CN105399110A - Synthetic method of porous ZSM-5 molecular sieve - Google Patents
Synthetic method of porous ZSM-5 molecular sieve Download PDFInfo
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- CN105399110A CN105399110A CN201510983918.7A CN201510983918A CN105399110A CN 105399110 A CN105399110 A CN 105399110A CN 201510983918 A CN201510983918 A CN 201510983918A CN 105399110 A CN105399110 A CN 105399110A
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- molecular sieve
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 42
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 238000010189 synthetic method Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 22
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 10
- 239000011148 porous material Substances 0.000 claims abstract description 10
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 239000008367 deionised water Substances 0.000 claims description 14
- 229910021641 deionized water Inorganic materials 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 8
- 229910052708 sodium Inorganic materials 0.000 claims description 8
- 239000011734 sodium Substances 0.000 claims description 8
- LPSKDVINWQNWFE-UHFFFAOYSA-M tetrapropylazanium;hydroxide Chemical compound [OH-].CCC[N+](CCC)(CCC)CCC LPSKDVINWQNWFE-UHFFFAOYSA-M 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 6
- 238000005245 sintering Methods 0.000 claims description 4
- 238000003763 carbonization Methods 0.000 claims description 2
- 239000012535 impurity Substances 0.000 claims description 2
- 230000002045 lasting effect Effects 0.000 claims description 2
- 229910021536 Zeolite Inorganic materials 0.000 abstract description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000007787 solid Substances 0.000 abstract description 4
- 239000010457 zeolite Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- 230000001419 dependent effect Effects 0.000 abstract 1
- 239000002149 hierarchical pore Substances 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 238000010992 reflux Methods 0.000 description 4
- 230000003068 static effect Effects 0.000 description 4
- 230000009977 dual effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
- C01P2006/17—Pore diameter distribution
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a synthetic method of a porous ZSM-5 molecular sieve. A hard template is added during the synthetic process of the ZSM-5 molecular sieve, and then the synthesized ZSM-5 molecular sieve undergoes high-temperature calcination charring to remove the template so as to prepare the ZSM-5 molecular sieve containing multiple pore sizes. Based on traditional ZSM-5 molecular sieve synthesis, the porous ZSM-5 molecular sieve is prepared by a hard template method. According to mesopores introduced by the use of a hard template method, the structure and pore diameter are often dependent on morphology and size of a solid template. By using proper carbon nanotube as a solid template and by controlling conditions of a hydrothermal reaction, an ideal pore structure can be introduced into a zeolite molecular sieve. The synthesized porous ZSM-5 molecular sieve has a hierarchical pore structure. As a porous carbon nanotube template can penetrate through the whole zeolite crystal, the molecular sieve has larger specific surface area and more active sites. Thus, application range of the ZSM-5 molecular sieve is broadened.
Description
Technical field
The present invention relates to a kind of synthetic method of porous ZSM-5 molecular sieve.
Background technology
ZSM-5 molecular sieve because having the advantages such as the selective activization of good thermostability, acid resistance and excellence, and in absorption and the field such as catalysis by extensive concern.Adopt the ZSM-5 molecular sieve of traditional method synthesis, because aperture is little, structure is single, cause many macromolecular substance to be adsorbed, block duct and affect gas molecule and spread; Simultaneously because aperture is too little, the material that many molecules are larger cannot enter in duct catalyzed, reduces catalytic performance.For overcoming above shortcoming, the present invention adopts the ZSM-5 molecular sieve in the synthesizing porous road of new method.Namely there is being interconnected of the duct of the different sizes be interconnected in multi-pore channel, such as micropore, mesoporous, macropore, dual micropore, dual mesoporous, dual macropore etc. in same material of main part simultaneously.
At present, research and development and the application of porous material receive much concern, because this polyporous materials has the constructional feature in various duct concurrently, and obviously can increase the avtive spot of catalyzer.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of synthetic method of porous ZSM-5 molecular sieve is provided.
