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Preparation method of titanium-silicon material

A technology of titanium-silicon and silicon sources, which is applied in the field of preparation of titanium-silicon materials containing noble metals, can solve the problems of poor stability, low effective utilization rate, low catalyst activity, etc., and achieve improved synergy, good dispersion, selectivity and catalytic The effect of improving activity and stability

Active Publication Date: 2012-07-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In-situ generation of H by supporting noble metals on titanium-silicon materials 2 o 2 Although the method for the selective oxidation of organic matter has mild conditions and good selectivity (up to 95%), the titanium-silicon material catalysts loaded with noble metals have low activity and poor stability. 2 Low effective utilization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Mix tetraethyl orthosilicate, tetrabutyl titanate and Tween 80 evenly, then add it to tetrapropylammonium hydroxide aqueous solution containing palladium acetate and stir and mix evenly, wherein the molar composition is silicon source: titanium source: protective agent: Organic base: palladium source: water = 100: 0.1: 0.2: 0.02: 0.1: 600, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then put it into a sealed reactor, hydrothermally treat it at a temperature of 120°C and autogenous pressure for 120 hours, take out the resultant and filter it, wash it, dry it, and roast it to obtain an intermediate crystalline material. Mix the intermediate crystalline material with the organic base tetrapropylammonium hydroxide and water according to the ratio of intermediate crystalline material (gram): organic base (mol): water (mol) = 100:0.5:150, and add the above-mentioned palladium at the same time Source equimolar hyd...

Embodiment 2

[0034] Mix tetraethyl orthosilicate, tetrabutyl titanate and Span 60, then add it into tetrapropylammonium hydroxide aqueous solution containing palladium ammonium chloride, stir and mix evenly, wherein the molar composition is silicon source: titanium source: protection Agent: organic base: palladium source: water = 100: 1.0: 0.8: 1.0: 0.2: 1500, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 150°C and autogenous pressure for 48 hours, take out the resultant and filter it, wash it, dry it, and roast it to obtain an intermediate crystalline material. The intermediate crystalline material is mixed with organic base hexamethylenediamine and water according to the ratio of intermediate crystalline material (gram): organic base (mol): water (mol) = 100: 0.1: 100, add 2 times the above-mentioned palladium source ( mol) o...

Embodiment 3

[0036] Tetraethyl orthosilicate, TiCl 4 After mixing with cyclodextrin, add it to the mixed aqueous solution of tetrapropylammonium hydroxide and triethanolamine containing palladium nitrate and stir and mix evenly, wherein the molar composition is silicon source: titanium source: protective agent: organic base (tetrapropyl ammonium hydroxide The molar ratio of ammonium and triethanolamine is 1): palladium source: water = 100: 0.03: 0.5: 0.05: 0.02: 550, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then put it into a sealed reactor, hydrothermally treat it at a temperature of 120°C and autogenous pressure for 120 hours, take out the resultant and filter it, wash it, dry it, and roast it to obtain an intermediate crystalline material. The intermediate crystalline material is mixed with the organic base tetrapropylammonium hydroxide and water according to the ratio of intermediate crystalline material (gram): organic...

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Abstract

The invention relates to a preparation method of a titanium-silicon material. The method comprises the following steps: firstly uniformly mixing a titanium source, a silicon source and a protective agent; adding to an aqueous organic base solution containing noble metal sources to uniformly mix; then, crystallizing to obtain an intermediate crystalline material; mixing the intermediate crystalline material with an organic base and water; carrying out hydrothermal treatment in a reaction kettle at 80-200 DEG C under self-generated pressure for 2-360 hours; and recycling a product. The method improves the synergy of noble metals and a titanium-silicon molecular sieve in the titanium-silicon material. Compared with the prior art, the selectivity, the catalytic activity and the stability of the reaction product are obviously improved in an oxidation reaction, such as a propylene epoxidation reaction for preparing propylene oxide.

Description

technical field [0001] The invention relates to a method for preparing a titanium-silicon material, in particular to a method for preparing a titanium-silicon material containing noble metals. 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, MCM-22 with MWW structure and TS-48 with larger pore structure have been synthesized. Among them, the titanium-silicon molecular sieve TS-1 developed and synthesized by the Italian company Enichem is a new type of titanium-silicon molecular sieve with excellent catalytic selective oxidation performance formed by introducing the transition metal element titanium into the molecular sieve framework with a ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. Using TS-1 molecular...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00
Inventor 史春风林民朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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