CN105692647B - A kind of preparation method of the molecular sieves of SSZ 13 - Google Patents
A kind of preparation method of the molecular sieves of SSZ 13 Download PDFInfo
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- CN105692647B CN105692647B CN201610152114.7A CN201610152114A CN105692647B CN 105692647 B CN105692647 B CN 105692647B CN 201610152114 A CN201610152114 A CN 201610152114A CN 105692647 B CN105692647 B CN 105692647B
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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
- C01B39/04—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 using at least one organic template directing agent, e.g. an ionic quaternary ammonium compound or an aminated compound
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- 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
- C01P2006/12—Surface area
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- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
Description
Relative crystallinity/% | Total specific surface area/m2/g | |
Embodiment 1 | 105 | 565 |
Embodiment 2 | 98 | 570 |
Embodiment 3 | 99 | 576 |
Embodiment 4 | 100 | 582 |
Claims (4)
- A kind of 1. preparation method of SSZ-13 molecular sieves, it is characterised in that:Comprise the following steps:It is well mixed, obtains 1. sequentially adding silicon source, silicon source, sodium hydroxide and the first template in water in autoclave Mixed liquor, SSZ-13 molecular sieves are added into mixed liquor and organic amine promoter is well mixed and obtains reaction solution;Described first Template is N, and N, N- trimethyl -1- adamantyl ammonium hydroxide, described organic amine promoter is cetyl trimethyl bromine Change ammonium, H in the reaction solution2O:Na2O:Al2O3:SiO2:The mol ratio of first template is 15 ~ 30:0.1~0.3:0.02~ 0.04:1:0.05~0.08;The mass ratio of the SSZ-13 molecular sieves, cetyl trimethylammonium bromide and mixed liquor is 1:2~ 3:280~320;The silicon source is silica gel, Ludox or aerosil;Silicon source is aluminum sulfate or aluminium hydroxide;2. by reaction solution be warming up to 115 ~ 125 DEG C under agitation react 9 ~ 10 hours, then heat to 155 ~ 165 DEG C reaction 35 ~ 45 hours, the second template was then added thereto and continues stirring reaction 45 ~ 50 hours, obtains crystallization product;Described second Template is triethylamine or pyridine;The mol ratio of second template and the first template is 1:2~4;3. by step, 2. gained crystallization product is centrifuged, and filtrate and filter cake is obtained, by gained filter cake through washing, being dried to obtain SSZ-13 molecular screen primary powders, gained SSZ-13 molecular screen primary powders are placed in 500 ~ 600 DEG C of Muffle kiln roastings 4 ~ 6 hours, obtained SSZ-13 molecular sieves.
- A kind of 2. preparation method of SSZ-13 molecular sieves according to claim 1, it is characterised in that:Second template is three Ethamine.
- A kind of 3. preparation method of SSZ-13 molecular sieves according to claim 1, it is characterised in that:To step, 3. gained is filtered Liquid adds sodium tripolyphosphate and guar gum, obtains mixed liquor, by mixed liquor standing sedimentation 10 ~ 12 hours, is separated by filtration, is sunk Shallow lake and recirculated water;The mass ratio of the filtrate, sodium tripolyphosphate and guar gum is 190 ~ 210:1:2~3.
- A kind of 4. preparation method of SSZ-13 molecular sieves, it is characterised in that:Comprise the following steps:It is well mixed, obtains 1. sequentially adding silica gel, aluminum sulfate, sodium hydroxide and the first template in water in autoclave To mixed liquor, SSZ-13 molecular sieves are added into mixed liquor and organic amine promoter is well mixed and obtains reaction solution;Described One template is N, and N, N- trimethyl -1- adamantyl ammonium hydroxide, described organic amine promoter is cetyl trimethyl Ammonium bromide, H in the reaction solution2O:Na2O:Al2O3:SiO2:The mol ratio of first template is 25:0.2:0.03:1:0.06; The mass ratio of the SSZ-13 molecular sieves, cetyl trimethylammonium bromide and mixed liquor is 1:3:280;2. reaction solution is warming up into 120 DEG C to react 9 hours under agitation, then heats to 160 DEG C and react 40 hours, then to it The second template of middle addition continues stirring reaction 48 hours, obtains crystallization product;The second described template is triethylamine;Second The mol ratio of template and the first template is 1:3;3. by step, 2. gained crystallization product is centrifuged, and filtrate and filter cake is obtained, by gained filter cake through washing, being dried to obtain SSZ-13 molecular screen primary powders, gained SSZ-13 molecular screen primary powders are placed in 550 DEG C of Muffle kiln roastings 5 hours, obtain SSZ-13 Molecular sieve.
