Ti-Si molecular sieve modifying method

A titanium-silicon molecular sieve and molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problem of poor activity and stability of TS-1 molecular sieves, which restricts the industrial application of TS-1 molecular sieves, and is difficult to stabilize Obtain problems such as TS-1 molecular sieve, 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: 2004-09-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 good catalytic oxidation activity, the active stability of gained TS-1 molecular sieve is relatively poor, therefore restricts TS-1 Industrial Application of Molecular Sieve

Method used

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Embodiment 1

[0031] Tetraethyl orthosilicate, tetrapropylammonium hydroxide and distilled water were uniformly mixed in a molar ratio of 1:0.06:155.60, and hydrolyzed at normal pressure and 25° C. for 25 minutes to obtain a hydrolysis solution of tetraethyl orthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 and mix it evenly with the hydrolysis solution of tetraethyl orthosilicate mentioned above according to the ratio of molecular sieve (g): Si (mol) = 426.68: 1, stir and disperse at normal pressure and temperature for 2 hours , to obtain a homogeneous dispersion. The dispersion was put into a sealed stainless steel reaction kettle, 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 until the pH value is 6-8, and calcined at 550° C. for 3 hours to obtain the silicon-modified TS-1 molecular sieve of the present invention.

Embodiment 2

[0033] Tetrapropyl orthosilicate, tetraethylammonium hydroxide and distilled water were uniformly mixed at a molar ratio of 1:0.45:215.10, and hydrolyzed at normal pressure and 30° C. for 60 minutes to obtain a hydrolysis solution of tetrapropyl orthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 and mix it uniformly with the hydrolysis solution of tetrapropyl orthosilicate mentioned above according to the ratio of molecular sieve (g): Si (mol) = 125.34: 1, and stir and disperse at normal pressure and 50°C for 1 hour , to obtain a homogeneous dispersion. The dispersion was put into a sealed stainless steel reaction kettle, 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 until the pH is 6-8, and calcined at 550° C. for 3 hours to obtain the silicon-modified TS-1 molecular sieve of the present invention.

Embodiment 3

[0035] Tetrapropyl orthosilicate, tetrapropylammonium hydroxide and distilled water were uniformly mixed at a 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 tetrapropyl orthosilicate. Take the TS-1 molecular sieve obtained in Comparative Example 1 and mix it uniformly with the hydrolysis solution of tetrapropyl orthosilicate mentioned above according to the ratio of molecular sieve (g): Si (mol) = 143.55: 1, and stir and disperse at normal pressure and 55°C for 1.5 hours , to obtain a homogeneous dispersion. The dispersion was put into a sealed stainless steel reaction kettle, and kept 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 until the pH is 6-8, and calcined at 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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Patent Type & Authority Patents(China)
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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