2:Ceramic pipe type film intimal surface silanization:The ceramic pipe type film that step 1 pre-processes is placed in homemade
In stainless steel membrane component, the shell side of stainless steel membrane component is full of pure dimethylbenzene, and shell side sealing configures 5 ~ 15wt.% silane coupling agents
Xylene solution, and place it in 1L opening three-necked flask reactor in, which is connected with 70 ~ 75 DEG C of condenser,
Reaction solution is warming up to 138 DEG C in oil bath pan, is circulated in the tube side of stainless steel membrane component under the promotion of peristaltic pump, fortune
2 ~ 7 h of row time takes out ceramic pipe type film from stainless steel membrane component, 3 ceramic tubes is cleaned with pure dimethylbenzene after reaction
Formula film removes unreacted silane molecule, then dry 24 h in 140 DEG C of vacuum drying chamber;
Step 3:The ceramic pipe type film of vinyl acetate grafted silane:The ceramic pipe type film of step 2 silanization is placed in not
It becomes rusty in steel component, stainless steel membrane component shell side is full of pure ethyl acetate or water, and shell side sealing configures 5 ~ 50% polymer monomers
Ethyl acetate solution is placed in the reaction vessel of nitrogen atmosphere, and reaction temperature is added 0 ~ 0.05mol/L after being increased to 30 ~ 70 DEG C and draws
Agent is sent out, is circulated in the tube side of stainless steel component under the promotion of peristaltic pump, 1 ~ 6 h of run time, after reaction, from
Ceramic pipe type film is taken out in stainless steel component, 3 ceramic pipe type films is cleaned with ethyl acetate, then in 110 DEG C of vacuum drying
Dry 24 h in case.
Specific implementation mode two:A kind of preparation of ceramic base polyvinyl acetate composite membrane described in specific implementation mode one
Method, in step 1, the ceramic pipe type film is alumina-supported zirconia ceramics tubular membrane.
Specific implementation mode three:A kind of preparation of ceramic base polyvinyl acetate composite membrane described in specific implementation mode one
Method, in step 2, the silane coupling agent is vinyltrimethoxysilane, functions as ceramic membrane and poly- acetic acid second
The bridge of enester forms covalent bond.
Specific implementation mode four:A kind of preparation of ceramic base polyvinyl acetate composite membrane described in specific implementation mode one
Method, in step 2, in the stainless steel membrane component, ceramic pipe type film internal diameter is 8mm, outer diameter 12.5mm, stainless steel tube
Intracavity diameter is 14mm, and stainless steel membrane component overall length is 60mm.
Specific implementation mode five:A kind of preparation of ceramic base polyvinyl acetate composite membrane described in specific implementation mode one
Method, in step 3, the polymer monomer is vinyl acetate, and the initiator is azobisisoheptonitrile.
Embodiment 1:
The alumina-supported zirconia ceramics tubular membrane of bore dia 0.1um is cleaned by ultrasonic in acetone, ethyl alcohol, water each successively
10min.Ceramic membrane after cleaning is immersed in 1% hydrochloric acid after 180min.Again by film immersion 10min in deionized water, take
Membrane is dried in vacuo 110 DEG C, for 24 hours.Before silanization, ceramic membrane submerges 30min, drying at room temperature 1h in deionized water, so
It is placed in the climatic chamber that humidity is 50%, balance is for 24 hours.Obtain the ceramic membrane of surface hydroxylation.The ceramics of surface hydroxylation
Film is placed in stainless steel component, first, the shell side of stainless steel membrane component is full of pure xylene solvent, sealing.Configure 10% second
The xylene solvent of alkenyl trimethoxy silane is placed in the 1L opening three-necked flask reactors of 75 DEG C of condensers of a connection.Instead
It answers device to heat up in oil bath pan and reaches 138 DEG C, circulated in the tube side of stainless steel membrane membrane module under the promotion of peristaltic pump,
Run time 5h.After reaction, ceramic membrane is taken out from stainless steel membrane component.3 ceramic membranes are cleaned with pure dimethylbenzene, are removed
Then unreacted silane molecule is dried for 24 hours in 140 DEG C of vacuum drying chamber.The ceramic membrane of silanization is placed in stainless steel group
In part, first, the shell side of stainless steel membrane component is full of pure ethyl acetate solvent, sealing.Configure 40% vinyl acetate monomer
Ethyl acetate solution is placed in the reaction vessel of nitrogen atmosphere, and 0.03mol/L azos two are added after being increased to 50 DEG C in reaction temperature
Different heptonitrile circulates under the promotion of peristaltic pump in the tube side of stainless steel membrane component, run time 6h.After reaction,
Ceramic membrane is taken out from stainless steel membrane component, 3 ceramic membranes are cleaned with ethyl acetate, then in 110 DEG C of vacuum drying chamber
Drying is for 24 hours.
