CN109351208A - A kind of preparation method of graphene oxide-NaY zeolite composite membrane - Google Patents
A kind of preparation method of graphene oxide-NaY zeolite composite membrane Download PDFInfo
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- CN109351208A CN109351208A CN201811299217.1A CN201811299217A CN109351208A CN 109351208 A CN109351208 A CN 109351208A CN 201811299217 A CN201811299217 A CN 201811299217A CN 109351208 A CN109351208 A CN 109351208A
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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
- B01D71/02—Inorganic material
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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
- B01D67/0039—Inorganic membrane manufacture
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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
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- B01D2325/36—Hydrophilic membranes
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Abstract
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, is related to zeolite technical field of membrane, includes the following steps, prepares NaY zeolite film；Prepare graphene oxide-NaY zeolite composite membrane, configure the aqueous dispersions of graphene oxide, graphene oxide is introduced in the NaY film surface of above-mentioned preparation, and by corona treatment and hot setting, then repeats this step and obtains graphene oxide-NaY zeolite composite membrane several times.The graphene oxide of preparation-NaY zeolite composite membrane includes applying below, can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；It can be used for 50wt.% acetic acid dehydration；It is expansible to be applied to organics dehydration.Graphene oxide-NaY zeolite composite membrane of this method preparation can effectively enhance the acid resistance of NaY zeolite film, while keep excellent hydrophily, solve the problems, such as that traditional NaY zeolite film acid resistance is poor；On the other hand, the graphene oxide on surface layer repairs NaY zeolite film film layer defect, is conducive to the separating property for improving film.
Description
Technical field
The present invention relates to zeolite technical field of membrane, the preparation side of specially a kind of graphene oxide-NaY zeolite composite membrane
Method.
Background technique
Zeolite membrane is normally used as on support being used to separate with zeolite film composite made of membranaceous formation zeolite,
Concentration, such as by contacting the mixture of organic compound and water with zeolite film composite, penetrate with making water selective, thus
It can separate, organic compound is concentrated, using the separation of zeolite membrane, concentration, with the separation phase carried out by distillation or adsorbent
Than in addition to the usage amount of energy can be cut down, due also to being inorganic material, therefore can be in temperature model more wider array of than polymeric membrane
Implementation separation, concentration are enclosed, and can be applicable to the separation of the mixture containing organic compound.But prepared by zeolite membrane
Or in application process, easily there is defect and membrane separating property is caused to decline in film layer, therefore the reparation of film layer defect seems especially heavy
It wants；Simultaneously NaY zeolite molecular sieve crystal acid resistance it is poor, the crystal structure dealuminzation under acidic environment and structure collapse occurs,
So NaY zeolite film is also difficult to directly apply in acidic environment.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides a kind of graphene oxide-NaY zeolite composite membrane preparation sides
Method solves the problems, such as that existing traditional NaY zeolite film acid resistance is poor, and the graphene oxide developed-NaY zeolite composite membrane can
The effectively acid resistance of enhancing NaY zeolite film, while keeping excellent hydrophily；On the other hand, the graphene oxide on surface layer is to NaY
Zeolite membrane film layer defect is repaired, and the separating property for improving film is conducive to.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs: a kind of graphene oxide-NaY zeolite
The preparation method of composite membrane, includes the following steps,
(1) NaY zeolite molecular sieve seed is dispersed in pure water, obtains NaY zeolite molecular sieve seed liquid；
(2) NaY crystalline substance is introduced on porous matrix material surface using NaY zeolite molecular sieve seed liquid obtained in step (1)
Kind layer；
(3) alkali source, silicon source and silicon source are dissolved in pure water and are arranged to Synthesis liquid, each component rubs in the Synthesis liquid
That ratio are as follows:
Silicon source: silicon source=5~50, alkali source: silicon source=5~50, water: silicon source=40~150；
(4) porous matrix material that the load for obtaining step (2) has NaY seed layer is placed in the synthesis that step (3) obtains
In liquid, synthesized by hydro-thermal static crystallization, crystallization temperature be 80~140 DEG C, crystallization time be 1~for 24 hours, crystallization terminates
Afterwards, NaY zeolite film pure water is taken out to neutrality, is placed in drying 6 at 50~100 DEG C~for 24 hours；
(5) graphene oxide is dispersed in pure water, obtains the aqueous dispersions of graphene oxide；
(6) drawn using the aqueous dispersions of graphene oxide obtained in step (5) in the NaY film surface that step (4) obtains
Enter graphene oxide layer；
(7) membrane tube for obtaining step (6) enhances the combination of graphene oxide and NaY zeolite film by corona treatment
Power；
(8) membrane tube that step (7) obtains is placed in vacuum at high temperatures solidification, solidification temperature is 200~600 DEG C, when solidification
Between be 2~8h；
(9) step (5)~(8) are repeated, number of repetition is 1~60 time.
