CN106542537A - In the method for omnipotent gel synthesizing high-silicon zeolite molecular sieve - Google Patents
In the method for omnipotent gel synthesizing high-silicon zeolite molecular sieve Download PDFInfo
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- CN106542537A CN106542537A CN201610938025.5A CN201610938025A CN106542537A CN 106542537 A CN106542537 A CN 106542537A CN 201610938025 A CN201610938025 A CN 201610938025A CN 106542537 A CN106542537 A CN 106542537A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/36—Pentasil type, e.g. types ZSM-5, ZSM-8 or ZSM-11
- C01B39/38—Type ZSM-5
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/42—Type ZSM-12
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/44—Ferrierite type, e.g. types ZSM-21, ZSM-35 or ZSM-38
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
Abstract
The present invention relates to molecular sieve preparation method, it is desirable to provide a kind of method with omnipotent gel synthesizing high-silicon zeolite molecular sieve.Including step：After deionized water is mixed homogeneously with silicon source, NaOH is added thereto to, adds silicon source under agitation, persistently stir and silica-alumina gel is formed until solution；Zeolite molecular sieve crystal seed is added in silica-alumina gel, is placed in after stirring in reactor, the product sucking filtration of crystallization, drying obtain the former powder of silica-rich zeolite molecular sieve.Product obtained by the present invention not only maintains good degree of crystallinity and purity, with good catalytic reaction activity.Whole production process does not only use organic formwork agent, can greatly shorten crystallization time by crystal seed synthetic method, which reduces loss unnecessary in process of production.The inorganic raw material for being adopted is environmentally friendly, and price is less expensive, thus the present invention has unusual significance to the basic research of zeolite molecular sieve and in actual chemical production field.
Description
Technical field
The invention belongs to molecular sieve preparation method, more particularly to a kind of to synthesize serial silica-rich zeolite molecular sieve with omnipotent gel
Method.
Background technology
Zeolite molecular sieve has the structure and big surface area of spaciousness because of which, thus is widely used in catalysis, ion and hands over
The field such as change, adsorb and separate.Initial zeolite (A, X, Y) synthesis is carried out all under the conditions of organic-free template.With
Organic formwork agent is incorporated in the synthesis of zeolite molecular sieve, and this causes the species of zeolite molecular sieve to become rich and varied.But this
The use of a little organic formwork agents has the shortcomings that many：Synthesis high cost, toxicity are big, waste liquid and waste gas discharge are serious.In the last few years,
In view of organic formwork agent using the shortcoming brought, organic-free template synthesis is suggested again.Wherein, crystal seed method synthesis
It is a kind of brand-new synthetic method being recently proposed.It is original to add crystal seed toward synthetic system primarily to increasing crystallization speed
Rate, suppresses dephasign and control crystalline size, and now only needs and avoid making for organic formwork agent by addition crystal seed toward system
With this is in my innocent life.However, the mechanism of the effect of crystal seed and whole crystallization process is not also managed completely among these
Solution.
Recently, in without the synthesis of organic formwork crystal seed method, Okubo et al. proposes a hypothesis, i.e. Synthesis liquid presoma
There is certain identical secondary structure unit (mor, cas, mtw etc.) crystallization of zeolite is able to both zeolite seed crystals
Carry out, then by example enriching this hypothesis, such as Beta and ZSM-12 have identical secondary structure unit mtw,
Can also carry out as Beta zeolites can synthesize so ZSM-12 zeolites using Laue method.However, they are not from most basic
Construction unit (four-membered ring, five-membered ring, hexatomic ring) go out the synthesis for sending zeolite molecular sieve of discussing.
The content of the invention
The technical problem to be solved in the present invention is to overcome deficiency of the prior art, there is provided a kind of to be synthesized with omnipotent gel
The method of silica-rich zeolite molecular sieve.
To solve technical problem, the solution of the present invention is：
A kind of method with omnipotent gel synthesizing high-silicon zeolite molecular sieve is provided, is comprised the steps：
After deionized water is mixed homogeneously with silicon source, NaOH is added thereto to, adds silicon source under agitation, persistently stir straight
Silica-alumina gel is formed to solution；The zeolite molecular sieve crystal seed for accounting for silicon source quality 10% is added in silica-alumina gel, is placed in after stirring
In reactor, in 160 DEG C of 8～24h of crystallization；；Product sucking filtration, drying, that is, obtain the former powder of silica-rich zeolite molecular sieve；
The addition for controlling each reaction raw materials makes its molar ratio range for SiO2∶0.0083Al2O3∶0.28Na2O∶35H2O；
The zeolite molecular sieve crystal seed be it is following any one：ZSM-5、MOR、ZSM-12、ZSM-22、ZSM-23、ZSM-
35th, EU-1 or ZSM-22/ZSM-23 coexisting phases.