Embodiment 2:
The alumina-supported zirconia ceramics tubular membrane of bore dia 0.1um is cleaned by ultrasonic in acetone, ethyl alcohol, water each successively
10min.Ceramic membrane after cleaning is immersed in 1% hydrochloric acid after 180min.Again by film immersion 10min in deionized water, take
Membrane is dried in vacuo 110 DEG C, for 24 hours.Before silanization, ceramic membrane submerges 30min, drying at room temperature 1h in deionized water, so
It is placed in the climatic chamber that humidity is 50%, balance is for 24 hours.Obtain the ceramic membrane of surface hydroxylation.The ceramics of surface hydroxylation
Film is placed in the component of stainless steel, first, the shell side of stainless steel membrane component is full of pure xylene solvent, sealing.Configuration 10%
The xylene solution of vinyltrimethoxysilane is placed in the 1L opening three-necked flask reactors of 75 DEG C of condensers of a connection.
Reactor heats up in oil bath pan reaches 138 DEG C, is circulated in the tube side of stainless steel membrane component under the promotion of peristaltic pump,
Run time 5h.After reaction, ceramic membrane is taken out from stainless steel membrane component.3 ceramic membranes are cleaned with pure dimethylbenzene, are removed
Then unreacted silane molecule is dried for 24 hours in 140 DEG C of vacuum drying chamber.The ceramic membrane of silanization is placed in stainless steel
In component, first, the shell side of stainless steel membrane component is full of pure ethyl acetate solvent, sealing.Configure 45% vinyl acetate monomer
Ethyl acetate solution be placed in the reaction vessel of nitrogen atmosphere, reaction temperature be increased to 60 DEG C after be added 0.03mol/L azos
Two different heptonitriles, circulate under the promotion of peristaltic pump in the tube side of stainless steel membrane component, run time 6h.Reaction terminates
Afterwards, ceramic membrane is taken out from stainless steel membrane component, ceramic membrane is cleaned multiple times with ethyl acetate.Then in 110 DEG C of vacuum drying
It is dried for 24 hours in case.
Embodiment 3:
The alumina-supported zirconia ceramics tubular membrane of bore dia 0.1um is cleaned by ultrasonic in acetone, ethyl alcohol, water each successively
10min.Ceramic membrane after cleaning is immersed in 1% hydrochloric acid after 180min.Again by film immersion 10min in deionized water, take
Membrane is dried in vacuo 110 DEG C, for 24 hours.Before silanization, ceramic membrane submerges 30min, drying at room temperature 1h in deionized water, so
It is placed in the climatic chamber that humidity is 50%, balance is for 24 hours.Obtain the ceramic membrane of surface hydroxylation.The ceramics of surface hydroxylation
Film is placed in the component of stainless steel, first, the shell side of stainless steel membrane component is full of pure xylene solvent, sealing.Configuration 10%
The xylene solution of vinyltrimethoxysilane is placed in the 1L opening three-necked flask reactors of 75 DEG C of condensers of a connection.
Reactor heats up in oil bath pan reaches 138 DEG C, is circulated in the tube side of stainless steel membrane component under the promotion of peristaltic pump,
Run time 5h.After reaction, ceramic membrane is taken out from stainless steel membrane component.3 ceramic membranes are cleaned with pure dimethylbenzene, are removed
Then unreacted silane molecule is dried for 24 hours in 140 DEG C of vacuum drying chamber.The ceramic membrane of silanization is placed in stainless steel
In component, first, the shell side of stainless steel membrane component is full of pure ethyl acetate solvent, sealing.Configure 40% vinyl acetate monomer
Ethyl acetate solution be placed in the reaction vessel of nitrogen atmosphere, reaction temperature be increased to 60 DEG C after be added 0.03mol/L azos
Two different heptonitriles, circulate under the promotion of peristaltic pump in the tube side of stainless steel membrane component, run time 5h.Reaction terminates
Afterwards, ceramic membrane is taken out from stainless steel component, 3 ceramic membranes is cleaned with ethyl acetate.Then in 110 DEG C of vacuum drying chamber
Drying is for 24 hours.