To achieve these goals, the present invention adopts following technical scheme:
A kind of synthetic method of porous ZSM-5 molecular sieve, add hard mould agent in ZSM-5 molecular sieve building-up process, then high temperature sintering charing is carried out to the ZSM-5 molecular sieve of synthesis and remove template, thus prepare the ZSM-5 molecular sieve containing multiple duct size.
As preferably, in the synthetic method of above-mentioned porous ZSM-5 molecular sieve, described hard mould agent is the carbon nanotube of several different pore size size, and the Diameter distribution scope of carbon nanotube template is 8-50nm.
As preferably, in the synthetic method of above-mentioned porous ZSM-5 molecular sieve, described high temperature sintering adopts hydrothermal method, temperature 120-180 DEG C of lasting 15-24h; The temperature 400-800 DEG C of described charing, carbonization time 50-70h, form powdery porous ZSM-5 molecular sieve.
As preferably, in the synthetic method of above-mentioned porous ZSM-5 molecular sieve, specifically comprise the steps: to get different tube diameters carbon nanotube to add in concentrated hydrochloric acid and soak 6-24h, until the impurity contained by carbon nanotube can not make hydrochloric acid soln change color, take out dry after for subsequent use; Take sodium metaaluminate and be dissolved in TPAOH and deionized water; In above-mentioned solution, add dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature, then add tetraethyl orthosilicate, ambient temperatare puts 5-35h to gel form; Above-mentioned solution is moved to 120-180 DEG C of hydro-thermal 5-48h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization, carbonize 20-80h at retort furnace high temperature 500-800 DEG C and remove hard mould agent.The part by weight scope (0.2-1.5) of sodium metaaluminate, TPAOH, tetraethyl orthosilicate, dehydrated alcohol and deionized water: (3.0-12.0): (3.5-14.5): (2-14): (0.5-5).
Compared with prior art, the present invention has following beneficial effect: the present invention is on the synthesis basis of traditional Z SM-5 molecular sieve, adopts hard template method to prepare a kind of multi-pore channel ZSM-5 molecular sieve.What use hard template method to introduce is mesoporous, pattern and the size of solid template agent used are often depended in its structure and aperture, adopting the carbon nanotube be applicable to as solid template agent, by controlling the condition of hydro-thermal reaction, desirable pore passage structure can be introduced in zeolite molecular sieve.Multi-stage porous ZSM-5 molecular sieve through synthesis has multilevel size pore passage structure, and porous carbon nanotube template can run through whole zeolite crystal, has the more avtive spots of large specific surface sum, adds the application of ZSM-5 molecular sieve.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but protection scope of the present invention is not limited to the scope that embodiment describes.
The synthesis of the ZSM-5 molecular sieve of embodiment 1:8-20nm duct size
Getting caliber is 8-15nm and 10-20nm two kinds of carbon nanotubes.Weigh according to mass ratio 2:1 and amount to 6.6g, reflux 24h at 70 DEG C in 100mL concentrated hydrochloric acid, purifying 6 times.Take 0.8g sodium metaaluminate and be dissolved in 7.4g TPAOH (40% quality) and 2.0g deionized water.In above-mentioned solution, add 7.0g dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature, then add 8.4g tetraethyl orthosilicate, static placement 16h is to gel form.Above-mentioned solution is moved to 180 DEG C of hydro-thermal 70h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization.20h is carbonized at retort furnace high temperature 600 DEG C.
The synthesis of the ZSM-5 molecular sieve of embodiment 2:10-30nm duct size
Getting caliber is 10-20nm and 20-30nm two kinds of carbon nanotubes.Weigh according to mass ratio 2:1 and amount to 6.6g, reflux 24h at 70 DEG C in 100mL concentrated hydrochloric acid, purifying 6 times.Take 0.8g sodium metaaluminate and be dissolved in 7.4g TPAOH (40% quality) and 2.0g deionized water.In above-mentioned solution, add 7.0g dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature, then add 8.4g tetraethyl orthosilicate, static placement 16h is to gel form.Above-mentioned solution is moved to 180 DEG C of hydro-thermal 70h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization.20h is carbonized at retort furnace high temperature 600 DEG C.
