Preparation method of ZSM-11 molecular sieve

A technology of ZSM-11 and molecular sieve, which is applied in the field of preparation of ZSM-11 molecular sieve, can solve the problems of low production efficiency, low crystallinity, and long crystallization time, and achieve the effect of reducing synthesis cost and shortening crystallization time

Active Publication Date: 2012-05-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process of the above method is relatively complicated, and generally the crystallinity is not high in a relatively short period of time, and there are miscellaneous crystals
It takes a long time for crystallization to prepare ZSM-11 molecular sieve with no miscellaneous crystals, high crystallinity and high conversion rate, which has high energy consumption and low production efficiency

Method used

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  • Preparation method of ZSM-11 molecular sieve
  • Preparation method of ZSM-11 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Weigh 1.8g sodium hydroxide and 5.0g tetrabutylammonium bromide and dissolve in 50.0ml deionized water, then add 7.5g EU-1 molecular sieve while stirring at room temperature, stir for 0.5 hours, then add 5.0g white carbon black , After stirring for 0.5 hours, move to a closed stainless steel reaction kettle. Crystallize at 140°C for 48 hours to obtain ZSM-11 molecular sieve.

[0015] Proportion: 0.3Na 2 O: 1.1SiO 2 : 0.10 (TBA) 2 O: 100EU-1(g): 37H 2 O.

Embodiment 2

[0017] Weigh 1.6g of sodium hydroxide and 6.0g of tetrabutylammonium bromide and dissolve them in 50.0ml of deionized water, then add 5.0g of EU-1 molecular sieve while stirring at room temperature, stir for 0.5 hours, then add 5.0g of white carbon black, After stirring for 0.5 hours, move to a closed stainless steel reaction kettle. Crystallize at 140°C for 48 hours to obtain ZSM-11 molecular sieve.

[0018] Proportion: 0.40Na 2 O: 1.6SiO 2 :0.17(TBA) 2 O: 100EU-1(g): 55H 2 O.

Embodiment 3

[0020] Weigh 1.6g of sodium hydroxide and 6.0g of tetrabutylammonium bromide and dissolve them in 50.0ml of deionized water, then add 5.0g of EU-1 molecular sieve while stirring at room temperature, stir for 0.5 hours, then add 8.0g of white carbon black, After stirring for 0.5 hours, move to a closed stainless steel reaction kettle. Crystallize at 150°C for 36 hours to obtain ZSM-11 molecular sieve.

[0021] Proportion: 0.40Na 2 O: 2.7SiO 2 :0.17(TBA) 2 O: 100EU-1(g): 55H 2 O.

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Abstract

The invention relates to a preparation method of a ZSM-11 molecular sieve. The method comprises steps of: using an EU-1 molecular sieve as a seed; adding an EU-1 molecular sieve powder into a solution containing sodium hydroxide and a template; stirring uniformly and adding a silicon source to obtain a reaction mixture gel system, wherein a molar ratio of other components needed to be added into the reaction mixture gel system for per 100g of EU-1 molecular sieve seed is as below: 0-0.5 Na2O:0.8-5.0 SiO2:0.1-0.5 (TBA)2O:100(g)EU-1:20-110 H2O; crystallizing the reaction mixture gel under an enclosed condition at 120-180 DEG C for 36-72 h to obtain the ZSM-11 molecular sieve. Compared with a prior art, the invention has shortened crystallization time and reduced synthesis cost.

Description

technical field [0001] The invention relates to a synthesis technology of molecular sieves, in particular to a preparation technology of ZSM-11 molecular sieves. Background technique [0002] ZSM-11 molecular sieve is a molecular sieve with a MEL-type skeleton structure. Its all-silicon form of molecular sieve is Silicalite-2. It can be used as an inert carrier for shape-selective catalysts and a separation membrane material for organic-water phases, and has attracted widespread attention. [0003] In 1973 ChuP (USP3,709,979) used Bu 4 N + As a template agent, ZSM-11 molecular sieve was successfully synthesized. In 1978, Flanigen E M of U.C.C. Company successfully synthesized the last member of the Pentasil family, all-silicon ZSM-11-Silicalite-2, which in turn promoted the rapid development of the field of silica-rich zeolite synthesis. . In 1990, Mc William (USP4,894,212) et al. used octylamine as a template, and crystallized at 100-350°C for 12 hours-10 days by adding ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36
Inventor 秦波张喜文张志智
Owner CHINA PETROLEUM & CHEM CORP
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