In the present invention, source of aluminium is aluminum sulfate, and silicon source is the Ludox of dioxide-containing silica 30.5%, and alkali source is hydrogen-oxygen
Change sodium.
Inventive principle is described：
In the present invention, as long as different zeolite seed crystals are put under identical crystallization temperature, can just obtain different types of
Molecular sieve.Its principle is, the presence of most basic construction unit (four-membered ring, five-membered ring, hexatomic ring) in omnipotent aqueous precursor gel
So that zeolite molecular sieve crystallization.Based on this reason, crystal seed method synthesis greatly reduces the zeolite crystallization time, reduces cost.
Compared with prior art, the beneficial effects of the present invention is：
1st, compared with prior art, the product obtained by the present invention not only maintains good degree of crystallinity and purity, has
Good catalytic reaction activity.Whole production process does not only use organic formwork agent, can be very big by crystal seed synthetic method
Shorten crystallization time, which reduces loss unnecessary in process of production.
2nd, inorganic raw material of the present invention is environmentally friendly, and price is less expensive, thus the present invention is to zeolite molecules
The basic research of sieve and all there is unusual significance in actual chemical production field.
Description of the drawings
Fig. 1：The XRD spectra of products obtained therefrom after omnipotent presoma crystallization.
Fig. 2：The XRD spectra of crystal seed method synthetic ZSM-5 zeolite..
Fig. 3：Crystal seed method synthesizes the XRD spectra of MOR zeolites.
Fig. 4：Crystal seed method synthesizes the XRD spectra of ZSM-12 zeolites.
Fig. 5：Crystal seed method synthesizes the XRD spectra of ZSM-22 zeolites..
Fig. 6：Crystal seed method synthesizes the XRD spectra of ZSM-23 zeolites.
Fig. 7：Crystal seed method synthesizes the XRD spectra of ZSM-22/ZSM-23 zeolites.
Fig. 8：Crystal seed method synthesizes the XRD spectra of ZSM-35 zeolites.
Fig. 9：Crystal seed method synthesizes the XRD spectra of EU-1 zeolites.
Specific embodiment
In the present invention, zeolite molecular sieve crystal seed be it is following any one：ZSM-5、MOR、ZSM-12、ZSM-22、ZSM-23、
ZSM-35, EU-1 or ZSM-22/ZSM-23 coexisting phase.Each zeolite molecular sieve crystal seed can be by city available from or by ability
Preparation method known to domain is obtained, and the present invention is repeated no more.
Embodiment 1：Crystallization of the omnipotent presoma under the conditions of 160 DEG C
First, by 8.12gH2O (deionized water, same as below) is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to
0.38gNaOH, adds 3.32g Ludox (dioxide-containing silica 30.5%, same as below) afterwards under agitation, continues stirring straight
Become uniform to solution, then reaction raw materials are added in politef stainless steel cauldron, 160 DEG C of crystallization 24h, product are taken out
Filter, obtains product after drying.
The proportioning of reaction raw materials is as follows：SiO2:0.0083Al2O3:0.28Na2O:35H2O
Its structure of Jing X-ray diffraction analysis is unformed.Accompanying drawing 1 is omnipotent presoma after crystallization under the conditions of 160 DEG C
XRD spectra.
Embodiment 2：Crystallization of the omnipotent presoma in the case of addition ZSM-5 zeolite molecular sieve seed under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-5 molecular sieve and does crystal seed, stirs
After mixing uniformly, gel is added in politef stainless steel cauldron, crystallization 8h in 160 DEG C of baking ovens.Product sucking filtration, dries
It is dry.
Accompanying drawing 2 is the XRD spectra of ZSM-5 zeolite molecular sieve prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-5 zeolite molecular sieve structure, and sample have higher degree of crystallinity.
Embodiment 3：Crystallization of the omnipotent presoma in the case of addition MOR zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%MOR molecular sieve and does crystal seed, stirs
After uniform, gel is added in politef stainless steel cauldron, crystallization 12h in 160 DEG C of baking ovens.Product sucking filtration, drying.
