Method for in-situ crystallized synthesis of small-grain ZSM-5 molecular sieve by using direct method

A ZSM-5, chemical synthesis technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbonane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of high cost, template pollution of the environment, long crystallization time and other problems

Active Publication Date: 2013-08-21
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In the above-mentioned patents or documents, the relative crystallinity of ZSM-5 molecular sieve synthesized by template method in situ crystallization is relatively high, but the template itself is expensive, and it will pollute the environment during the post-treatment process of removing the template. In addition, in industrial production The template agent is often removed by high-temperature calcination, which requires energy consumption. Therefore, the use of the template agent will greatly increase the cost of in-situ crystallization catalyst generation, which should be avoided as much as possible; the other type in the above-mentioned patents or documents does not use The method of in-situ crystalliz

Method used

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  • Method for in-situ crystallized synthesis of small-grain ZSM-5 molecular sieve by using direct method
  • Method for in-situ crystallized synthesis of small-grain ZSM-5 molecular sieve by using direct method
  • Method for in-situ crystallized synthesis of small-grain ZSM-5 molecular sieve by using direct method

Examples

Experimental program
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Effect test

Embodiment 1

[0073] Preparation of kaolin microspheres:

[0074] 3071g of kaolin, 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%. Kaolin microspheres were analyzed by IR, at 550cm -1 There is a characteristic vibrational absorption peak of the five-membered ring nearby.

[0075] In situ crystallization ZSM-5 molecular sieve:

[0076] Weigh 30.0g of roasted kaolin microspheres and 131.1g of distilled water in a beaker, put the beaker in a 90°C water bath, and stir for 5 minutes; add 111.1g of water glass to the beaker, and stir for 20h; then add 131.1g of distilled water, and stir for 10min, Slowly add 36.1g of 3M sulfuric acid solution to the system to adjust the alkalinity...

Embodiment 2

[0079] Preparation of kaolin microspheres:

[0080] 2752g of kaolin, 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%. Kaolin microspheres were analyzed by IR, at 550cm -1 There is a characteristic vibrational absorption peak of the five-membered ring nearby.

[0081] In situ crystallization ZSM-5 molecular sieve:

[0082] Weigh 30.0g of roasted kaolin microspheres and 300.0g of distilled water in a beaker, put the beaker in a 60°C water bath, and stir for 5 minutes; add 282.0g of water glass into the beaker, and stir for 20h; then add 300.0g of distilled water, and stir for 10min, Slowly add 59.0 g of 3M sulfuric acid solution to the system to adjust the alk...

Embodiment 3

[0085] Preparation of kaolin microspheres:

[0086] 3012g of kaolin, 780g of water glass and 6206g 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 41.2wt%, active Al 2 o 3 Content 5.7wt%. Kaolin microspheres were analyzed by IR, at 550cm -1 There is a characteristic vibrational absorption peak of the five-membered ring nearby.

[0087] In situ crystallization ZSM-5 molecular sieve:

[0088] Weigh 30.0g of roasted kaolin microspheres and 55.0g of distilled water in a beaker, put the beaker in a 70°C water bath, and stir for 5 minutes; add 70.0g of water glass to the beaker, and stir for 24 hours; then add 55.0g of distilled water, and stir for 10 minutes, Slowly add 24.0 g of 3M sulfuric acid solution to the system to adjust the...

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Abstract

The invention provides a method of crystallized preparation of a ZSM-5 molecular sieve in-situ by using a direct method without a template. The method comprises pre-treating high-temperature-roasted kaolin microspheres containing a characteristic structural unit of a five-membered ring by using sodium silicate, adding acid to prepare a reaction mixture, and performing hydrothermal crystallization to obtain in-situ products containing the ZSM-5 molecular sieve and ex-situ ZSM-5 molecular sieve. The kaolin microsphere in-situ crystallized ZSM-5 molecular sieve has a relative crystallinity being capable of being adjusted within 65 % according to requirements, has a crystal size being 0.1-3 [mu]m, is good in wear resistance performance and can be used as a catalytic addictive for increasing propylene yield in a FCC technology. The co-produced ex-situ ZSM-5 molecular sieve has a crystallinity being more than 90 %, and a crystal size of 0.1-3 [mu]m, and can be used for preparing a semi-synthetic catalyst.

Description

technical field [0001] The invention relates to a method for synthesizing small-grain ZSM-5 molecular sieves through direct method and in-situ crystallization of kaolin microspheres as raw materials. Background technique [0002] Due to its unique three-dimensional pore structure, good hydrothermal stability and excellent shape-selective catalytic performance, ZSM-5 molecular sieve is introduced into FCC catalysts to increase the octane number of gasoline and increase the production of low-carbon olefins. [0003] There are generally two ways to introduce active components in FCC catalysts. One is to mix active components with matrix and binder to make slurry, and prepare microsphere catalysts through spray drying, roasting and other procedures, which are called semi-synthetic catalysts. The second is to prepare microspheres by spraying kaolin first, and after roasting, the molecular sieve active component is grown on the kaolin microspheres by hydrothermal crystallization u...

Claims

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Application Information

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IPC IPC(8): C01B39/38
Inventor 申宝剑孙兵高雄厚赵红娟郝坤秦松张君屹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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