The synthesis of the ZSM-5 molecular sieve of embodiment 3:8-40nm duct size
Getting caliber is 8-15nm, 15-30nm and 20-40nm tri-kinds of carbon nanotubes.Weigh according to mass ratio 3:2:1 and amount to 6.6g, reflux 24h at 70 DEG C in 100mL concentrated hydrochloric acid, purifying 6 times.Take 0.8g sodium metaaluminate and be dissolved in 7.4g TPAOH (40% quality) and 2.0g deionized water.In above-mentioned solution, add 7.0g dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature, then add 8.4g tetraethyl orthosilicate, static placement 16h is to gel form.Above-mentioned solution is moved to 180 DEG C of hydro-thermal 70h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization.20h is carbonized at retort furnace high temperature 600 DEG C.
The synthesis of the ZSM-5 molecular sieve of embodiment 4:8-50nm duct size
Getting caliber is 8-15nm, 10-20nm, 20-30nm and 30-50nm tetra-kinds of carbon nanotubes.Proportionally 4:3:2:1 weighs and amounts to 6.6g, reflux 24h at 70 DEG C in 100mL concentrated hydrochloric acid, purifying 6 times.Take 0.8g sodium metaaluminate and be dissolved in 7.4g TPAOH (40% quality) and 2.0g deionized water.In above-mentioned solution, add 7.0g dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature adds, then adds 8.4g tetraethyl orthosilicate, and static placement 16h is to gel form.Above-mentioned solution is moved to 180 DEG C of hydro-thermal 70h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization.20h is carbonized at retort furnace high temperature 600 DEG C.
Claims (5)
1. the synthetic method of a porous ZSM-5 molecular sieve, it is characterized in that adding hard mould agent in ZSM-5 molecular sieve building-up process, then high temperature sintering charing is carried out to the ZSM-5 molecular sieve of synthesis and remove template, thus prepare the ZSM-5 molecular sieve containing multiple duct size.
2. the synthetic method of porous ZSM-5 molecular sieve according to claim 1, is characterized in that, described hard mould agent is the carbon nanotube of several different pore size size, and the Diameter distribution scope of carbon nanotube template is 8-50nm.
3. the synthetic method of porous ZSM-5 molecular sieve according to claim 1, is characterized in that described high temperature sintering adopts hydrothermal method, temperature 120-180 DEG C of lasting 15-24h; The temperature 400-800 DEG C of described charing, carbonization time 50-70h.
4. the synthetic method of porous ZSM-5 molecular sieve according to claim 1, it is characterized in that comprising the steps: getting different tube diameters carbon nanotube to add in concentrated hydrochloric acid and soak 6-24h, until the impurity contained by carbon nanotube can not make hydrochloric acid soln change color, take out dry rear for subsequent use; Take sodium metaaluminate and be dissolved in TPAOH and deionized water; In above-mentioned solution, add dehydrated alcohol again, add pretreated carbon nanotube, unnecessary alcohol of volatilizing under room temperature, then add tetraethyl orthosilicate, ambient temperatare puts 5-35h to gel form; Above-mentioned solution is moved to 120-180 DEG C of hydro-thermal 5-48h in crystallization still, to filter, 100 DEG C of dry 24h with deionized water and washing with alcohol after crystallization, carbonize 20-80h at retort furnace high temperature 500-800 DEG C and remove hard mould agent.
5. the synthetic method of porous ZSM-5 molecular sieve according to claim 4, it is characterized in that, the part by weight scope (0.2-1.5) of sodium metaaluminate, TPAOH, tetraethyl orthosilicate, dehydrated alcohol and deionized water: (3.0-12.0): (3.5-14.5): (2-14): (0.5-5).
