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Preparation method of TS-1 titanium silicalite

A titanium-silicon molecular sieve, TS-1 technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of long hydrothermal crystallization time, poor experiment repeatability, complex reaction system, etc., and achieve easy control of particle size and low cost , The effect of simplifying the reaction system

Active Publication Date: 2015-12-30
BEIJING RISUN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] In the method for preparing TS-1 molecular sieve in the prior art, there are still problems such as complex reaction system, expensive template agent, long hydrothermal crystallization time, and poor repeatability of experiments.

Method used

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  • Preparation method of TS-1 titanium silicalite
  • Preparation method of TS-1 titanium silicalite
  • Preparation method of TS-1 titanium silicalite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] Organic silicon source and organic titanium source are TEOS and TEOT respectively

[0045] first hydrolysis

[0046] SiO in Si source in proportion (molar ratio) 2 : TiO in titanium source 2 : Template agent: H 2 O is 1:0.05:0.22:25, prepare the reaction mixture solution: first add TEOT to TEOS and mix evenly, slowly add the mixed solution of TEOS and TEOT to the template agent under vigorous stirring: H 2 O ratio of 0.22:25 (SiO 2 The molar ratio is 1) in the diluted TPAOH aqueous solution. After all the dropwise addition, the reaction mixture was hydrolyzed at 35°C for 5 hours;

[0047] second step alcohol

[0048] After hydrolyzing the titanium silicon treated in the previous step, the temperature of the reaction mixture solution was raised to 80°C, and the alcohol was removed for 4 hours. According to the calculation, deionized water was added dropwise during the alcohol removal process to ensure that the concentration of the template agent in the reaction mix...

Embodiment 2

[0055] Organic silicon source and organic titanium source are TEOS and TEOT respectively

[0056] first hydrolysis

[0057] SiO in Si source in proportion (molar ratio) 2 : TiO in titanium source 2 : Template agent: H 2 O is 1:0.04:0.25:20, prepare the reaction mixture solution: first add TEOT to TEOS and mix evenly, slowly add the mixed solution of TEOS and TEOT to the template agent under vigorous stirring: H 2 O ratio of 0.25:20 (SiO 2 The molar ratio is 1) in the diluted TPAOH aqueous solution. After all the dropwise addition, the reaction mixture was hydrolyzed at 45°C for 3 hours;

[0058] second step alcohol

[0059] Heat up the reaction mixture solution after hydrolyzing the titanium silicon treated in the previous step to 75°C, and chase the alcohol for 5 hours. According to the calculation, add deionized water dropwise during the alcohol chase to ensure that the concentration of the template agent in the reaction mixture solution is basically unchanged. In ter...

Embodiment 3

[0066] The organic silicon source and the organic titanium source are tetrabutyl orthosilicate and tetrabutyl titanate (TBOT), respectively.

[0067] first hydrolysis

[0068] SiO in Si source in proportion (molar ratio) 2 : TiO in titanium source 2 : Template agent: H 2 O is 1:0.04:0.245:19, prepare the reaction mixture solution: first add TBOT to tetrabutyl orthosilicate and mix evenly, slowly add the mixed solution of TBOT and tetrabutyl orthosilicate to the template under vigorous stirring Agent:H 2 O ratio of 0.245:19 (SiO 2 The molar ratio is 1) in the diluted TPAOH aqueous solution. After all the dropwise addition, the reaction mixture was hydrolyzed at 60°C for 3 hours;

[0069] second step alcohol

[0070] After hydrolyzing the titanium silicon treated in the previous step, the temperature of the reaction mixture solution was raised to 90°C, and the alcohol was removed for 4 hours. According to the calculation, deionized water was added dropwise during the alco...

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Abstract

The invention relates to a preparation method of titanium silicalite and the titanium silicalite prepared by the method. A TS-1 titanium silicalite crystal is prepared from an organic silicon source, an organic titanium source, an organic base template agent and water as raw materials through the steps of hydrolysis, alcoholization, hydrothermal crystallization, washing, roasting and the like; and the form of the TS-1 titanium silicalite crystal can be controlled by adjusting the concentration of the organic base template agent TPAOH in a hydrothermal crystallization reaction mixture and the concentration change in the process of alcoholization. The method has the advantages of easiness in control of process conditions, good repeatability, simple hydrothermal synthesis system ingredients, easiness in separation of hydrolysis products, and the like. The particle size of a TS-1 molecular catalyst prepared by the method provided by the invention is easy to control, and the TS-1 molecular catalyst is in a 'blackberry' form and has a favorable catalytic oxidation function; and in oximation reaction, for example, reaction for preparing cyclohexanone oxime through cyclohexanone ammoximation, the selectivity and catalytic activity of reaction products are obviously increased.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical synthesis, and in particular relates to a preparation method of a titanium-silicon molecular sieve, that is, a TS-1 titanium-silicon molecular sieve. Background technique [0002] TS-1 molecular sieve is a new catalytic material with a unique MFI topology developed in the early 1980s. It is a heteroatom zeolite molecular sieve in which silicon atoms in the framework are partially replaced by titanium atoms. Among them, titanium atoms are evenly distributed in the skeleton to form a skeleton Si-O-Ti bond with special properties, which has a three-dimensional channel structure represented by ZSM-5, which is formed by a zigzag channel and an intersecting elliptical straight channel. composition. In the mid-1980s, it was successfully developed by the Italian company Enichem and applied in the industrial production of caprolactam intermediate - cyclohexanone oxime in 1994. TS-1 can catalyz...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 杨雪岗张新志郑云张敏生王先鹏宋艾罗苏思正王福帅
Owner BEIJING RISUN TECH CO LTD
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