CN108380059A - A kind of method that microwave secondary growth method prepares MFI molecular screen membranes - Google Patents
A kind of method that microwave secondary growth method prepares MFI molecular screen membranes Download PDFInfo
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- CN108380059A CN108380059A CN201810161344.9A CN201810161344A CN108380059A CN 108380059 A CN108380059 A CN 108380059A CN 201810161344 A CN201810161344 A CN 201810161344A CN 108380059 A CN108380059 A CN 108380059A
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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
- B01D67/0051—Inorganic membrane manufacture by controlled crystallisation, e,.g. hydrothermal growth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- B01D71/028—Molecular sieves
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Abstract
The present invention relates to a kind of methods that microwave secondary growth method prepares MFI molecular screen membranes, conventional hydrothermal growth is carried out using first placing carrier seed layer upwardly, effectively avoid falling off for crystal seed, it can avoid the deposition of film surface again, enhance the active force between carrier and crystal seed, then the molecular screen membrane carrier crystal seed after the short time being reacted is placed downwards continues microwave hydrothermal diauxic growth, and downwards due to crystal seed, being deposited caused by eliminating microwave moment nucleation influences.Molecular screen membrane preparation time prepared by the present invention greatly shortens, at low cost, and building-up process repeatability is high, is suitable for industry amplification.
Description
Technical field
The present invention relates to the preparing technical fields of organic zeolite membrane, and in particular to a kind of microwave secondary growth method preparation
The method of MFI molecular screen membranes.
Background technology
Zeolite molecular sieve film is the continuous and uniform inoranic membrane for forming zeolite molecular sieve symbiosis, as porous, inorganic
One kind of film, because it is with various topological structures, unique pore canal system, orderly regular pore passage structure, suitable aperture point
Cloth and close pore passage structure is thought with molecular dimension, it can be achieved that being selected the molecule of different dynamic radius on molecular scale
Selecting property detaches, and can fully improve its differential permeability.Wherein, support membrane is that molecular sieve is grown on certain mechanical strength
On carrier, and continuous, fine and close molecular sieve film layer is formed in carrier surface, there is stronger mechanical strength, adapt to application range
More extensively.Due to the feature in zeolite molecules sieve structure and performance, in host-guest chemistry, chromatography, life science, electrode, sensing
The fields such as device, optical material, electricity material have a good application prospect.People have synthesized 20 different kinds of molecules sieve membranes at present,
Such as MFI, LTA, FAU, BEA, CHA, FER, MOR, MCM-41.Wherein, the aperture size of MFI molecular screen membranes and many important works
The molecular dimension of industry chemicals is suitable, and with complicated 3 D pore canal system, b axis be orientated the straight hole road of 0.53 × 0.56nm with
The sinusoidal duct that a axis is orientated 0.51 × 0.55nm intersects, and b axis is orientated straight hole road of the MFI-type molecular screen membrane because of its molecular sieve
It is vertical with supporting body surface and have wider application prospect.
The synthetic method of molecular screen membrane mainly has gas phase synthesis method, Vacuum-assisted method method, secondary growth method (crystal seed method)
Deng.Gas phase synthesis method is during synthesizing molecular sieve film, it is difficult to ensure that the complete conversion of its gel, and may give birth to simultaneously
At several molecular sieves, it is unfavorable for the stabilization of molecular screen membrane.Due to nucleation in situ and carrier surface nature and Synthesis liquid it is microcosmic
Environment has much relations, therefore the molecular screen membrane of Situ Hydrothermal method synthesis is less reproducible, additionally due in building-up process not first
Crystal seed is generated, easily occurs to turn crystalline substance.Secondary growth method (crystal seed method) is the most popular method of current synthesizing molecular sieve film, can be nucleation
Process and crystal growing process separate, and inhibit nucleus to be transformed into other crystal, improve the purity of molecular screen membrane.But conventional hydrothermal
MFI molecular screen membrane synthetic methods, growth film formation time it is longer, need ten a few houres even tens hours, working efficiency is low.
Generated time can significantly be shortened using microwave method hydrothermal synthesis MFI molecular screen membranes, and will be foreshortened to the film time several
Within hour, and it is at low cost, and production efficiency is high.But under microwave condition, the particle meeting instantaneous burst nucleation in Synthesis liquid,
A large amount of nucleus of different sizes or crystal predecessor are generated, can cause to deposit in carrier seed surface, to influence MFI molecular sieves
It is crosslinked in the face of film, causes film discontinuous, building-up process repeatability is low.
