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Method for synthesizing heteroatom Sn-beta zeolite

A heteroatom and beta zeolite technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolite, molecular sieve catalyst, etc., can solve the problems of difficult stirring, high preparation cost, pollution, etc., and achieve easy recovery and recycling, and improve The effect of mechanical stirring performance and high-efficiency catalytic effect

Inactive Publication Date: 2011-11-23
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The method used in this document has the following disadvantages: it needs to use strong acid for dealumination, and the pollution is serious; the crystallization time is long and the process is complicated; the use of expensive tetraethyl orthosilicate as the silicon source makes the preparation cost high and it is difficult to industrialize
However, this method has the following disadvantages in the process of Sn-β synthesis: in the process of preparing seed crystals, concentrated nitric acid needs to be used for dealumination, which causes serious pollution and corrosion; the synthesis is carried out in the HF system, which is highly toxic and volatile. Cause environmental pollution; due to the low water content in the synthesis system, serious gelation, difficult stirring, and difficulty in industrialization

Method used

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  • Method for synthesizing heteroatom Sn-beta zeolite
  • Method for synthesizing heteroatom Sn-beta zeolite

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Embodiment 1

[0026] The initial molar ratio of heteroatom Sn-β zeolite synthesis is as follows: 1SiO 2 / 0.002SnO 2 / 0.6TEAOH / 0.6NH 4 F / 6.5H 2 O / 0.5EtOH, the specific synthesis process is as follows: 18g of white carbon black was added to 66.28g of tetraethylammonium hydroxide solution (TEAOH 40wt%), and stirred for about 2 hours until the white carbon black was completely dissolved. After dissolving 0.215g of tin tetrachloride pentahydrate in 0.5g of deionized water, it was added dropwise to the above-mentioned glue solution, and then 10ml of ethanol solution was added to the above-mentioned synthetic solution. After stirring for 1 hour, a solution formed by dissolving 6.66g of ammonium fluoride in 2.5g of deionized water and 5ml of ethanol was added, stirred vigorously, and a viscous gel was formed after about 30 minutes. The above gel was transferred into a small stainless steel synthesis kettle for static crystallization at 100°C. After 10 days, it was taken out and cooled, filtered...

Embodiment 2

[0028] The initial molar ratio of heteroatom Sn-β zeolite synthesis is as follows: 1SiO 2 / 0.002SnO 2 / 0.6TEAOH / 0.6NH 4 F / 6.5H 2 O / 0.5EtOH, the specific synthesis process is as follows: 18g of white carbon black was added to 66.28g of tetraethylammonium hydroxide solution (TEAOH 40wt%), and stirred for about 2 hours until the white carbon black was completely dissolved. After dissolving 0.215g of tin tetrachloride pentahydrate in 0.5g of deionized water, it was added dropwise to the above-mentioned glue solution, and then 10ml of ethanol solution was added to the above-mentioned synthetic solution. After stirring for 1 hour, a solution formed by dissolving 6.66g of ammonium fluoride in 2.5g of deionized water and 5ml of ethanol was added, stirred vigorously, and a viscous gel was formed after about 30 minutes. The above gel was transferred into a small stainless steel synthesis kettle for static crystallization at 180°C. After 10 days, it was taken out and cooled, filtered...

Embodiment 3

[0030] The initial molar ratio of heteroatom Sn-β zeolite synthesis is as follows: 1SiO 2 / 0.002SnO 2 / 0.6TEAOH / 0.6NH 4 F / 6.5H 2 O / 0.5EtOH, the specific synthesis process is as follows: 18g of white carbon black was added to 66.28g of tetraethylammonium hydroxide solution (TEAOH 40wt%), and stirred for about 2 hours until the white carbon black was completely dissolved. After dissolving 0.215g of tin tetrachloride pentahydrate in 0.5g of deionized water, it was added dropwise to the above-mentioned glue solution, and then 10ml of ethanol solution was added to the above-mentioned synthetic solution. After stirring for 1 hour, a solution formed by dissolving 6.66g of ammonium fluoride in 2.5g of deionized water and 5ml of ethanol was added, stirred vigorously, and a viscous gel was formed after about 30 minutes. The above gel was transferred into a small stainless steel synthesis kettle for static crystallization at 140°C. After 10 days, it was taken out and cooled, filtered...

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Abstract

The invention belongs to the technical field of catalytic chemistry, and relates to a method for preparing a heteroatom Sn-beta zeolite molecular sieve. The method is characterized by comprising the following steps of: stirring a silicon source, tetraethyl ammonium hydroxide, a tin source, water and ethanol serving as a solvent in a ratio to form initial gel; adding fluoride serving as a mineralizing agent to form a viscose system, and crystallizing at the temperature of between 100 and 180 DEG C for 3 to 10 days to hydrothermally synthesize a Sn-heteroatom molecular sieve with a beta structure. The molecular sieve is synthesized in a neutral or subacid synthesis system under the conditions that a crystal seed is not added, relatively cheap white carbon black is taken as the silicon source, and ammonium fluoride meeting the environment-friendly requirement is taken as the mineralizing agent. The synthesis system has low water content, absolute ethanol serving as an auxiliary agent is added to reduce the viscosity of the synthesis system, convenience is provided for stirring, and the requirement on large-scale industrial production is well met. The method is low in cost, environment-friendly, simple, and easy to industrialize.

Description

technical field [0001] A method for synthesizing heteroatom Sn-beta zeolite of the invention belongs to the technical field of catalytic chemistry. Specifically relates to a preparation technology of a zeolite molecular sieve with high catalytic activity for Baeyer-Villiger reaction. Background technique [0002] Beta zeolite is the only microporous high-silica molecular sieve with a three-dimensional twelve-membered ring intersection channel structure. It was obtained by hydrothermal synthesis (USP308069) by Mobile Company in tetraethylammonium hydroxide strong alkali system in 1967. Due to its special BEA topology, good thermal and hydrothermal stability, acid catalytic activity and structural selectivity, it shows excellent performance in catalysis and adsorption. It has been widely used in petroleum refining and petrochemical engineering such as catalytic cracking, alkylation, esterification, isomerization, disproportionation and reforming. [0003] After the β zeolit...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/78B01J37/00
Inventor 张雄福康自华刘海鸥邱介山
Owner DALIAN UNIV OF TECH
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