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Beta/ZSM-5 compound borosilicate molecular sieve and preparation method thereof

A technology of ZSM-5 and molecular sieves, which is applied in the field of composite molecular sieves and its preparation, can solve the problems of difficult diffusion of products and inaccessibility of heavy components, and achieve high reactivity, selectivity of aromatics, and good thermal and hydrothermal stability.

Active Publication Date: 2012-03-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

However, due to its structure and pore size limitations, heavy components cannot enter this molecular sieve, and the products in some reactions are not easy to diffuse out.

Method used

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  • Beta/ZSM-5 compound borosilicate molecular sieve and preparation method thereof

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preparation example Construction

[0012] The preparation method of the composite borosilicate molecular sieve provided by the invention comprises adding β borosilicate molecular sieve as a crystal seed into the reaction mixture for synthesizing ZSM-5 borosilicate molecular sieve, and then performing hydrothermal crystallization.

[0013] The molar ratio of each substance contained in the reaction mixture is (0~0.05) boron source: silicon source: (0~0.2) inorganic base: (0.01~0.15) templating agent: (10~40) water, preferably ( 0.01-0.03) boron source: silicon source: (0.03-0.1) inorganic base: (0.04-0.1) templating agent: (15-25) water. Mix the boron source, silicon source, inorganic base, templating agent, water and β molecular sieve as the seed crystal evenly, carry out hydrothermal crystallization in a closed reactor and recover the product, wherein the boron contained in the boron source compound is B 2 o 3 The silicon contained in the silicon source compound is represented by SiO 2 count.

[0014] In t...

example 1

[0028] 0.64g of borax, 0.4g of NaOH, 4.88g of tetraethylammonium hydroxide solution with a concentration of 25% by mass and 52ml of deionized water were mixed evenly, and 1 g of the β borosilicate molecular sieve prepared in Comparative Example 1 was added under stirring as a seed crystal. After stirring until uniform, add 10g of solid silica gel, stir vigorously, age at 25°C for 2 hours, then transfer to a reaction kettle, crystallize at 140°C for 5 days, and then quickly cool to 30°C. The product is centrifuged and washed until the pH value is 8-9. The obtained solid was dried at 100° C. for 12 hours to obtain a composite borosilicate molecular sieve c whose crystal phase was β / ZSM-5, and its anhydrous chemical composition (calculated by oxide molar ratio) was: 0.5 Na 2 O·B 2 o 3 ·55SiO2 2 , in the composite molecular sieve, the β molecular sieve accounts for 5.4% by mass, and the ZSM-5 molecular sieve accounts for 94.6% by mass. The moles and crystallization conditions o...

example 2

[0030] Mix 0.64g of borax, 0.4g of NaOH, 4.88g of tetraethylammonium hydroxide solution with a concentration of 25% by mass and 52ml of deionized water evenly, add 2g of the β borosilicate molecular sieve prepared in Comparative Example 1 as a seed crystal under stirring, and stir After uniformity, add 10g of solid silica gel, stir vigorously, age at 25°C for 2 hours, then transfer to a reaction kettle, crystallize at 140°C for 5 days, and then quickly cool to 30°C. The product is centrifuged and washed until the pH value is 8-9. The solid was dried at 80°C for 10 hours to obtain a composite borosilicate molecular sieve d with a crystalline phase of β / ZSM-5, and its anhydrous chemical composition (based on the molar ratio of oxides) was: 0.5Na 2 O·B 2 o 3 48SiO2 2 , XRD spectrum see figure 1, in the composite molecular sieve, β molecular sieve accounts for 9% by mass, and ZSM-5 molecular sieve accounts for 91% by mass. The moles and crystallization conditions of each react...

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Abstract

The invention relates to a beta / ZSM-5 compound borosilicate molecular sieve. Non-water chemical constitution expression of the molecular sieve is: xNa2O.B2O3.ySiO2, wherein, x is 0.03-2 and y is 10-400. The molecular sieve is prepared by adding beta borosilicate molecular sieve, which is taken as inoculating seed, to synthetic materials of the ZSM-5 compound borosilicate molecular sieve by hydrothermal crystallization; therefore, the molecular sieve has strong acidic property and high aromatization performance.

Description

technical field [0001] The invention relates to a composite molecular sieve and a preparation method thereof, in particular to a composite borosilicate molecular sieve and a preparation method thereof. Background technique [0002] Borosilicate molecular sieve is a kind of silicon-aluminum heteroatom molecular sieve, that is, a molecular sieve in which the aluminum on the framework of the silicon-alumina molecular sieve is completely replaced by boron atoms. The acidity of borosilicate molecular sieves is significantly lower than that of silica-alumina molecular sieves, and the acidity of molecular sieves can be adjusted by changing the Si / B ratio, showing special catalytic performance for the catalytic conversion of alkanes. Taramasso et al. (Proceedings of Fifth International conference on Zeolites, 40-49, London, 1980) reported for the first time the synthesis of ZSM-5 borosilicate molecular sieves using tetrapropylammonium hydroxide as a template. Van der Waal et al. (J...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/86B01J29/80
Inventor 王嘉欣马爱增张大庆陈志祥臧高山张玉红
Owner CHINA PETROLEUM & CHEM CORP
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