Since the active force between carrier and film is weaker, under microwave condition, rapid a large amount of nucleation, deposition velocity in the short time
Much larger than crosslinking rate, even if using different carrier modes of emplacement, it will also result in the deposition of film surface or fall off, to lead
It causes film surface uneven, and easy tos produce defect.Therefore, there is an urgent need for a kind of new synthetic methods to be used to prepare building-up process repeatability
High, the continuous MFI-type molecular screen membrane of film.
Invention content
For current defect, the present invention provides a kind of methods that microwave secondary growth method prepares MFI molecular screen membranes, can
Low, the discontinuous problem of film with effective solution microwave hydrothermal growth method preparation MFI molecular screen membrane repeatability, when shortening film
Between, it is suitable for industry amplification.
The present invention is adopted the technical scheme that solve technical problem present in known technology：
To achieve the above object, the present invention proposes the method that improved microwave secondary growth method prepares MFI molecular screen membranes.It is first
First carrier seed layer is placed upwardly and carries out conventional hydrothermal growth, enhances the active force between carrier and crystal seed, using dilute
Growth-promoting media, since growth-promoting media concentration is dilute, the reaction time is short, nucleation influences to ignore less, caused by deposition in the short time.Then
Molecular screen membrane taking-up after short time is reacted is put into the microwave reaction kettle for filling growth-promoting media, and carrier seed layer is towards decentralization
It sets, continued growth, downwards due to carrier crystal seed, being deposited caused by eliminating microwave moment nucleation influences.It is as follows：
1) the MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry,
It will be placed in reaction kettle in carrier crystal seed level horizontal direction again, then growth-promoting media poured into along kettle wall, growth-promoting media submerges carrier, institute
The mol ratio for stating growth-promoting media is TPAOH：TEOS：H2O=0.2：1：(500-1200) seals hydrothermal growth after reaction kettle,
It is taken out after reacting 120-240min at 140-200 DEG C；
2) molecular screen membrane made from step 1) is cleaned with deionized water, after drying, it will be under carrier crystal seed level horizontal direction
It is put into the microwave reaction kettle for filling growth-promoting media, growth-promoting media submerges carrier, and the mol ratio of the growth-promoting media is TPAOH：
TEOS：H2O=0.2：1：(200-350) seals microwave hydrothermal diauxic growth after reaction kettle, reacts 90- at 140-170 DEG C
120min, is cooled to room temperature after taking-up, and diaphragm is cleaned with deionized water, obtains continuous MFI molecular screen membranes.
Preferably, in step 1), the mol ratio of the growth-promoting media is TPAOH：TEOS：H2O=0.2：1：(800-
1000)。
Preferably, in step 1), the synthesis condition of hydrothermal growth is to react 180min at 150-170 DEG C.
Preferably, in step 2), the mol ratio of the growth-promoting media is TPAOH：TEOS：H2O=0.2：1：(240-
300)。
Preferably, in step 2), the synthesis condition of microwave heating diauxic growth is to react 100- at 150-160 DEG C
110min。
Compared with prior art, the invention has the advantages and positive effects that：
The present invention under the conditions of conventional hydrothermal, makes carrier seed layer place the short period upward first, carries out the water of crystal seed
Thermally grown, relatively slow due to being nucleated under hydrothermal condition, deposition velocity is matched with crosslinking rate, you can falling off for crystal seed effectively is avoided,
The deposition that can avoid film surface again, enhances the binding force between carrier and crystal seed, eliminates gravity sedimentation in preparation process
It influences, then uses microwave-hydrothermal method, carrier seed layer is made to place downwards, carry out diauxic growth and synthesize MFI molecular screen membranes, system
Standby molecular screen membrane preparation time greatly shortens, at low cost, and building-up process repeatability is high, is suitable for industry amplification；It solves existing
The technology of preparing consuming time is long, and microwave technology surface deposition leads to repeated low, the discontinuous problem of film of film；From scanning electron
The MFI-type molecular screen membrane even compact that microscope figure can see synthesis is continuous.
Description of the drawings
Fig. 1 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that embodiment 1 synthesizes；
Fig. 2 is scanning electron microscope (SEM) figure for the molecular screen membrane section that embodiment 1 synthesizes；
Fig. 3 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that embodiment 2 synthesizes；
Fig. 4 is scanning electron microscope (SEM) figure for the molecular screen membrane section that embodiment 2 synthesizes；
Fig. 5 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that embodiment 3 synthesizes；
Fig. 6 is scanning electron microscope (SEM) figure for the molecular screen membrane section that embodiment 3 synthesizes；
Fig. 7 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that embodiment 4 synthesizes；
Fig. 8 is scanning electron microscope (SEM) figure for the molecular screen membrane section that embodiment 4 synthesizes；
Fig. 9 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that comparative example 1 synthesizes；
Figure 10 is scanning electron microscope (SEM) figure for the molecular screen membrane section that comparative example 1 synthesizes；
Figure 11 is scanning electron microscope (SEM) figure on the molecular screen membrane surface that comparative example 2 synthesizes；
Figure 12 is scanning electron microscope (SEM) figure for the molecular screen membrane section that comparative example 2 synthesizes.