In above-mentioned all technical solutions of the invention, NaY zeolite in NaY zeolite molecular sieve seed liquid described in step (1)
The content of molecular sieve is 0.05~10wt.%, preferably 0.05~2wt.%；Zeolite molecular sieve crystal granular size be 0.05~
4 μm, preferably 0.05~1.5 μm.
In above-mentioned all technical solutions of the invention, the shape of porous material substrates described in step (2) is plate, pipe
Shape, multichannel or doughnut, preferably plate or tubulose；The material of the porous material substrates is aluminium oxide, mullite, oxygen
Change zirconium, silica, titanium oxide or metal, preferably aluminium oxide；The aperture of the porous material substrates is 0.02~10 μm, preferably
It is 0.02~1 μm.
In above-mentioned all technical solutions of the invention, NaY seed layer is introduced on porous matrix material surface in step (2)
Method is infusion process, hot submersion method, vacuum crystal method, spray coating method, swabbing process or spin-coating method, preferably infusion process or hot submersion
Method.
In above-mentioned all technical solutions of the invention, the molar ratio of each component in Synthesis liquid described in step (3) are as follows:
Silicon source: silicon source=10~25, alkali source: silicon source=20~35, water: silicon source=60~100.
In above-mentioned all technical solutions of the invention, crystallization temperature described in step (4) be 90~130 DEG C, preferably 90
~110 DEG C, crystallization time is 1~20h, preferably 4~10h.
In above-mentioned all technical solutions of the invention, stone is aoxidized in the aqueous dispersions of graphene oxide described in step (5)
The content of black alkene is 0.001~0.5wt.%, preferably 0.01~0.1wt.%.
In above-mentioned all technical solutions of the invention, it is in the method that NaY film surface introduces graphene oxide in step (6)
Infusion process, hot submersion method, vacuum crystal method, spray coating method, swabbing process or spin-coating method, preferably infusion process or hot submersion method.
In above-mentioned all technical solutions of the invention, plasma described in step (7) is Ar, H2Or N2Plasma, it is excellent
It is selected as N2Plasma.
In above-mentioned all technical solutions of the invention, solidification temperature described in step (8) is 200~500 DEG C, preferably
200~400 DEG C；Curing time is 2~5h, preferably 2~4h.
In above-mentioned all technical solutions of the invention, number of repetition described in step (9) be 5~40 times, preferably 5~30
It is secondary.
In above-mentioned all technical solutions of the invention, including apply below:
(1) it can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；
(2) it can be used for 50wt.% acetic acid dehydration；
(3) expansible to be applied to organics dehydration or gas separation.
(3) beneficial effect
The present invention provides a kind of graphene oxide-NaY zeolite composite membrane preparation methods.Have it is following the utility model has the advantages that
(1) graphene oxide-NaY zeolite composite membrane preparation method, by advance on porous matrix material surface
NaY zeolite film is prepared, it is compound to introduce graphene oxide layer formation graphene oxide-NaY zeolite on NaY zeolite film surface layer later
Film can repair NaY zeolite film film layer defect, can effectively improve the separating property of film, on the other hand, can solve tradition
The problem of NaY zeolite film acid resistance difference, graphene oxide-NaY zeolite composite membrane can effectively enhance the acidproof of NaY zeolite film
Property, while keeping excellent hydrophily.
(2) graphene oxide-NaY zeolite composite membrane preparation method, the crystallization temperature during NaY zeolite film preparation
90~110 DEG C and 4~10h are respectively preferably with the time, can be improved NaY zeolite crystallinity, stray crystal content therein is reduced, mentions
The separating property of high zeolite membrane.
