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Method for treating titanium-silicon molecular sieve

A titanium-silicon molecular sieve, the said technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor activity stability, not easy to TS-1 molecular sieve, low effective titanium content, etc., to achieve volume utilization and improve environmental protection efficiency , the effect of improving production efficiency

Active Publication Date: 2012-01-11
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The problem with the synthesis technology of the above-mentioned TS-1 molecular sieve is that the effective titanium content entering the molecular sieve framework is low, and it is not easy to stably obtain a TS-1 molecular sieve with good catalytic oxidation activity, and the activity stability is poor

Method used

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  • Method for treating titanium-silicon molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Mix measured tetraethyl orthosilicate and tetraethylammonium hydroxide, add distilled water, mix well, stir at room temperature for 1.0 hour, and then stir at 75°C for 3 hours to obtain a modified solution, which consists of silicon (mol ): titanium (mol): organic base (mol): water (mol) = 1: 0: 0.85: 20 (where silicon and titanium are SiO 2 and TiO 2 count)). Take 12 grams of the TS-1 molecular sieve obtained above and mix with 10 grams of the modifying liquid evenly. The above mixture was charged into a 50 ml polytetrafluoroethylene liner and placed in a 100 ml polytetrafluoroethylene liner, and then reacted in a sealed autoclave at 175° C. for 12 hours.

[0032] The obtained product was dried at 150° C. for 120 minutes, and then calcined at 580° C. for 5 hours to obtain modified TS-1 molecular sieve A.

Embodiment 2

[0034] Mix measured amount of amorphous silica gel with tetrapropylammonium hydroxide, add distilled water, mix well, stir at room temperature for 1.5 hours, then add n-butyl titanate and stir for 0.5 hours, then stir at 70°C for 3 hours to obtain modified Liquid, its composition is silicon (mol): titanium (mol): organic base (mol): water (mol) = 1: 0.02: 0.75: 25 (where silicon and titanium are SiO 2 and TiO 2 count)). Take 10 grams of the TS-1 molecular sieve obtained above and mix with 8.5 grams of the modified liquid evenly. The mixture was charged into a 50 ml polytetrafluoroethylene liner, then placed in a 100 ml polytetrafluoroethylene liner, and then reacted at 180° C. for 24 hours in a sealed autoclave.

[0035] The obtained product was dried at 150° C. for 120 minutes, and then calcined at 650° C. for 2 hours to obtain modified TS-1 molecular sieve B.

Embodiment 3

[0037] Mix measured tetraethyl orthosilicate, tetraethyl titanate and tetrapropylammonium hydroxide, add distilled water, mix well, stir at room temperature for 1.0 hour, and then stir at 80°C for 3 hours to obtain a modified solution. Its composition is silicon (mol): titanium (mol): organic base (mol): water (mol) = 1: 0.02: 0.75: 35 (where silicon and titanium are SiO 2 and TiO 2 count)). Take 15 grams of the above-obtained TS-1 molecular sieve and mix with 13 grams of modifying liquid evenly. The mixture was charged into a 50 ml polytetrafluoroethylene liner and placed in a 100 ml polytetrafluoroethylene liner, and then reacted at 160° C. for 62 hours in a sealed autoclave.

[0038] The obtained product was dried at 135° C. for 240 minutes, and then calcined at 560° C. for 3 hours to obtain modified TS-1 molecular sieve C.

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Abstract

The invention relates to a method for treating a titanium-silicon molecular sieve. The method is characterized by modifying the titanium-silicon molecular sieve by a modifying solution in the presence of saturated steam, wherein the modifying solution is obtained by hydrolyzing a silicon source and a titanium source in a base solution. According to the method, mother liquor separation is not required, the filtration and washing procedures are omitted, pollution to environment is reduced greatly, the volume utilization efficiency of a high-pressure device is improved, the preparation cost is lowered, and the environmental protection and economic benefits of synthesis are improved.

Description

technical field [0001] The invention relates to a method for treating titanium-silicon molecular sieves, in particular to a method for treating titanium-silicon molecular sieves under water vapor. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, TS-1 with MFI structure, TS-2 with MEL structure, and Ti-MWW with larger pore structure have been synthesized. This type of molecular sieve has excellent selective oxidation performance and high catalytic activity for many organic oxidation reactions, such as epoxidation of olefins, hydroxylation of aromatic hydrocarbons, oximation of cyclohexanone, and oxidation of alcohols. -ox) type molecular sieve catalysts have good application prospects. [0003] TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing transition metal element titanium ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 龙立华林民舒兴田朱斌史春风慕旭宏罗一斌邹飞艳夏长久汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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