Specific implementation mode
In order to further understand the content, features and effects of the present invention, the following examples are hereby given, and coordinate attached drawing
Detailed description are as follows：
Embodiment 1
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:1200H2O is slowly added into reaction kettle (volume of experiment reaction kettle used is 50ml), sealing along crystallizing kettle wall
Reaction kettle.Reaction kettle is put into crystallization in the baking oven of preheating, takes out, is cooled to room temperature after 150 DEG C of reaction 2h, sample deionized water
It cleans, is dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:350H2O is placed under the horizontal direction of carrier crystal seed face, and 140 DEG C of reaction 120min are cooled to room temperature after taking-up, use deionization
Water cleans, and obtains continuous MFI molecular screen membranes.Fig. 1 and Fig. 2 is respectively surface and the section SEM figures of synthesized film.From figure
As can be seen that molecular screen membrane is continuous, film thickness is about 9 μm.
Embodiment 2
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:1000H2O is slowly added into reaction kettle (volume of experiment reaction kettle used is 50ml) along crystallizing kettle wall, and sealing is anti-
Answer kettle.Reaction kettle is put into crystallization in the baking oven of preheating, takes out, is cooled to room temperature, sample is washed with deionized water after 160 DEG C of reaction 2h
Only, dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:300H2O is placed under the horizontal direction of carrier crystal seed face, and 170 DEG C of reaction 90min are cooled to room temperature after taking-up, use deionization
Water cleans, and obtains continuous MFI molecular screen membranes.Fig. 3 and Fig. 4 is respectively surface and the section SEM figures of synthesized film.From figure
As can be seen that molecular screen membrane is continuous, film thickness is about 7 μm.
Embodiment 3
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:800H2O is slowly added into reaction kettle (volume of experiment reaction kettle used is 50ml) along crystallizing kettle wall, and sealing is anti-
Answer kettle.Reaction kettle is put into crystallization in the baking oven of preheating.It takes out, is cooled to room temperature, sample is washed with deionized water after 170 DEG C of reaction 3h
Only, dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:240H2O is placed under the horizontal direction of carrier crystal seed face, 160 DEG C of reaction 100min.It is cooled to room temperature after taking-up, uses deionization
Water cleans, and obtains continuous MFI molecular screen membranes.Fig. 5 and Fig. 6 is respectively surface and the section SEM figures of synthesized film.From figure
As can be seen that molecular screen membrane is continuous, film thickness is about 8 μm.
Embodiment 4
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:500H2O is slowly added into reaction kettle (volume of experiment reaction kettle used, be 50ml) along crystallizing kettle wall, and sealing is anti-
Answer kettle.Reaction kettle is put into crystallization in the baking oven of preheating.It takes out, is cooled to room temperature, sample is washed with deionized water after 190 DEG C of reaction 3h
Only, dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:200H2O is placed under the horizontal direction of carrier crystal seed face, 150 DEG C of reaction 110min.It is cooled to room temperature after taking-up, uses deionization
Water cleans, and obtains continuous MFI molecular screen membranes.Fig. 7 and Fig. 8 is respectively surface and the section SEM figures of synthesized film.From figure
As can be seen that molecular screen membrane is continuous, film thickness is about 8 μm.
Comparative example 1
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:1000H2O is slowly added into reaction kettle (volume of experiment reaction kettle used is 50ml) along crystallizing kettle wall, and sealing is anti-
Answer kettle.Reaction kettle is put into crystallization in the baking oven of preheating, takes out, is cooled to room temperature, sample is washed with deionized water after 160 DEG C of reaction 2h
Only, dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:300H2O is placed in carrier crystal seed face or horizontal direction, and 150 DEG C of reaction 90min are cooled to room temperature after taking-up, spend
Ionized water cleans, and obtains molecular screen membrane.Fig. 9 and Figure 10 is respectively surface and the section SEM figures of synthesized film.It is generated in Synthesis liquid
Useful constituent and useless component deposit to film surface under gravity condition, it can be seen from the figure that film surface is uneven, defect
It is more.
