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Method for synthesizing TS-1 molecular sieve

A TS-1, molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor oxidation activity and high non-framework titanium content, achieve low synthesis cost, overcome activity decline, Low dosage effect

Active Publication Date: 2011-06-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved in the present invention is to overcome the shortcomings of high non-skeleton titanium content and poor oxidation activity in the TS-1 molecular sieve synthesized by the prior art, and provide a new method for synthesizing titanium-silicon molecular sieve (TS-1)

Method used

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  • Method for synthesizing TS-1 molecular sieve
  • Method for synthesizing TS-1 molecular sieve
  • Method for synthesizing TS-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 120-200 mesh silica gel particles and tetrabutyl titanate to the aqueous solution of tetrapropyl ammonium hydroxide and stir well, wherein the silica gel particles (in the form of SiO 2 In terms of), tetrabutyl titanate (as TiO 2 The mol ratio of tetrapropylammonium hydroxide and water is 1: 0.04: 0.1: 15, and then put into a stainless steel sealed reactor, and hydrothermally treat 4 hours at a temperature of 170° C. under autogenous pressure to obtain mixture a; 40- 80 mesh silica gel particles and tetrabutyl titanate were added to the aqueous solution of tetrapropyl ammonium hydroxide and stirred evenly, wherein the silica gel particles (using SiO 2 In terms of), tetrabutyl titanate (as TiO 2 The molar ratio of tetrapropylammonium hydroxide to water is 1:0.04:0.1:15. After the titanium source is hydrolyzed, add the above-mentioned mixture a and mix evenly, wherein the amount of mixture a accounts for 25% of the total volume after mixing. , and then transferred t...

Embodiment 2

[0041] Add 80-120 mesh silica gel particles and tetrabutyl titanate to the aqueous solution of tetrapropyl ammonium hydroxide and n-butylamine and stir well, wherein the silica gel particles (as SiO 2 In terms of), tetrabutyl titanate (as TiO 2 The molar ratio of tetrapropylammonium hydroxide, n-butylamine and water is 1: 0.01: 0.2: 0.1: 25, then put into a stainless steel sealed reaction kettle, and hydrothermally treat at 160°C for 6 hours under autogenous pressure to obtain Mixture a: 20-40 mesh silica gel particles and tetrabutyl titanate are added to the aqueous solution of tetrapropyl ammonium hydroxide and stirred evenly, wherein the silica gel particles (in the form of SiO 2 In terms of), tetrabutyl titanate (as TiO 2 ), the molar ratio of tetrapropylammonium hydroxide and water is 1:0.08:0.01:15, after the hydrolysis of the titanium source is completed, add the above-mentioned mixture a and mix evenly, wherein the amount of the mixture a accounts for 50% of the total...

Embodiment 3

[0043] First mix 120-160 mesh silica gel particles with TiCl 4 Add to the aqueous solution of tetrapropyl ammonium hydroxide and diethanolamine and mix well, wherein the silica gel particles (as SiO 2 count), TiCl 4 , tetrapropylammonium hydroxide, diethanolamine and water in a mol ratio of 1: 0.08: 0.05: 0.1: 40, then put into a stainless steel sealed reactor, and hydrothermally treat it at a temperature of 150° C. under autogenous pressure for 9 hours to obtain mixture a; Add 10-20 mesh silica gel particles and tetrabutyl titanate into the aqueous solution of tetrapropyl ammonium hydroxide and stir evenly, wherein the silica gel particles (in the form of SiO 2 In terms of), tetrabutyl titanate (as TiO 2 ), the molar ratio of tetrapropylammonium hydroxide and water is 1:0.1:0.1:50, after the hydrolysis of the titanium source is completed, add the above-mentioned mixture a and mix evenly, wherein the amount of the mixture a accounts for 60% of the total volume after mixing ...

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Abstract

A method for synthesizing a TS-1 molecular sieve comprises the steps that: (1) the aqueous solutions of solid silica gel particles, titanium source and organo-alkali compound are mixed and treated with hydro-thermal treatment at 80-180 DEG C for 3-96 hours, wherein, the molar ratio of SiO2: TiO2: organo-alkali compound: water is 1: 0.001-0.5: 0.01-0.5: 5-100; (2) the aqueous solutions of the solid silica gel particles, the titanium source and the organo-alkali compound is mixed until the titanium source are completely hydrolyzed; wherein, the molar ratio of SiO2: TiO2: organo-alkali compound: water is 1: 0.001-0.5: 0.001-0.80: 5-150; (3) the products obtained from step (1) and step (2) are mixed; and crystallization reaction is carried out by a conventional method to recover the product; wherein, the product of step (1) accounts for 10-80 percent. The method of the invention can synthesize the TS-1 molecular sieve with certain granularity, and the synthesized molecular sieve has low content of non-skeleton titanium and has high activity, stability and selectivity when being used in oxidation reaction.

Description

technical field [0001] The invention relates to a method for synthesizing titanium-silicon molecular sieve (TS-1) with MFI structure. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized so far. Among them, TS-1 molecular sieve is a molecular sieve with ZSM-5 structure containing transition metal element titanium in the framework, which has excellent performance in catalytic selective oxidation reaction, excellent stability and shape selection. TS-1 molecular sieve is used in the oxidation reaction of organic matter. It can use non-polluting low-concentration hydrogen peroxide as the oxidant, thereby simplifying the oxidation process and reducing environmental pollution. It has the incomparable advantages of energy saving, economy and environmental friendlines...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08B01J29/89
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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