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 PDF

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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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molecular sieves
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CN105692647A (en
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刘环昌
明曰信
陈文勇
彭立
周泳冰
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SHANDONG QILU HUAXIN HIGH-TECHNOLOGY Co Ltd
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    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B39/00Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
    • C01B39/02Crystalline 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
    • C01B39/04Crystalline 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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2006/12Surface area

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  • Silicates, Zeolites, And Molecular Sieves (AREA)

Abstract

The invention discloses a kind of preparation method of the molecular sieves of SSZ 13, this method is using supplement crystallization technology, the measure such as organic amine crystallization accelerator and crystal seed of addition, improve the utilization rate of synthesis material, effectively shorten crystallization induction period, the generated time of molecular sieve has been saved, has improved the integrality of molecular sieve crystal;The present invention uses triethylamine or pyridine and the adamantyl ammonium hydroxide of N, N, N trimethyl 1 composition mixed templates, the N of costliness is replaced with triethylamine or pyridine, the adamantyl ammonium hydroxide of N, N trimethyl 1, thus considerably reduce the synthesis cost of the molecular sieves of SSZ 13;Preferred embodiments of the present invention are using sodium tripolyphosphate and guar gum as the waste water in flocculant process filtered fluid, the silicoaluminate contained in mother liquor and template are settled, gained recirculated water can be used for production or directly discharge, and avoid the environmental pollution caused by the directly lower row of filtered fluid causes chemical oxygen consumption of sewage COD and ammonia nitrogen compound exceeded.