Specific embodiment
In order to be easy to understand the technical means, the creative features, the aims and the efficiencies achieved by the present invention, tie below
Specific embodiment is closed, the present invention is further explained.
Embodiment one
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, includes the following steps,
(1) NaY zeolite molecular sieve seed is dispersed in pure water, obtains NaY zeolite molecular sieve seed liquid, the NaY zeolite
The content of NaY zeolite molecular sieve is 0.1wt.% in molecular sieve seed liquid, and granular size is about 500nm；
(2) pass through infusion process on porous matrix material surface using NaY zeolite molecular sieve seed liquid obtained in step (1)
NaY seed layer is introduced, the porous matrix material is aluminium oxide tubulose matrix, and the aperture of matrix is 100nm；
(3) alkali source, silicon source and silicon source are dissolved in pure water and are arranged to Synthesis liquid, each component rubs in the Synthesis liquid
That ratio are as follows:
Silicon source: silicon source=12.8, alkali source: silicon source=34, water: silicon source=75；
(4) porous matrix material that the load for obtaining step (2) has NaY seed layer is placed in the synthesis that step (3) obtains
It in liquid, is synthesized by hydro-thermal static crystallization, crystallization temperature is 100 DEG C, crystallization time 7h, after crystallization, takes out NaY
Zeolite membrane pure water is placed at 80 DEG C and dries for 24 hours to neutrality；
(5) graphene oxide is dispersed in pure water, obtains the aqueous dispersions of graphene oxide, the water of the graphene oxide
The content of graphene oxide is 0.01wt.% in dispersion liquid；
(6) the NaY film surface benefit obtained using the aqueous dispersions of graphene oxide obtained in step (5) in step (4)
Graphene oxide layer is introduced with infusion process,；
(7) membrane tube that step (6) obtains is passed through into N2The knot of corona treatment enhancing graphene oxide and NaY zeolite film
With joint efforts；
(8) membrane tube that step (7) obtains is placed in vacuum at high temperatures solidification, solidification temperature is 250 DEG C, and curing time is
4h；
(9) step (5)~(8) are repeated 5 times.
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, including apply below
(1) it can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；
(2) it can be used for 50wt.% acetic acid dehydration；
(3) expansible to be applied to organics dehydration or gas separation.
Embodiment two
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, includes the following steps,
(1) NaY zeolite molecular sieve seed is dispersed in pure water, obtains NaY zeolite molecular sieve seed liquid, the NaY zeolite
The content of NaY zeolite molecular sieve is 0.1wt.% in molecular sieve seed liquid, and granular size is about 500nm；
(2) pass through infusion process on porous matrix material surface using NaY zeolite molecular sieve seed liquid obtained in step (1)
NaY seed layer is introduced, the porous matrix material is aluminium oxide tubulose matrix, and the aperture of matrix is 100nm；
(3) alkali source, silicon source and silicon source are dissolved in pure water and are arranged to Synthesis liquid, each component rubs in the Synthesis liquid
That ratio are as follows:
Silicon source: silicon source=12.8, alkali source: silicon source=34, water: silicon source=75；
(4) porous matrix material that the load for obtaining step (2) has NaY seed layer is placed in the synthesis that step (3) obtains
It in liquid, is synthesized by hydro-thermal static crystallization, crystallization temperature is 100 DEG C, crystallization time 6h, after crystallization, takes out NaY
Zeolite membrane pure water is placed at 80 DEG C and dries for 24 hours to neutrality；
(5) graphene oxide is dispersed in pure water, obtains the aqueous dispersions of graphene oxide, the water of the graphene oxide
The content of graphene oxide is 0.02wt.% in dispersion liquid；
(6) the NaY film surface benefit obtained using the aqueous dispersions of graphene oxide obtained in step (5) in step (4)
Graphene oxide layer is introduced with infusion process,；
(7) membrane tube that step (6) obtains is passed through into N2The knot of corona treatment enhancing graphene oxide and NaY zeolite film
With joint efforts；
(8) membrane tube that step (7) obtains is placed in vacuum at high temperatures solidification, solidification temperature is 300 DEG C, and curing time is
4h；
(9) step (5)~(8) are repeated 15 times.
