CN111217379A - 一种低硅铝比mtw型分子筛合成方法 - Google Patents
一种低硅铝比mtw型分子筛合成方法 Download PDFInfo
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- CN111217379A CN111217379A CN201811431268.5A CN201811431268A CN111217379A CN 111217379 A CN111217379 A CN 111217379A CN 201811431268 A CN201811431268 A CN 201811431268A CN 111217379 A CN111217379 A CN 111217379A
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- Prior art keywords
- mixture
- molecular sieve
- aluminum
- type molecular
- mtw type
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- 239000002808 molecular sieve Substances 0.000 title claims abstract description 66
- 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 66
- 238000000034 method Methods 0.000 title claims abstract description 15
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 230000002194 synthesizing effect Effects 0.000 title abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000010438 heat treatment Methods 0.000 claims abstract description 22
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 17
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 12
- 239000010703 silicon Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 10
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 21
- 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 20
- 229910052708 sodium Inorganic materials 0.000 claims description 20
- 239000011734 sodium Substances 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 14
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims description 14
- 238000005406 washing Methods 0.000 claims description 14
- 150000001412 amines Chemical class 0.000 claims description 13
- 238000002425 crystallisation Methods 0.000 claims description 12
- 230000008025 crystallization Effects 0.000 claims description 12
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 11
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 claims description 11
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 8
- 229910052593 corundum Inorganic materials 0.000 claims description 8
- 238000003786 synthesis reaction Methods 0.000 claims description 8
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 8
- HWCKGOZZJDHMNC-UHFFFAOYSA-M tetraethylammonium bromide Chemical compound [Br-].CC[N+](CC)(CC)CC HWCKGOZZJDHMNC-UHFFFAOYSA-M 0.000 claims description 5
- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 claims description 3
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 2
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical compound [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 2
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- YMBCJWGVCUEGHA-UHFFFAOYSA-M tetraethylammonium chloride Chemical compound [Cl-].CC[N+](CC)(CC)CC YMBCJWGVCUEGHA-UHFFFAOYSA-M 0.000 claims description 2
- GRVPDGGTLNKOBZ-UHFFFAOYSA-M triethyl(methyl)azanium;bromide Chemical compound [Br-].CC[N+](C)(CC)CC GRVPDGGTLNKOBZ-UHFFFAOYSA-M 0.000 claims description 2
- NIUZJTWSUGSWJI-UHFFFAOYSA-M triethyl(methyl)azanium;chloride Chemical compound [Cl-].CC[N+](C)(CC)CC NIUZJTWSUGSWJI-UHFFFAOYSA-M 0.000 claims description 2
- 238000010189 synthetic method Methods 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 21
- 238000001308 synthesis method Methods 0.000 abstract description 7
- 239000000126 substance Substances 0.000 abstract description 4
- 239000003245 coal Substances 0.000 abstract description 3
- 238000005504 petroleum refining Methods 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000006243 chemical reaction Methods 0.000 description 26
- 229910001220 stainless steel Inorganic materials 0.000 description 24
- 239000010935 stainless steel Substances 0.000 description 24
- 239000011259 mixed solution Substances 0.000 description 20
- -1 polytetrafluoroethylene Polymers 0.000 description 20
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 20
- 239000004810 polytetrafluoroethylene Substances 0.000 description 20
- 239000000243 solution Substances 0.000 description 16
- 238000012512 characterization method Methods 0.000 description 13
- 239000008367 deionised water Substances 0.000 description 12
