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Method for in situ synthesizing titanium silicon materials containing noble metal

An in-situ synthesis, precious metal technology, applied in non-metallic elements, chemical instruments and methods, molecular sieves and alkali exchange compounds, etc., can solve the problems of low effective utilization, poor stability, low catalyst activity, etc. Improved synergy and good dispersibility

Active Publication Date: 2012-12-12
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

[0023] Mix tetraethyl orthosilicate and tetrabutyl titanate and add them into tetrapropylammonium hydroxide aqueous solution containing palladium acetate, stir and mix evenly, wherein the molar composition is silicon source: titanium source: alkali source: palladium source: water =100:0.1:0.2:0.02:600, silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then add hydrazine hydrate equimolar to the above-mentioned palladium source to the mixture, and then hydrothermally treat it in a sealed reaction vessel at a temperature of 170°C and autogenous pressure for 36 hours, filter the resultant, wash with water, and dry it naturally at a temperature of 550°C. Calcined at lower temperature for 3 hours, the noble metal-containing titanium-silicon material A was obtained. The X-ray diffraction spectrum of the material has the spectrum characteristics of TS-1 molecular sieve.

Embodiment 2

[0025] Mix tetraethyl orthosilicate and tetrabutyl titanate and add them into tetrapropylammonium hydroxide aqueous solution containing ammonium chloride palladium, stir and mix evenly, wherein the molar composition is silicon source: titanium source: alkali source: palladium source : water = 100: 1.0: 2.2: 1.0: 1500, silicon source is SiO 2 In terms of titanium source as TiO 2In terms of palladium source in terms of Pd. Then add 2 times the hydrazine hydrochloride with the above-mentioned palladium source (mole) to the mixture and then hydrothermally treat it in a sealed reactor at a temperature of 120°C and autogenous pressure for 144 hours, filter the resultant, wash with water, and dry naturally at 550 ℃ for 3 hours to obtain the noble metal-containing titanium-silicon material B. The X-ray diffraction spectrum of the material has the spectrum characteristics of TS-1 molecular sieve.

Embodiment 3

[0027] Tetraethyl orthosilicate and TiCl 4 After mixing, add to the mixed aqueous solution of tetrapropylammonium hydroxide and butanediamine containing palladium nitrate and stir and mix evenly, wherein the molar composition silicon source: titanium source: alkali source (tetrapropylammonium hydroxide and butanediamine The molar ratio is 1): palladium source: water = 100: 0.03: 0.5: 0.05: 250, the silicon source is SiO 2 In terms of titanium source as TiO 2 In terms of palladium source in terms of Pd. Then add 4 times the hydrazine hydrate of the above-mentioned palladium source (mole) to the mixture and then hydrothermally treat it in a sealed reactor at a temperature of 170°C and autogenous pressure for 6 hours, filter the resultant, wash with water, and dry naturally at 550 °C for 3 hours to obtain the noble metal-containing titanium-silicon material C. The X-ray diffraction spectrum of the material has the spectrum characteristics of TS-1 molecular sieve.

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Abstract

The invention relates to a method for in situ synthesizing titanium silicon materials containing noble metal, which is characterized by comprising the following steps: firstly, adding a titanium source and a silicon source into alkali source water solution containing a noble metal source to be uniformly mixed after the titanium source and the silicon source are uniformly mixed; and secondly, adding reducing agent, carrying out hydrothermal treatment in a reactor, and recovering the products. The method ensures that the synergistic effect of the noble metal and a titanium silicon molecular sieve is enhanced and obviously enhances the selectivity, the catalytic activity and the stability of the reaction products in oxidation reaction i.e. reaction for preparing propylene oxide through propylene epoxidation compared with the prior art.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-silicon molecular sieve material, in particular to a method for synthesizing a titanium-silicon molecular sieve 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...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/00
Inventor 林民史春风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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