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106276967A (en) * | 2016-08-16 | 2017-01-04 | 中国科学院福建物质结构研究所 | A kind of synthetic method of mesoporous zeolite |
| CN107572548A (en) * | 2017-11-02 | 2018-01-12 | 肇庆高新区国专科技有限公司 | A kind of method for the MFI molecular sieves for synthesizing the microporous mesoporous structure of pure silicon |
| CN109351206A (en) * | 2018-10-23 | 2019-02-19 | 黄山学院 | A kind of preparation method of zeolite molecular sieve membrane for nanofiltration |
| CN109354037A (en) * | 2018-11-30 | 2019-02-19 | 太原理工大学 | A kind of HZSM-5 molecular sieve with nanorod binding structure and its preparation method and application |
| CN113198527A (en) * | 2021-04-25 | 2021-08-03 | 西南化工研究设计院有限公司 | Composite hierarchical pore molecular sieve catalyst for preparing aromatic hydrocarbon from low-carbon alkane and preparation method thereof |
| CN113636566A (en) * | 2021-08-05 | 2021-11-12 | 肯特催化材料股份有限公司 | All-silicon Beta molecular sieve synthesis process and all-silicon Beta molecular sieve prepared by same |
| CN114471674A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Carbon nano tube/ZSM-5 molecular sieve compound and synthesis method and application thereof |
| CN117816227A (en) * | 2023-12-28 | 2024-04-05 | 中国科学院山西煤炭化学研究所 | A method for preparing a core-shell structure composite molecular sieve with through pores |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106276967A (en) * | 2016-08-16 | 2017-01-04 | 中国科学院福建物质结构研究所 | A kind of synthetic method of mesoporous zeolite |
| CN107572548A (en) * | 2017-11-02 | 2018-01-12 | 肇庆高新区国专科技有限公司 | A kind of method for the MFI molecular sieves for synthesizing the microporous mesoporous structure of pure silicon |
| CN109351206A (en) * | 2018-10-23 | 2019-02-19 | 黄山学院 | A kind of preparation method of zeolite molecular sieve membrane for nanofiltration |
| CN109354037A (en) * | 2018-11-30 | 2019-02-19 | 太原理工大学 | A kind of HZSM-5 molecular sieve with nanorod binding structure and its preparation method and application |
| CN109354037B (en) * | 2018-11-30 | 2021-09-24 | 太原理工大学 | A kind of HZSM-5 molecular sieve with nanorod binding structure and its preparation method and application |
| CN114471674A (en) * | 2020-10-26 | 2022-05-13 | 中国石油化工股份有限公司 | Carbon nano tube/ZSM-5 molecular sieve compound and synthesis method and application thereof |
| CN114471674B (en) * | 2020-10-26 | 2024-05-07 | 中国石油化工股份有限公司 | Carbon nano tube/ZSM-5 molecular sieve compound and synthetic method and application thereof |
| CN113198527A (en) * | 2021-04-25 | 2021-08-03 | 西南化工研究设计院有限公司 | Composite hierarchical pore molecular sieve catalyst for preparing aromatic hydrocarbon from low-carbon alkane and preparation method thereof |
| CN113636566A (en) * | 2021-08-05 | 2021-11-12 | 肯特催化材料股份有限公司 | All-silicon Beta molecular sieve synthesis process and all-silicon Beta molecular sieve prepared by same |
| CN117816227A (en) * | 2023-12-28 | 2024-04-05 | 中国科学院山西煤炭化学研究所 | A method for preparing a core-shell structure composite molecular sieve with through pores |
| CN117816227B (en) * | 2023-12-28 | 2025-12-19 | 中国科学院山西煤炭化学研究所 | Preparation method of core-shell structure composite molecular sieve with through pore canal |
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