Description

A kind of preparation method of SSZ-13 molecular sieves
Technical field
The present invention relates to technical field of molecular sieve, and in particular to a kind of preparation method of SSZ-13 molecular sieves.
Background technology
SSZ-13 molecular sieves are in oil such as air purifying preparation, auto-exhaust catalyst, alkene aromatisation and coal-to-olefin Work field has superior selective catalysis performance, but current preparation technology manufacturing cost is higher, yield is low, synthesis technique is multiple It is miscellaneous to limit it and widely use;On the one hand due to template N, N, the N- front three used in the preparation process of SSZ-13 molecular sieves Base -1- adamantyl ammonium hydroxide is expensive, and on the other hand, the useful constituent in crystallization mother liquor does not obtain effective profit With needing to add excessive silicon source, silicon source and organic formwork agent in building-up process, to promote the realization of crystallization process, therefore Contain substantial amounts of silicoaluminate and template in the filtrated stock after crystallization terminates, this dirty underwater drainage can cause sewage Learn oxygen demand COD and ammonia nitrogen compound severe overweight.
The content of the invention
To solve the above problems, it is an object of the invention to provide a kind of preparation method of SSZ-13 molecular sieves.
The present invention to achieve the above object, is achieved through the following technical solutions:
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
It is well mixed 1. sequentially adding silicon source, silicon source, sodium hydroxide and the first template in water in autoclave, Mixed liquor is obtained, 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 front three Base ammonium bromide, 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;
2. reaction solution is warming up into 115 ~ 125 DEG C to react 9 ~ 10 hours under agitation, 155 ~ 165 DEG C of reactions are then heated to 35 ~ 45 hours, the second template was then added thereto and continues stirring reaction 45 ~ 50 hours, obtains crystallization product;Described Two templates are triethylamine or pyridine;The mol ratio of second template and the first template is 1:2~4;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 500 ~ 600 DEG C of Muffle kiln roastings 4 ~ 6 hours, Obtain SSZ-13 molecular sieves.
Further to realize the purpose of the present invention, following technical scheme can also be used:
Preferably, silicon source is silica gel, Ludox or aerosil;Silicon source is aluminum sulfate or aluminium hydroxide.
Preferably, the second template is triethylamine.
Preferably, to step, 3. gained filtrate adds sodium tripolyphosphate and guar gum, obtains mixed liquor, mixed liquor is stood Sedimentation 10 ~ 12 hours, is separated by filtration, and is precipitated and recirculated water;The mass ratio of the filtrate, sodium tripolyphosphate and guar gum is 190~210:1:2~3。
The preparation method of further preferred SSZ-13 molecular sieves, comprises the following steps:
Mixed 1. sequentially adding silica gel, aluminum sulfate, sodium hydroxide and the first template in water in autoclave It is even, mixed liquor is obtained, SSZ-13 molecular sieves are added into mixed liquor and organic amine promoter is well mixed and obtains reaction solution;It is described The first template be N, N, N- trimethyl -1- adamantyl ammonium hydroxide, described organic amine promoter is cetyl three Methyl bromide ammonium, 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. by reaction solution be warming up to 120 DEG C under agitation react 9 hours, then heat to 160 DEG C react 40 hours, then The second template is added thereto and continues stirring reaction 48 hours, obtains crystallization product;The second described template is triethylamine; The mol ratio of second template and the first template is 1:3;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 550 DEG C of Muffle kiln roastings 5 hours, obtained SSZ-13 molecular sieves.
The advantage of the invention is that:
Present invention uses double template, and N, N, N- trimethyls -1- gold are replaced using cheap triethylamine or pyridine Firm alkyl ammonium hydroxide, the synthesis cost of molecular sieve is greatly reduced, and the second template triethylamine or pyridine are in crystallization Later stage adds, and now the first template is most of in the duct of established SSZ-13 molecular sieves, the template in crystallization system Agent concentration is relatively low, and crystallization motive force dies down.Now, the second template is added, may proceed to keep crystallization motive force, it is superfluous in system Silicon and aluminium can further assemble, and modify the segmental defect of crystal generated, thus, relative crystallinity improves, raw silicon With the utilization rate also relative raising of aluminium;The present invention adds isostructural molecular sieve as crystal seed in the synthetic system of molecular sieve, And the organic amine promoter of quaternary ammonium salt is with the addition of, both additions add the solubility of organic formwork agent in Primogel, Crystallization rate is improved, shortens crystallization induction period, hence it is evident that improves combined coefficient, has saved synthesis cost;It is of the invention preferred Scheme using sodium tripolyphosphate and guar gum as the waste water in flocculant process filtered fluid, the siallitization that will contain in mother liquor Compound and template sedimentation, gained recirculated water can be used for production or directly discharges, avoids filtered fluid and directly descend row to cause sewage Environmental pollution caused by chemical oxygen demand cod and ammonia nitrogen compound are exceeded.
Embodiment
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
It is well mixed 1. sequentially adding silicon source, silicon source, sodium hydroxide and the first template in water in autoclave, Mixed liquor is obtained, 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 front three Base ammonium bromide, 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;
2. reaction solution is warming up into 115 ~ 125 DEG C to react 9 ~ 10 hours under agitation, 155 ~ 165 DEG C of reactions are then heated to 35 ~ 45 hours, the second template was then added thereto and continues stirring reaction 45 ~ 50 hours, obtains crystallization product;Described Two templates are triethylamine or pyridine;The mol ratio of second template and the first template is 1:2~4;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 500 ~ 600 DEG C of Muffle kiln roastings 4 ~ 6 hours, Obtain SSZ-13 molecular sieves.
Further to realize the purpose of the present invention, following technical scheme can also be used:
