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Method for in situ synthesis of titanium-silicon molecular sieve material containing noble metal

A titanium-silicon molecular sieve and in-situ synthesis technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low effective utilization rate, poor stability, low catalyst activity, etc., and achieve improved synergy, good dispersion, and selectivity and the effect of improving catalytic activity and stability

Active Publication Date: 2012-01-25
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

[0028] Tetraethyl orthosilicate, tetrabutyl titanate and Tween 80 are added to the tetrapropylammonium hydroxide aqueous solution containing palladium acetate and stirred and mixed evenly, wherein the molar composition is silicon source: titanium source: alkali source: palladium source: Protective agent: water=100:0.03:0.5:0.2:0.02:550, 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, filter it, dry it, and roast it to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above remaining filtrate, add hydrazine hydrate equimolar to the above palladium source, and then perform hydrothermal treatment at a temperature of 170° C. and autogenous pressure for 36 hours, filter the resultant, wash with water, and dry naturally. And conti...

Embodiment 2

[0030] Add tetraethyl orthosilicate, tetrabutyl titanate and sodium dodecylbenzenesulfonate to tetrapropylammonium hydroxide aqueous solution containing palladium ammonium chloride and stir to mix evenly, wherein the molar composition is silicon source: titanium source : alkali source: palladium source: protective agent: water=100:2.0:5.2:0.5:0.6:2500, 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 96 hours, take out the resultant, filter it, dry it, and roast it to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above remaining filtrate, add hydrazine hydrochloride twice as much as the above palladium source (mole), and then hydrothermally treat it at a temperature of 120° C. under autogenous pressure for 48 hours, filter the result...

Embodiment 3

[0032] Tetraethyl orthosilicate, tetrabutyl titanate and Tween 80 are added to the tetrapropylammonium hydroxide aqueous solution containing palladium acetate and stirred and mixed evenly, wherein the molar composition is silicon source: titanium source: alkali source: palladium source: Protective agent: 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, filter it, dry it, and roast it to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above remaining filtrate, add hydrazine hydrate 5 times the mole of the above palladium source, and then perform hydrothermal treatment at a temperature of 170°C and autogenous pressure for 36 hours, filter the resultant, wash with water, and dry naturally , and ...

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Abstract

The invention provides a method for in situ synthesis of a titanium-silicon molecular sieve material containing a noble metal. The method is characterized by comprising: adding a titanium source, a silicon source and a protectant to an aqueous solution of an alkali source containing a noble metal source and evenly mixing; putting the mixed solution in a closed reactor for reaction at a temperature of between 120 and 200 DEG C and at a self elevating pressure for at least half an hour; filtering, drying and roasting the product to obtain an intermediate crystalline state material; mixing the intermediate crystalline state material and the filtrate obtained after the product is filtered, and adding a reducer to the mixed solution; and putting the mixed solution in a closed reaction kettle for treatment at a temperature of between 80 and 200 DEG C and under a self elevating pressure for 2 to 360 hours, and recovering the product. By the method, the synergetic effect of the noble metal and the titanium-silicon molecular sieves is improved; and compared with the prior art, when the titanium-silicon molecular sieve material synthesized by the method is used for oxidizing reactions such as a reaction of preparing propylene oxide by epoxidation of propylene, the selectivity, the catalytic activity and the stability of the reaction product are obviously improved.

Description

technical field [0001] The invention relates to a method for preparing a microporous titanium-silicon material, in particular to a method for preparing a microporous titanium-silicon material containing precious 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 s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
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