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, including apply below
(1) it can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；
(2) it can be used for 50wt.% acetic acid dehydration；
(3) expansible to be applied to organics dehydration or gas separation.
Embodiment three
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, includes the following steps,
(1) NaY zeolite molecular sieve seed is dispersed in pure water, obtains NaY zeolite molecular sieve seed liquid, the NaY zeolite
The content of NaY zeolite molecular sieve is 0.1wt.% in molecular sieve seed liquid, and granular size is about 500nm；
(2) pass through infusion process on porous matrix material surface using NaY zeolite molecular sieve seed liquid obtained in step (1)
NaY seed layer is introduced, the porous matrix material is aluminium oxide tubulose matrix, and the aperture of matrix is 100nm；
(3) alkali source, silicon source and silicon source are dissolved in pure water and are arranged to Synthesis liquid, each component rubs in the Synthesis liquid
That ratio are as follows:
Silicon source: silicon source=12.8, alkali source: silicon source=34, water: silicon source=75；
(4) porous matrix material that the load for obtaining step (2) has NaY seed layer is placed in the synthesis that step (3) obtains
It in liquid, is synthesized by hydro-thermal static crystallization, crystallization temperature is 100 DEG C, crystallization time 5h, after crystallization, takes out NaY
Zeolite membrane pure water is placed at 80 DEG C and dries for 24 hours to neutrality；
(5) graphene oxide is dispersed in pure water, obtains the aqueous dispersions of graphene oxide, the water of the graphene oxide
The content of graphene oxide is 0.03wt.% in dispersion liquid；
(6) the NaY film surface benefit obtained using the aqueous dispersions of graphene oxide obtained in step (5) in step (4)
Graphene oxide layer is introduced with infusion process,；
(7) membrane tube that step (6) obtains is passed through into N2The knot of corona treatment enhancing graphene oxide and NaY zeolite film
With joint efforts；
(8) membrane tube that step (7) obtains is placed in vacuum at high temperatures solidification, solidification temperature is 200 DEG C, and curing time is
4h；
(9) step (5)~(8) are repeated 30 times.
A kind of preparation method of graphene oxide-NaY zeolite composite membrane, including apply below
(1) it can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；
(2) it can be used for 50wt.% acetic acid dehydration；
(3) expansible to be applied to organics dehydration or gas separation.
The embodiment of the present invention and the common zeolite membrane table of comparisons
| Common NaY zeolite film | Embodiment one | Embodiment two | Embodiment three | |
| Zeolite crystallinity | 90% | 95% | 98% | 96% |
| Stray crystal | Have | Nothing | Nothing | Nothing |
| Obvious shortcoming | Have | Nothing | Nothing | Nothing |
| Separating property | Generally | Well | It is excellent | Well |
| Acid resistance | Difference | Well | It is excellent | It is excellent |
From above table as can be seen that compared with zeolite membrane commonly in the market, the present invention has apparent zeolite knot
The characteristics of brilliant degree is high, is free of stray crystal, while zeolite membrane film layer no significant defect, film layer acid resistance are effectively improved and are mentioned
Height avoids the problem of existing NaY zeolite membrane separating property and acid resistance difference.
The above shows and describes the basic principles and main features of the present invention and the advantages of the present invention.The technology of the industry
Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and the above embodiments and description only describe this
The principle of invention, without departing from the spirit and scope of the present invention, various changes and improvements may be made to the invention, these changes
Change and improvement all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and its
Equivalent thereof.
