Titanium silicalite TS-1 catalyst preparation method

A titanium-silicon molecular sieve, TS-1 technology, applied in molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc.

Inactive Publication Date: 2010-07-07
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In order to solve the problems of high cost, complex preparation process, long period, high energy consumption and poor catalytic activity in the prior art, the present invention provides a new method for preparing titanium-silicon molecular sieve TS-1 catalyst, which uses cheap inorganic titanium-silicon raw materials , does not require long-term hydrolysis, only needs a small amount of tetrapropylammonium hydroxide or tetrapropylammonium bromide as a template, and uses an inorganic base such as ammonia water as an alkali source, which overcomes the shortcomings of the prior art and prepares a Low-cost, high-activity, and catalytically stable titanium-silicon molecular sieve TS-1 catalyst

Method used

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  • Titanium silicalite TS-1 catalyst preparation method

Examples

Experimental program
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Embodiment 1

[0047] with H 2 SO 4 -H 2 o 2 Carry out aftertreatment to the TS-1 that obtains by comparative example 1, promptly use H 2 SO 4 (30%) solution and dilute H 2 o 2 (30%) solution was boiled at 80° C. for 2 hours, washed with deionized water until neutral, and dried. Take 10g TPAOH solution and 40gNH 4 HCO 3 Solution, the concentration is 2.5mol / L, add 10g TS-1 and stir slowly for 30min, transfer the reaction solution to an autoclave, and conduct the second crystallization at 170°C for 48 hours, filter, wash, dry, and dry at 550 Calcined at ℃ for 5.5 hours to obtain titanium silicon molecular sieve TS-1 catalyst.

Embodiment 2

[0049] The preparation of TS-1 was carried out according to Comparative Example 1. with H 2 SO 4 -H 2 o 2 Post-processing, that is, using H 2 SO 4 (30%) solution and dilute H 2 o 2 (30%) solution was boiled at 80° C. for 2 hours, washed with deionized water until neutral, and dried. Take 50g of ammonia water, add 10g of TS-1 and stir slowly for 30min, transfer the reaction solution to an autoclave, conduct the second crystallization at 170°C for 48 hours, filter, wash, dry, and roast at 550°C for 5.5 hours A titanium silicate molecular sieve TS-1 catalyst was obtained.

Embodiment 3

[0051] The preparation of TS-1 was carried out according to Comparative Example 1. with H 2 SO 4 -H 2 o 2 Post-processing, that is, using H 2 SO 4 (30%) solution and dilute H 2 o 2 (30%) solution was boiled at 80° C. for 2 hours, washed with deionized water until neutral, and dried. Take 10g2.5mol / L NH 4 HCO 3 Solution and 40g of ammonia water, add 10g of TS-1 and stir slowly for 30min, transfer the reaction solution to an autoclave, and conduct the second crystallization at 170°C for 24 hours, filter, wash, dry, and roast at 550°C for 5.5 Hours to obtain titanium silicon molecular sieve TS-1 catalyst.

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Abstract

The invention discloses a titanium silicalite TS-1 catalyst preparation method. Cheap inorganic Titanium silicalite is used as raw material, low quantity of tetrapropylammonium hydroxide or tetrapropylammonium bromide is adopted as template agent, and inorganic alkali such as ammonia water is used as alkali source so that the raw materials for preparation have low price and the production cost isgreatly reduced. The precursor preparation process is simple and easy to control, seed crystal is added to reduce the crystallization time and the repeatability is good. As secondary crystallization is adopted, the non-framework titanium is further reduced, and the acid site of the molecular sieve is reduced, the grain size is controllable within certain range, the molecular sieve channel becomessmoother to facilitate direct membrane separation of micrometer crystalline grains, and the obtained Titanium silicalite TS-1 catalyst has large grains, high activity, stable catalytic performance and broad industrial application prospect.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon molecular sieve TS-1 catalyst. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the 1980s. It has an MFI structure, referred to as TS-1, a MEL structure called TS-2, and a larger pore structure called TS-48. . In the 1990s, mesoporous TiHMS, TiMCM-41, TiMCM-48, etc. were synthesized. This titanium-silicon molecular sieve has good catalytic activity and directional oxidation performance for many organic oxidation reactions, such as the epoxidation of olefins, the hydroxylation of aromatic hydrocarbons, the oximation of cyclohexanone, and the oxidation of alcohols. Catalytic properties, so it has broad application prospects. [0003] The synthesis method of TS-1 was first disclosed by M. Taramassor et al. in Italy in 1981 (GB2071071A, US4410501). The method comprises firstly preparing a reaction mixture containing...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/00C07C251/44C07C249/04C07D303/08C07D301/12
Inventor 周继承赵虹肖沙黄先亮
Owner XIANGTAN UNIV
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