Comparative example 2
The MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then
It will be inserted into tetrafluoro bearing after the carrier side tetrafluoro adhesive tape for not supporting seed layer and the sealing of tetrafluoro supporter, is placed in crystallizing kettle kettle
Bottom is placed in carrier crystal seed level horizontal direction.The clear growth-promoting medias of 30ml, growth-promoting media molar ratio group is taken to become 0.2TPAOH:
1TEOS:800H2O is slowly added into reaction kettle (volume of experiment reaction kettle used is 50ml) along crystallizing kettle wall, and sealing is anti-
Answer kettle.Reaction kettle is put into crystallization in the baking oven of preheating.It takes out, is cooled to room temperature, sample is washed with deionized water after 170 DEG C of reaction 3h
Only, dry.It is then placed in the microwave reaction kettle of 50ml, growth-promoting media 30ml, growth-promoting media molar ratio group becomes 0.2TPAOH:
1TEOS:240H2O, carrier crystal seed face are placed vertically, 160 DEG C of reaction 100min.It is cooled to room temperature after taking-up, it is clear with deionized water
It washes, obtains MFI molecular screen membranes.Figure 11 and Figure 12 is respectively surface and the section SEM figures of synthesized film.It can be seen from the figure that
Still there is deposition on molecular screen membrane surface, and film surface is uneven, and defect is more.
The above is only the preferred embodiments of the present invention, and is not intended to limit the present invention in any form,
Every any simple modification made to the above embodiment according to the technical essence of the invention, equivalent variations and modification, belong to
In the range of technical solution of the present invention.
Claims (5)
1. a kind of method that microwave secondary growth method prepares MFI molecular screen membranes, which is characterized in that be as follows：
1) the MFI molecular sieve seed solution that mass fraction is 3% is first spun to carrier surface and prepares seed layer, it is dry, then will
It is placed in reaction kettle in carrier crystal seed level horizontal direction, then growth-promoting media is poured into along kettle wall, growth-promoting media submerges carrier, the life
The mol ratio of long liquid is TPAOH：TEOS：H2O=0.2：1：(500-1200) seals hydrothermal growth after reaction kettle, in 140-
It is taken out after reacting 120-240min at 200 DEG C；
2) molecular screen membrane made from step 1) is cleaned, after drying with deionized water, will be placed under carrier crystal seed level horizontal direction
It is put into the microwave reaction kettle for filling growth-promoting media, growth-promoting media submerges carrier, and the mol ratio of the growth-promoting media is TPAOH：TEOS：
H2O=0.2：1：(200-350) seals microwave hydrothermal diauxic growth after reaction kettle, reacts 90-120min at 140-170 DEG C,
It is cooled to room temperature after taking-up, diaphragm is cleaned with deionized water, obtain continuous MFI molecular screen membranes.
2. the method that a kind of microwave secondary growth method according to claim 1 prepares MFI molecular screen membranes, which is characterized in that
In the step 1), the mol ratio of the growth-promoting media is TPAOH：TEOS：H2O=0.2：1：(800-1000).
3. the method that a kind of microwave secondary growth method according to claim 1 prepares MFI molecular screen membranes, which is characterized in that
In the step 1), the synthesis condition of hydrothermal growth is to react 180min at 150-170 DEG C.
4. the method that a kind of microwave secondary growth method according to claim 1 prepares MFI molecular screen membranes, which is characterized in that
In the step 2), the mol ratio of the growth-promoting media is TPAOH：TEOS：H2O=0.2：1：(240-300).
5. the method that a kind of microwave secondary growth method according to claim 1 prepares MFI molecular screen membranes, which is characterized in that
In the step 2), the synthesis condition of microwave heating diauxic growth is to react 100-110min at 150-160 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109569316A (en) * | 2018-12-05 | 2019-04-05 | 广西大学 | A kind of preparation method of Silicalite-1 molecular screen membrane |
| CN112408411A (en) * | 2020-11-25 | 2021-02-26 | 上海绿强新材料有限公司 | Method for synthesizing SAPO-34 molecular sieve membrane based on microwave heating |
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| CN101774607A (en) * | 2009-12-31 | 2010-07-14 | 太原理工大学 | Method for preparing oriented molecular sieve membrane by using diauxic growth method |
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2018
- 2018-02-27 CN CN201810161344.9A patent/CN108380059A/en active Pending
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| CN101774607A (en) * | 2009-12-31 | 2010-07-14 | 太原理工大学 | Method for preparing oriented molecular sieve membrane by using diauxic growth method |
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| XIAOFEI LU ET AL.: "A facile fabrication of highly b-oriented MFI zeolite films in the TEOS-TPAOH-H2O system without additives", 《MICROPOROUS AND MESOPOROUS MATERIALS》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109569316A (en) * | 2018-12-05 | 2019-04-05 | 广西大学 | A kind of preparation method of Silicalite-1 molecular screen membrane |
| CN112408411A (en) * | 2020-11-25 | 2021-02-26 | 上海绿强新材料有限公司 | Method for synthesizing SAPO-34 molecular sieve membrane based on microwave heating |
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Application publication date: 20180810 |