Claims (5)
1. a kind of preparation method of ceramic base polyvinyl acetate composite membrane, it is characterised in that:Steps are as follows for the method:
Step 1:Ceramic pipe type film surface hydroxylating pre-processes:Ceramic pipe type film is cleaned by ultrasonic 5 in acetone, ethyl alcohol, water successively
Alumina tube film after cleaning is impregnated 30 ~ 180min by ~ 30min, ultrasonic power 250w in the hydrochloric acid of 1wt.%, then
In deionized water impregnate 10 ~ 30min, take out film be dried in vacuo 24 h at a temperature of 110 DEG C, then by ceramic pipe type film go from
30min is submerged in sub- water, dries 1h at room temperature, is subsequently placed in the climatic chamber that humidity is 35 ~ 65%, is balanced at 20 ~ 28 DEG C
24 h obtain the ceramic pipe type film of surface hydroxylation;
Step 2:Ceramic pipe type film intimal surface silanization:The ceramic pipe type film that step 1 pre-processes is placed in stainless steel
In pipe, stainless steel membrane component is formed, ceramic pipe type film is arranged concentrically with stainless steel tube, and the shell side of stainless steel membrane component is full of pure two
Toluene, shell side sealing, configures the xylene solution of 5 ~ 15wt.% silane coupling agents, and places it in 1L opening three-necked flask reactions
In device, which is connected with 70 ~ 75 DEG C of condenser, and reaction solution is warming up to 138 DEG C in oil bath pan, in the promotion of peristaltic pump
Under circulated in the tube side of stainless steel membrane component, 2 ~ 7 h of run time takes from stainless steel membrane component after reaction
Go out ceramic pipe type film, 3 ceramic pipe type films are cleaned with pure dimethylbenzene, then dry 24 h in 140 DEG C of vacuum drying chamber;
Step 3:The ceramic pipe type film of vinyl acetate grafted silane:The ceramic pipe type film of step 2 silanization is placed in not
It becomes rusty in steel component, stainless steel membrane component shell side is full of pure ethyl acetate or water, and shell side sealing configures 5 ~ 50% polymer monomers
Ethyl acetate solution is placed in the reaction vessel of nitrogen atmosphere, and reaction temperature is added 0 ~ 0.05mol/L after being increased to 30 ~ 70 DEG C and draws
Agent is sent out, is circulated in the tube side of stainless steel membrane component under the promotion of peristaltic pump, 1 ~ 6 h of run time, after reaction,
Alumina tube film is taken out from stainless steel membrane component, and 3 ceramic pipe type films are cleaned with ethyl acetate, it is then true at 110 DEG C
Dry 24 h in empty drying box.
2. a kind of preparation method of ceramic base polyvinyl acetate composite membrane according to claim 1, it is characterised in that:Step
In rapid one, the ceramic pipe type film is alumina-supported zirconia ceramics tubular membrane.
3. a kind of preparation method of ceramic base polyvinyl acetate composite membrane according to claim 1, it is characterised in that:Step
In rapid two, the silane coupling agent is vinyltrimethoxysilane.
4. a kind of preparation method of ceramic base polyvinyl acetate composite membrane according to claim 1, it is characterised in that:Step
In rapid two, in the stainless steel membrane component, ceramic pipe type film internal diameter is 8mm, outer diameter 12.5mm, stainless steel tube intracavity diameter
For 14mm, stainless steel membrane component overall length is 60mm.
5. a kind of preparation method of ceramic base polyvinyl acetate composite membrane according to claim 1, it is characterised in that:Step
In rapid three, the polymer monomer is vinyl acetate, and the initiator is azobisisoheptonitrile.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN113173805A (en) * | 2021-04-30 | 2021-07-27 | 萍乡学院 | Method for constructing ceramic-based lotus leaf bionic hydrophobic micro-nano mastoid structure on glaze |
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2018
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