Method of in-situ crystallized synthesis of ZSM-5/mordenite compound

A technology of ZSM-5 and mordenite, which is applied in the direction of mordenite crystalline aluminosilicate zeolite, crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of long high temperature crystallization time and the like, Achieve the effect of low cost, developed pore structure and large specific surface area

Active Publication Date: 2015-04-29
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] EP0156595 technology mixes clay, silicon-aluminum source and high-silicon molecular sieve seed crystals (such as ZSM series molecular sieves), roasts them at high temperature, and then mixes them with alkali solution to make a mixture that meets the ratio of high-silicon molecular sieves. After low-temperature aging The method of high temperature crystallization has obtained in-situ crystallization products with a high silicon molecular sieve content of up to 60%, but the high temperature crystallization time is as long as 4 days

Method used

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  • Method of in-situ crystallized synthesis of ZSM-5/mordenite compound
  • Method of in-situ crystallized synthesis of ZSM-5/mordenite compound
  • Method of in-situ crystallized synthesis of ZSM-5/mordenite compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Preparation of kaolin microspheres:

[0065] 3071g of kaolin, 199g of ZSM-5 molecular sieve seeds, 536g of water glass and 5002g of distilled water were mixed and beaten, then spray-dried to prepare kaolin microspheres with a particle size of 10-210um. The kaolin microspheres were calcined at 950°C for 2 hours to obtain the calcined kaolin microspheres, the active SiO2 in the calcined kaolin microspheres 2 Content is 40.0wt%, active Al 2 o 3 Content 5.95wt%.

[0066] Synthesis of ZSM-5 / mordenite composite by in situ crystallization:

[0067] (1) Pretreatment of kaolin microspheres: Weigh 30.0g of roasted kaolin microspheres and 161.1g of distilled water in a beaker, put the beaker in a 90°C water bath, stir for 5min; add 111.1g of water glass into the beaker, and stir for 20h ;

[0068] (2) Preparation of the initial reactant: add 161.1g of distilled water to the above mixing system, after stirring for 10min, slowly add 31.1g concentration of 3M sulfuric acid solut...

Embodiment 2

[0072] Preparation of kaolin microspheres:

[0073] 2752g of kaolin, 183g of mordenite seed crystals, 263g of water glass and 4698g of distilled water were mixed and beaten, then spray-dried to prepare kaolin microspheres with a particle size of 10-210um. The kaolin microspheres were calcined at 950°C for 2 hours to obtain the calcined kaolin microspheres, the active SiO2 in the calcined kaolin microspheres 2 The content is 40.2wt%, active Al 2 o 3 Content 5.92wt%.

[0074] Synthesis of ZSM-5 / mordenite composite by in situ crystallization:

[0075] (1) Pretreatment of kaolin microspheres: Weigh 30.0g of roasted kaolin microspheres and 240.0g of distilled water in a beaker, put the beaker in a 60°C water bath, stir for 5min; add 64.2g of water glass into the beaker, and stir for 20h;

[0076] (2) Preparation of the initial reactant: add 240.0g distilled water to the above mixing system, after stirring for 10min, slowly add 10.0g concentration in the system and be 3M sulfuri...

Embodiment 3

[0080] Preparation of kaolin microspheres:

[0081] 3012g of kaolin, 99g of ZSM-5 molecular sieve seed crystals, 100g of mordenite zeolite seeds, 780g of water glass and 6206g of distilled water were mixed and beaten, then spray-dried to produce kaolin microspheres with a particle size of 10-210um. The kaolin microspheres were calcined at 950°C for 2 hours to obtain the calcined kaolin microspheres, the active SiO2 in the calcined kaolin microspheres 2 The content is 41.2wt%, active Al 2 o 3 Content 5.7wt%.

[0082] Synthesis of ZSM-5 / mordenite composite by in situ crystallization:

[0083] (1) Pretreatment of kaolin microspheres: Weigh 30.0g of roasted kaolin microspheres and 155.0g of distilled water in a beaker, put the beaker in a 70°C water bath, stir for 5min; add 92.5g of water glass into the beaker, and stir for 24h;

[0084] (2) Preparation of the initial reactant: add 155.0g distilled water to the above-mentioned mixed system, after stirring for 10min, slowly add...

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Abstract

The invention provides a method of in-situ crystallized synthesis of ZSM-5 / mordenite compound by using a direct method without a template. The method comprises pre-treating high-temperature-roasted kaolin microspheres by using sodium silicate, adding acid to prepare a reaction mixture, and performing hydrothermal crystallization to obtain in-situ products containing the ZSM-5 / mordenite compound and ex-situ ZSM-5 / mordenite composite molecular sieve. The kaolin microsphere in-situ crystallized ZSM-5 / mordenite composite molecular sieve prepared by the invention is relatively high in relative crystallinity of the ZSM-5 / mordenite, wherein the crystallinity can be adjusted according to requirements, is good in wear resistance performance, and can be used to improve propylene yield in a FCC technology. The co-produced ex-situ ZSM-5 / mordenite composite molecular sieve has a crystallinity of the ZSM-5 being more than 80%, and a crystallinity of the mordenite being more than 70 %.

Description

technical field [0001] The invention relates to a method for synthesizing ZSM-5 / mordenite composite by direct method and in-situ crystallization of kaolin microspheres as raw materials. Background technique [0002] In petroleum refining and petrochemical industry, two molecular sieve materials, ZSM-5 molecular sieve and mordenite, are widely used. ZSM-5 molecular sieve has a unique three-dimensional ten-membered ring channel structure, good hydrothermal stability and excellent shape-selective catalytic performance, and is used to increase the production of light olefins in the FCC process. However, the ten-membered ring channel is relatively small, which is not conducive to the occurrence of heavy oil macromolecule cracking reactions, while mordenite has larger twelve-membered ring one-dimensional straight channel channels and a certain acidity, which is conducive to reactants with larger molecular diameters. Diffusion and reaction can effectively make up for the deficienc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/38C01B39/26
Inventor 申宝剑孙兵张君屹赵红娟郝坤秦松高雄厚刘宏海赵晓争郭巧霞李德富袁儒婷王宝杰张莉胡清勋熊晓云
Owner PETROCHINA CO LTD
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