Accompanying drawing 3 is the XRD spectra of MOR zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typically
MOR zeolite molecules sieve structures, and sample has higher degree of crystallinity.
Embodiment 4：Crystallization of the omnipotent presoma in the case of addition ZSM-12 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-12 molecular sieve and does crystal seed,
After stirring, gel is added in politef stainless steel cauldron, crystallization 15h in 160 DEG C of baking ovens.Product sucking filtration,
Drying.
Accompanying drawing 4 is the XRD spectra of ZSM-12 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-12 zeolite molecules sieve structures, and sample have higher degree of crystallinity.
Embodiment 5：Crystallization of the omnipotent presoma in the case of addition ZSM-22 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-22 molecular sieve and does crystal seed,
After stirring, gel is added in politef stainless steel cauldron, crystallization 15h in 160 DEG C of baking ovens.Product sucking filtration,
Drying.
Accompanying drawing 5 is the XRD spectra of ZSM-22 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-22 zeolite molecules sieve structures, and sample have higher degree of crystallinity.
Embodiment 6：Crystallization of the omnipotent presoma in the case of addition ZSM-23 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-23 molecular sieve and does crystal seed,
After stirring, gel is added in politef stainless steel cauldron, crystallization 10h in 160 DEG C of baking ovens.Product sucking filtration,
Drying.
Accompanying drawing 6 is the XRD spectra of ZSM-23 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-23 zeolite molecules sieve structures, and sample have higher degree of crystallinity.
Embodiment 7：In the case of omnipotent presoma adds ZSM-22/ZSM-23 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
Crystallization
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-22/ZSM-23 molecular sieve
Crystal seed is done, after stirring, gel is added in politef stainless steel cauldron, crystallization 18h in 160 DEG C of baking ovens.Produce
Thing sucking filtration, drying.
Accompanying drawing 7 is the XRD spectra of ZSM-23 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-23 zeolite molecules sieve structures, and sample have higher degree of crystallinity.
Embodiment 8：Crystallization of the omnipotent presoma in the case of addition ZSM-35 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%ZSM-35 molecular sieve and does crystal seed,
After stirring, gel is added in politef stainless steel cauldron, crystallization 14h in 160 DEG C of baking ovens.Product sucking filtration,
Drying.
Accompanying drawing 8 is the XRD spectra of ZSM-35 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typical case
ZSM-35 zeolite molecules sieve structures, and sample have higher degree of crystallinity.
Embodiment 9：Crystallization of the omnipotent presoma in the case of addition EU-1 zeolite molecular sieve crystal seeds under the conditions of 160 DEG C
By 8.12gH2O is mixed homogeneously with 0.092g aluminum sulfate, then is added thereto to 0.38gNaOH, adds under agitation afterwards
Enter 3.32g Ludox, continue stirring after solution becomes uniform, addition accounts for silicon source quality 10%EU-1 molecular sieve and does crystal seed, stirs
After mixing uniformly, gel is added in politef stainless steel cauldron, crystallization 24h in 160 DEG C of baking ovens.Product sucking filtration, dries
It is dry.
Accompanying drawing 9 is the XRD spectra of EU-1 zeolite molecular sieves prepared by crystal seed method, by spectrogram it can be seen that product has typically
EU-1 zeolite molecules sieve structures, and sample has higher degree of crystallinity.
The above, is only several case study on implementation of the present invention, any pro forma restriction is not done to the present invention,
Although the present invention is disclosed as above with preferable case study on implementation, but is not limited to the present invention, any to be familiar with this professional skill
Art personnel, in the range of without departing from technical solution of the present invention, when the structure and technology contents using the disclosure above makes a little
Change or be modified to the equivalence enforcement case of equivalent variations.But every content without departing from technical solution of the present invention, foundation
Any simple modification, equivalent variations and modification that the technical spirit of the present invention is made to above case study on implementation, still belong to the present invention
In the range of technical scheme.
Claims (2)
1. a kind of method with omnipotent gel synthesizing high-silicon zeolite molecular sieve, it is characterised in that comprise the steps：
After deionized water is mixed homogeneously with silicon source, NaOH is added thereto to, adds silicon source under agitation, persistently stirred until molten
Liquid forms silica-alumina gel；The zeolite molecular sieve crystal seed for accounting for silicon source quality 10% is added in silica-alumina gel, reaction after stirring, is placed in
In kettle, in 160 DEG C of 8～24h of crystallization；；Product sucking filtration, drying, that is, obtain the former powder of silica-rich zeolite molecular sieve；
The addition for controlling each reaction raw materials makes its molar ratio range for SiO2∶0.0083Al2O3∶0.28Na2O∶35H2O；
The zeolite molecular sieve crystal seed be it is following any one：ZSM-5、MOR、ZSM-12、ZSM-22、ZSM-23、ZSM-35、
EU-1 or ZSM-22/ZSM-23 coexisting phases.