Claims (12)
1. a kind of graphene oxide-NaY zeolite composite membrane preparation method, which comprises the following steps:
(1) NaY zeolite molecular sieve seed is dispersed in pure water, obtains NaY zeolite molecular sieve seed liquid；
(2) NaY seed layer is introduced on porous matrix material surface using NaY zeolite molecular sieve seed liquid obtained in step (1)；
(3) alkali source, silicon source and silicon source are dissolved in pure water and are arranged to Synthesis liquid, the molar ratio of each component in the Synthesis liquid
Are as follows:
Silicon source: silicon source=5~50, alkali source: silicon source=5~50, water: silicon source=40~150；
(4) porous matrix material that the load for obtaining step (2) has NaY seed layer is placed in the Synthesis liquid that step (3) obtains,
Synthesized by hydro-thermal static crystallization, crystallization temperature be 80~140 DEG C, crystallization time be 1~for 24 hours, after crystallization, take out
NaY zeolite film pure water is placed in drying 6 at 50~100 DEG C~for 24 hours to neutrality；
(5) graphene oxide is dispersed in pure water, obtains the aqueous dispersions of graphene oxide；
(6) oxygen is introduced in the NaY film surface that step (4) obtains using the aqueous dispersions of graphene oxide obtained in step (5)
Graphite alkene layer；
(7) membrane tube for obtaining step (6) enhances the binding force of graphene oxide and NaY zeolite film by corona treatment.
(8) membrane tube that step (7) obtains is placed under vacuum and carries out hot setting, solidification temperature is 200~600 DEG C, when solidification
Between be 2~8h；
(9) step (5)~(8) are repeated, number of repetition is 1~60 time.
2. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly the content of NaY zeolite molecular sieve is 0.05~10wt.%, NaY zeolite point in NaY zeolite molecular sieve seed liquid described in (1)
Son sieve crystal grain size is 0.05~4 μm.
3. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly the shape of porous material substrates described in (2) is plate, tubulose, multichannel or doughnut；The porous material substrates
Material is aluminium oxide, mullite, zirconium oxide, silica, titanium oxide or metal；The aperture of the porous material substrates be 0.02~
10μm。
4. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
It suddenly is infusion process, hot submersion method, vacuum crystal method, spraying in the method that porous matrix material surface introduces NaY seed layer in (2)
Method, swabbing process or spin-coating method.
5. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly in Synthesis liquid described in (3) each component molar ratio are as follows:
Silicon source: silicon source=10~30, alkali source: silicon source=10~40, water: silicon source=60~120.
6. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly crystallization temperature described in (4) is 90~130 DEG C, and crystallization time is 1~20h.
7. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly the content of graphene oxide is 0.001~0.5wt.% in the aqueous dispersions of graphene oxide described in (5).
8. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
It suddenly is infusion process, hot submersion method, vacuum crystal method, spray coating method, wiping in the method that NaY film surface introduces graphene oxide in (6)
Coating or spin-coating method.
9. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that step
Suddenly plasma described in (7) is Ar, H2Or N2Plasma.
10. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that
Solidification temperature described in step (8) is 200~500 DEG C, and curing time is 2~5h.
11. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that
Number of repetition described in step (9) is 5~40 times.
12. a kind of preparation method of graphene oxide-NaY zeolite composite membrane according to claim 1, which is characterized in that
Including applying below:
(1) it can be used for the alcohols dehydrations such as ethanol dehydration, isopropanol dehydration；
(2) it can be used for 50wt.% acetic acid dehydration；
(3) expansible to be applied to organics dehydration or gas separation.
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| CN112999890A (en) * | 2021-03-03 | 2021-06-22 | 大连理工大学 | Organic-inorganic hybrid SiO of flat plate2Composite membrane and preparation method and application thereof |
| CN113144922A (en) * | 2021-03-31 | 2021-07-23 | 大连理工大学 | Coaxial cable type graphene oxide-zeolite molecular sieve @ hollow fiber composite membrane and preparation method thereof |
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| CN112479304A (en) * | 2020-06-11 | 2021-03-12 | 中科远方(北京)科技有限公司 | Porous material with functional graphene oxide film on surface, and preparation method and application thereof |
| CN112999890A (en) * | 2021-03-03 | 2021-06-22 | 大连理工大学 | Organic-inorganic hybrid SiO of flat plate2Composite membrane and preparation method and application thereof |
| CN112999890B (en) * | 2021-03-03 | 2022-04-19 | 大连理工大学 | Organic-inorganic hybrid SiO of flat plate2Composite membrane and preparation method and application thereof |
| CN113144922A (en) * | 2021-03-31 | 2021-07-23 | 大连理工大学 | Coaxial cable type graphene oxide-zeolite molecular sieve @ hollow fiber composite membrane and preparation method thereof |
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Application publication date: 20190219 |