- 229910021641 deionized water Inorganic materials 0.000 description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 238000001228 spectrum Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 5
- 239000013078 crystal Substances 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 3
- 229910021536 Zeolite Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000010457 zeolite Substances 0.000 description 2
- 238000007171 acid catalysis Methods 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000004517 catalytic hydrocracking Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
Images
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
- C01B39/46—Other types characterised by their X-ray diffraction pattern and their defined composition
- C01B39/48—Other types characterised by their X-ray diffraction pattern and their defined composition using at least one organic template directing agent
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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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)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
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CN111217379A true CN111217379A (zh) | 2020-06-02 |
CN111217379B CN111217379B (zh) | 2022-12-06 |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112499644A (zh) * | 2020-12-10 | 2021-03-16 | 安徽纳蓝环保科技有限公司 | 一种低SiO2/Al2O3的Cu-CHA分子筛及其制备方法 |
CN113325042A (zh) * | 2021-06-11 | 2021-08-31 | 吉林大学 | 一种钠型mtw分子筛及其制备方法和应用、氨气气体传感器及其制备方法和应用 |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3970544A (en) * | 1974-05-06 | 1976-07-20 | Mobil Oil Corporation | Hydrocarbon conversion with ZSM-12 |
US20050158237A1 (en) * | 2004-01-16 | 2005-07-21 | Indian Oil Corporation Limited | Process for enhancing yield of sodium aluminosilicate molecular sieves during synthesis |
CN101205072A (zh) * | 2006-12-18 | 2008-06-25 | 中国石油化工股份有限公司 | 一种低硅铝比β沸石的合成方法 |
CN102910646A (zh) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | 一种梯度酸分布zsm-5分子筛及其制备方法 |
CN103880037A (zh) * | 2012-12-20 | 2014-06-25 | 中国石油化工股份有限公司 | 一种zsm-5分子筛及其制备方法 |
CN106946266A (zh) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | 一种sapo-34/zsm-12复合分子筛及其合成方法 |
-
2018
- 2018-11-26 CN CN201811431268.5A patent/CN111217379B/zh active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3970544A (en) * | 1974-05-06 | 1976-07-20 | Mobil Oil Corporation | Hydrocarbon conversion with ZSM-12 |
US20050158237A1 (en) * | 2004-01-16 | 2005-07-21 | Indian Oil Corporation Limited | Process for enhancing yield of sodium aluminosilicate molecular sieves during synthesis |
CN101205072A (zh) * | 2006-12-18 | 2008-06-25 | 中国石油化工股份有限公司 | 一种低硅铝比β沸石的合成方法 |
CN102910646A (zh) * | 2011-08-01 | 2013-02-06 | 中国石油化工股份有限公司 | 一种梯度酸分布zsm-5分子筛及其制备方法 |
CN103880037A (zh) * | 2012-12-20 | 2014-06-25 | 中国石油化工股份有限公司 | 一种zsm-5分子筛及其制备方法 |
CN106946266A (zh) * | 2016-01-07 | 2017-07-14 | 中国石油化工股份有限公司 | 一种sapo-34/zsm-12复合分子筛及其合成方法 |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112499644A (zh) * | 2020-12-10 | 2021-03-16 | 安徽纳蓝环保科技有限公司 | 一种低SiO2/Al2O3的Cu-CHA分子筛及其制备方法 |
CN113325042A (zh) * | 2021-06-11 | 2021-08-31 | 吉林大学 | 一种钠型mtw分子筛及其制备方法和应用、氨气气体传感器及其制备方法和应用 |
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Inventor after: Tian Zhijian Inventor after: Wang Xiaoping Inventor after: Wang Shuaiqi Inventor after: Chi Kebin Inventor after: Wang Congxin Inventor after: Yan Lijun Inventor after: Lv Guang Inventor after: Li Mengchen Inventor after: Wang Ping Inventor after: Shen Yuge Inventor before: Tian Zhijian Inventor before: Wang Shuaiqi Inventor before: Wang Congxin Inventor before: Lv Guang Inventor before: Wang Ping Inventor before: Wang Xiaoping |
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Effective date of registration: 20210127 Address after: No.16 ande Road, Dongcheng District, Beijing Applicant after: PetroChina Company Limited Applicant after: DALIAN INSTITUTE OF CHEMICAL PHYSICS, CHINESE ACADEMY OF SCIENCES Address before: 116023 No. 457-41 Zhongshan Road, Shahekou District, Dalian City, Liaoning Province Applicant before: DALIAN INSTITUTE OF CHEMICAL PHYSICS, CHINESE ACADEMY OF SCIENCES |
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