2. method according to claim 1, it is characterised in that source of aluminium is aluminum sulfate, and silicon source is dioxide-containing silica
30.5% Ludox, alkali source are sodium hydroxide.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106809846A (en) * | 2017-01-10 | 2017-06-09 | 浙江大学 | The method that crystal seed synthetic method prepares the molecular sieves of EU 1 |
| WO2018218736A1 (en) * | 2017-06-02 | 2018-12-06 | 中山大学 | Aluminosilicate zeolite molecular sieve having bog structure and preparation method therefor |
| CN110372003A (en) * | 2019-08-22 | 2019-10-25 | 正大能源材料(大连)有限公司 | A kind of preparation method of big partial size Beta molecular sieve |
| CN110683558A (en) * | 2018-07-06 | 2020-01-14 | 中国石油天然气股份有限公司 | Synthesis method of MTT zeolite molecular sieve with short shaft morphology |
| CN110877912A (en) * | 2018-09-06 | 2020-03-13 | 中国科学院大连化学物理研究所 | Rapid synthesis method of FER molecular sieve with controllable size |
| US20210094836A1 (en) * | 2019-09-30 | 2021-04-01 | China University Of Petroleum-Beijing | Method of synthesizing an aluminosilicate molecular sieve by a crystal seed-assisted method |
| CN113415808A (en) * | 2021-06-13 | 2021-09-21 | 浙江大学 | Method for in-situ synthesis of formed molecular sieve without organic template agent |
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| CN102992346A (en) * | 2012-12-09 | 2013-03-27 | 浙江大学 | Seed crystal synthesis method for preparing ZSM-23 molecular sieve |
| CN103101924A (en) * | 2013-02-01 | 2013-05-15 | 浙江大学 | Method for preparing ZSM-22 molecular sieve by using seed crystal synthesis method |
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| CN101249968A (en) * | 2008-03-10 | 2008-08-27 | 吉林大学 | Method for synthesizing Beta molecular sieve by organic-free template |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106809846A (en) * | 2017-01-10 | 2017-06-09 | 浙江大学 | The method that crystal seed synthetic method prepares the molecular sieves of EU 1 |
| WO2018218736A1 (en) * | 2017-06-02 | 2018-12-06 | 中山大学 | Aluminosilicate zeolite molecular sieve having bog structure and preparation method therefor |
| CN110683558A (en) * | 2018-07-06 | 2020-01-14 | 中国石油天然气股份有限公司 | Synthesis method of MTT zeolite molecular sieve with short shaft morphology |
| CN110683558B (en) * | 2018-07-06 | 2022-02-01 | 中国石油天然气股份有限公司 | Synthesis method of MTT zeolite molecular sieve with short shaft morphology |
| CN110877912A (en) * | 2018-09-06 | 2020-03-13 | 中国科学院大连化学物理研究所 | Rapid synthesis method of FER molecular sieve with controllable size |
| CN110877912B (en) * | 2018-09-06 | 2023-01-13 | 中国科学院大连化学物理研究所 | Rapid synthesis method of FER molecular sieve with controllable size |
| CN110372003A (en) * | 2019-08-22 | 2019-10-25 | 正大能源材料(大连)有限公司 | A kind of preparation method of big partial size Beta molecular sieve |
| US20210094836A1 (en) * | 2019-09-30 | 2021-04-01 | China University Of Petroleum-Beijing | Method of synthesizing an aluminosilicate molecular sieve by a crystal seed-assisted method |
| US11634334B2 (en) * | 2019-09-30 | 2023-04-25 | China University Of Petroleum-Beijing | Method of synthesizing an aluminosilicate molecular sieve by a crystal seed-assisted method |
| CN113415808A (en) * | 2021-06-13 | 2021-09-21 | 浙江大学 | Method for in-situ synthesis of formed molecular sieve without organic template agent |
| CN113415808B (en) * | 2021-06-13 | 2023-02-28 | 浙江大学 | Method for in-situ synthesis of formed molecular sieve without organic template |
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