Preparation method of titanium silicalite molecular sieve catalyst with high performance

A titanium-silicon molecular sieve and catalyst technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor stability, low catalytic activity and high cost of titanium-silicon molecular sieve catalyst

Active Publication Date: 2013-07-24
SHANGHAI NOVEL CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] What the present invention is to solve is the problem of high cost, low catalytic activity and poor stability of the titanium-silicon molecular sieve catalyst prepared by the prior art. The method of silicon molecular sieve catalyst significantly improves the performance of titanium silicon molecular sieve catalyst in the oximation reaction of cyclohexanone

Method used

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  • Preparation method of titanium silicalite molecular sieve catalyst with high performance
  • Preparation method of titanium silicalite molecular sieve catalyst with high performance
  • Preparation method of titanium silicalite molecular sieve catalyst with high performance

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh 0.2g of sodium hydroxide solid, dissolve it in 100ml of water, and make 0.05mol / L sodium hydroxide alkali treatment solution, add 10g of molecular sieve A1 to it, configure it into a mixed solution with a liquid-solid ratio of 10:1, and mix well Then transfer it to a stainless steel crystallization kettle lined with polytetrafluoroethylene, use hydrothermal crystallization method, treat at 100°C for 12h, filter and wash the product to neutrality, and then dry at 120°C for 4h to obtain a modified titanium-silicon molecular sieve catalyst B1.

Embodiment 2~6

[0023] The preparation process is the same as in Example 1, and the specific raw material ratio and alkali treatment conditions are shown in Table 1. The sample numbers of the obtained alkali-treated modified titanium-silicon molecular sieve catalysts are B2-B6.

Embodiment 7

[0025] 1.1g tetrabutyl titanate (TBOT, TiO 2 wt%>23%), 1.71g tetrapropylammonium bromide (TPABr,>99wt%), 32.1g ammonia solution (NH 3 , 17wt%), 1.45g hydrogen peroxide solution (H 2 o 2 , 27wt%) and 88.4g of water were mixed evenly to form a yellow titanium modified solution, and then 10.0g of alkali-treated titanium-silicon molecular sieve B5 was added, and after stirring at room temperature, it was transferred to a stainless steel crystallization kettle lined with polytetrafluoroethylene to form The molar ratio is titanium source: organic template agent: alkali source: water: silicon dioxide=0.01:0.02:1.0:20:1, hydrogen peroxide: titanium source molar ratio=4:1 crystallization mother liquor, at 170 The secondary modification was carried out under the condition of dynamic stirring at ℃, and the treatment time was 24 hours. The product was filtered, washed, dried and calcined to obtain the modified titanium-silicon molecular sieve catalyst C1.

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Abstract

The invention relates to a preparation method of a titanium silicalite molecular sieve catalyst with high performance. The preparation method comprises the following steps of: (1) by taking a silicon source, a titanium source, an organic template and an alkali source as raw materials, synthesizing a micron-sized titanium silicalite molecular sieve A by using a hydrothermal crystallization method; (2) carrying out modification treatment on the titanium silicalite molecular sieve A by using an alkaline solution to obtain a modified molecular sieve B; and (3) preparing a titaniferous modification solution containing the titanium source, the organic template and the alkali source, and carrying out modification treatment on the modified molecular sieve B to obtain the titanium silicalite molecular sieve catalyst C with high performance. By using the preparation method, the problems that the titanium silicalite molecular sieve catalyst prepared in the prior art is high in cost, low in catalytic activity and poor in stability are mainly solved, and the performance of the titanium silicalite molecular sieve catalyst in cyclohexanone-oxime reaction is remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic materials, and in particular relates to a preparation method of a high-performance titanium-silicon molecular sieve catalyst. Background technique [0002] In 1983, Taramasso et al. of ENI successfully synthesized the titanium-containing molecular sieve catalyst TS-1 for the first time. In recent years, titanium silicate molecular sieves have become one of the fastest growing fields in molecular sieve science. Similar to ZSM-5 molecular sieve, which is widely used at present, titanium silicon molecular sieve also has MFI topology, which is the product of isomorphic substitution of silicon molecular sieve Silicalite-1 by the transition metal titanium with variable valence characteristics, and the general composition is xTiO 2 (1-x)SiO 2 (0.00<x<0.04mol). The molecular sieve is widely used in many fields such as petrochemical industry and fine chemical industry, and has gre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 夏建超夏娟李慧民文怀有谈赟
Owner SHANGHAI NOVEL CHEM TECH
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