Ti-Si molecular sieve modifying method

A technology of titanium-silicon molecular sieve and molecular sieve, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the constraints on the industrial application of TS-1 molecular sieves, and it is difficult to obtain TS-1 molecular sieves and TS-1 molecular sieves stably. 1 Poor activity and stability of molecular sieves, etc., to achieve the effect of improving selectivity and activity stability, good catalytic oxidation activity, and increasing the content of titanium in the skeleton

Inactive Publication Date: 2003-06-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The main problem existing in the prior art of above-mentioned synthesizing TS-1 molecular sieve is: it is difficult to stably obtain the TS-1 molecular sieve with go

Method used

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Examples

Experimental program
Comparison scheme
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Example Embodiment

[0030] Example 1

[0031] Tetraethylorthosilicate, tetrapropylammonium hydroxide and distilled water are mixed uniformly according to a molar ratio of 1:0.06:155.60, and hydrolyzed under normal pressure and 25°C for 25 minutes to obtain a hydrolysis solution of tetraethylorthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 according to the ratio of molecular sieve (g): Si (mole) = 426.68:1 and mix with the hydrolysis solution of tetraethylorthosilicate, and stir and disperse for 2 hours under normal pressure and normal temperature. , To obtain a uniform dispersion. The dispersion was put into a stainless steel sealed reactor, and kept at a constant temperature of 165° C. for 24 hours to obtain a mixture containing liquid and solid. The mixture is filtered, washed with water to pH=6-8, and calcined at 550°C for 3 hours to obtain the silicon-modified TS-1 molecular sieve of the present invention.

Example Embodiment

[0032] Example 2

[0033] The tetrapropylorthosilicate, tetraethylammonium hydroxide and distilled water are mixed uniformly according to the molar ratio of 1:0.45:215.10, and hydrolyzed under normal pressure and 30°C for 60 minutes to obtain a hydrolysis solution of tetrapropylorthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 according to the ratio of molecular sieve (g): Si (mole) = 125.34:1 and mix it with the hydrolysis solution of tetrapropylorthosilicate, stir and disperse for 1 hour at normal pressure and 50°C , To obtain a uniform dispersion. The dispersion was put into a stainless steel sealed reactor, and kept at a constant temperature of 175°C for 36 hours to obtain a mixture containing liquid and solid. The mixture is filtered, washed with water to a pH of 6-8, and calcined at a temperature of 550°C for 3 hours to obtain the silicon-modified TS-1 molecular sieve of the present invention.

Example Embodiment

[0034] Example 3

[0035] The tetrapropylorthosilicate, tetrapropylammonium hydroxide and distilled water are mixed uniformly according to the molar ratio of 1:0.28:185.54, and hydrolyzed at normal pressure and 55°C for 20 minutes to obtain a hydrolysis solution of tetrapropylorthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 according to the ratio of molecular sieve (g): Si (mole) = 143.55:1 and mix it with the hydrolysis solution of tetrapropylorthosilicate, stir and disperse for 1.5 hours at normal pressure and 55°C , To obtain a uniform dispersion. The dispersion was put into a stainless steel sealed reactor, and placed at a constant temperature of 165° C. for 5 hours to obtain a mixture containing liquid and solid. The mixture is filtered, washed with water to a pH of 6-8, and calcined at a temperature of 550°C for 3 hours to obtain the silicon-modified TS-1 molecular sieve of the present invention.

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Abstract

The preparation process of modified Ti-Si molecular sieve TS-1 with MFI structure includes mixing water solution of Si and synthesized TS-1 molecular sieve, the reaction of the mixture at 80-190 deg.c in the reactor for 0.1-150 hr, filtering, washing and drying. The modified Ti-Si molecular sieve TS-1 has certain amount of inert component Si covering the surface and pores and less Ti content in the surface and pores and thus less side reaction in the said places, and these results in raised catalytic oxidation activity, prolonged service life and less side product.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve, and more specifically relates to a modification method of a five-membered ring titanium-silicon molecular sieve (TS-1) with an MFI structure. Background technique [0002] Titanium silicate molecular sieve is a new 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. This type of molecular sieve has excellent catalytic activity and directional oxidation performance for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oxidation of cyclohexanone, and oxidation of alcohols. They are used as redox molecular sieves The catalyst has a good application prospect. [0003] TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent directional oxidation catalytic performance ...

Claims

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Application Information

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IPC IPC(8): B01J29/89C01B39/08
Inventor 林民舒兴田汪燮卿朱斌汝迎春王一萌宗保宁
Owner CHINA PETROLEUM & CHEM CORP
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