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CN201610152114.7A CN105692647B (en) | 2016-03-17 | 2016-03-17 | A kind of preparation method of the molecular sieves of SSZ 13 |
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CN201610152114.7A CN105692647B (en) | 2016-03-17 | 2016-03-17 | A kind of preparation method of the molecular sieves of SSZ 13 |
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CN105692647A CN105692647A (en) | 2016-06-22 |
CN105692647B true CN105692647B (en) | 2018-03-06 |
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Families Citing this family (14)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106276953B (en) * | 2016-08-26 | 2018-02-06 | 天津南化催化剂有限公司 | A kind of preparation method of the molecular sieves of SSZ 13 |
CN106334577A (en) * | 2016-09-29 | 2017-01-18 | 南昌大学 | Preparation method of Mo modified Cu-SSZ-13 catalyst |
CN106629761B (en) * | 2016-12-20 | 2017-11-24 | 上海卓悦化工科技有限公司 | A kind of synthetic method of the molecular sieves of SSZ 13 |
CN106587097A (en) * | 2016-12-26 | 2017-04-26 | 中国地质大学(武汉) | Method for synthesizing SSZ-13 zeolite molecular sieve by utilizing micron-silicon powder |
CN107627422A (en) * | 2017-11-01 | 2018-01-26 | 徐州得铸生物科技有限公司 | A kind of garden landscape wood of resistance to deformation |
CN108059172B (en) * | 2017-12-13 | 2020-07-10 | 山东齐鲁华信高科有限公司 | Preparation method of H-SSZ-13 molecular sieve |
CN108529642B (en) * | 2018-05-24 | 2021-07-20 | 山东泓泰恒瑞新材料有限公司 | Preparation method of Cu-SSZ-13 molecular sieve |
CN109126862A (en) * | 2018-08-20 | 2019-01-04 | 中国汽车技术研究中心有限公司 | It is a kind of accelerate synthesis CHA structure molecular sieve method and its catalyst NH3-SCR reaction in application |
CN109534354A (en) * | 2018-11-12 | 2019-03-29 | 山东国瓷功能材料股份有限公司 | A kind of synthetic method of SSZ-13 molecular sieve |
CN109569320B (en) * | 2018-12-26 | 2020-11-17 | 福州宇卓科技有限公司 | Method for preparing pure-phase SSZ-13 molecular sieve membrane by mixed crystal seed method |
CN109665545B (en) * | 2019-02-14 | 2022-07-01 | 正大能源材料(大连)有限公司 | Synthesis method of morphology-controllable SSZ-13 molecular sieve |
CN110156610B (en) * | 2019-05-22 | 2021-12-24 | 无锡威孚环保催化剂有限公司 | Method for recovering template from SSZ-13 molecular sieve synthesis waste liquid |
CN110357121B (en) * | 2019-08-02 | 2022-09-09 | 太原理工大学 | Preparation method of small-grain nano hierarchical pore SSZ-13 molecular sieve |
CN112939020B (en) * | 2021-04-09 | 2023-09-29 | 南京诚志清洁能源有限公司 | Stepped crystallization preparation method and application of Cu-SSZ-13 molecular sieve catalyst |
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US8007763B2 (en) * | 2006-09-25 | 2011-08-30 | Chevron U.S.A. Inc. | Preparation of molecular sieves using a structure directing agent and an N,N,N-trialkyl benzyl quaternary ammonium cation |
CN105312083B (en) * | 2014-07-29 | 2019-03-08 | 南京开丽环保材料有限公司 | CHA type sial phosphorus molecular sieve and its preparation method and application |
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Denomination of invention: A preparation method of SSZ-13 molecular sieve Effective date of registration: 20220606 Granted publication date: 20180306 Pledgee: Shandong Zhoucun Rural Commercial Bank Co.,Ltd. Pledgor: SHANDONG QILU HUAXIN HIGH-TECH Co.,Ltd. Registration number: Y2022980007075 |
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Date of cancellation: 20230509 Granted publication date: 20180306 Pledgee: Shandong Zhoucun Rural Commercial Bank Co.,Ltd. Pledgor: SHANDONG QILU HUAXIN HIGH-TECH Co.,Ltd. Registration number: Y2022980007075 |