Preferably, silicon source is silica gel, Ludox or aerosil;Silicon source is aluminum sulfate or aluminium hydroxide.
Preferably, the second template is triethylamine.
Preferably, to step, 3. gained filtrate adds sodium tripolyphosphate and guar gum, obtains mixed liquor, mixed liquor is stood Sedimentation 10 ~ 12 hours, is separated by filtration, and is precipitated and recirculated water;The mass ratio of the filtrate, sodium tripolyphosphate and guar gum is 190~210:1:2~3。
The preparation method of further preferred SSZ-13 molecular sieves, comprises the following steps:
Mixed 1. sequentially adding silica gel, aluminum sulfate, sodium hydroxide and the first template in water in autoclave It is even, mixed liquor is obtained, SSZ-13 molecular sieves are added into mixed liquor and organic amine promoter is well mixed and obtains reaction solution;It is described The first template be N, N, N- trimethyl -1- adamantyl ammonium hydroxide, described organic amine promoter is cetyl three Methyl bromide ammonium, 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. by reaction solution be warming up to 120 DEG C under agitation react 9 hours, then heat to 160 DEG C react 40 hours, then The second template is added thereto and continues stirring reaction 48 hours, obtains crystallization product;The second described template is triethylamine; The mol ratio of second template and the first template is 1:3;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 550 DEG C of Muffle kiln roastings 5 hours, obtained SSZ-13 molecular sieves.
Embodiment 1
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
1. by 60kg Ludox, 6.84kg aluminum sulfate, 8kg sodium hydroxides, the templates of 10.55kg first in autoclave Agent sequentially add in 270kg water be well mixed, obtain mixed liquor, into mixed liquor add 1.27kgSSZ-13 molecular sieves and The organic amine promoters of 2.54kg are well mixed to obtain reaction solution;The first described template is N, N, N- trimethyl -1- adamantane Base ammonium hydroxide, described organic amine promoter are cetyl trimethylammonium bromide;
2. reaction solution is warming up into 115 DEG C to react 9 hours under agitation, then heats to 155 DEG C and react 35 ~ 45 hours, Then the second templates of 2.53kg triethylamine is added thereto and continues stirring reaction 45 hours, obtains crystallization product;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 500 DEG C of Muffle kiln roastings 4 hours, obtained SSZ-13 molecular sieves.
Embodiment 2
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
1. by 60kg silica gel, 6.24kg aluminium hydroxides, 24kg sodium hydroxides and the moulds of 16.88kg first in autoclave Plate agent sequentially add in 540kg water be well mixed, obtain mixed liquor, into mixed liquor add 2.02kgSSZ-13 molecular sieves and The organic amine promoters of 6.06kg are well mixed to obtain reaction solution;The first described template is N, N, N- trimethyl -1- adamantane Base ammonium hydroxide, described organic amine promoter are cetyl trimethylammonium bromide;
2. by reaction solution be warming up to 125 DEG C under agitation react 10 hours, then heat to 165 DEG C react 45 hours, so Add the templates of 1.58kg second thereto afterwards and continue stirring reaction 50 hours, obtain crystallization product;The second described template For pyridine;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 600 DEG C of Muffle kiln roastings 6 hours, obtained SSZ-13 molecular sieves.
Embodiment 3
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
1. in autoclave by 60kg aerosils, 4.68kg aluminium hydroxides, 16kg sodium hydroxides and The templates of 12.66kg first are sequentially added in 360kg water and are well mixed, and are obtained mixed liquor, are added into mixed liquor 1.51kgSSZ-13 molecular sieves and the organic amine promoters of 3.78kg, which are well mixed, obtains reaction solution;The first described template is N, N, N- trimethyl -1- adamantyl ammonium hydroxide, described organic amine promoter are cetyl trimethylammonium bromide;
2. by reaction solution be warming up to 120 DEG C under agitation react 9.5 hours, then heat to 160 DEG C react 40 hours, so Add the templates of 2.02kg second thereto afterwards and continue stirring reaction 48 hours, obtain crystallization product;The second described template For triethylamine;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 580 DEG C of Muffle kiln roastings 5 hours, obtained SSZ-13 molecular sieves;
4. adding 1.81kg sodium tripolyphosphates and 3.63kg guar gums in step 3. gained 345kg filtrates, mixed Liquid, by mixed liquor standing sedimentation 10 hours, it is separated by filtration, is precipitated and recirculated water, gained recirculated water can be directly used for SSZ- The production of 13 molecular sieves.
Embodiment 4
A kind of preparation method of SSZ-13 molecular sieves, comprises the following steps:
1. by 60kg silica gel, 10.26kg aluminum sulfate, 16kg sodium hydroxides and the moulds of 12.66kg first in autoclave Plate agent sequentially add in 450kg water be well mixed, obtain mixed liquor, into mixed liquor add 1.96kgSSZ-13 molecular sieves and The organic amine promoters of 5.88kg are well mixed to obtain reaction solution;The first described template is N, N, N- trimethyl -1- adamantane Base ammonium hydroxide, described organic amine promoter are cetyl trimethylammonium bromide;
2. by reaction solution be warming up to 120 DEG C under agitation react 9 hours, then heat to 160 DEG C react 40 hours, then The templates of 2.02kg second are added thereto and continue stirring reaction 48 hours, obtain crystallization product;The second described template is Triethylamine;
3. by step 2. gained crystallization product be centrifuged, obtain filtrate and filter cake, by gained filter cake through washing, dry SSZ-13 molecular screen primary powders are obtained, gained SSZ-13 molecular screen primary powders are placed in 550 DEG C of Muffle kiln roastings 5 hours, obtained SSZ-13 molecular sieves.
The detection data of the gained SSZ-13 molecular sieves of embodiment 1 ~ 4 are as shown in table 1.
The detection tables of data of the gained SSZ-13 molecular sieves of 1 embodiment of table 1 ~ 4
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)

  1. 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.
  2. 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.
  3. 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.
  4. 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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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

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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Pledgee: Shandong Zhoucun Rural Commercial Bank Co.,Ltd.

Pledgor: SHANDONG QILU HUAXIN HIGH-TECH Co.,Ltd.

Registration number: Y2022980007075