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Method for synthesizing titanium silicon materials containing noble metal

A technology of noble metals and titanium silicon, which is applied in the field of synthesis of titanium silicon materials containing noble metals, can solve the problems of low catalyst activity, poor stability, and low effective utilization rate, and achieve good dispersion, improved synergy, selectivity and catalytic activity and improved stability

Active Publication Date: 2012-07-25
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

[0023] After mixing tetraethyl orthosilicate and tetrabutyl titanate, add them to tetrapropylammonium hydroxide aqueous solution containing palladium acetate and 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 put it into a sealed reactor, hydrothermally treat it at a temperature of 120°C and an autogenous pressure for 120 hours, filter the resultant out (the filtrate is ready for use), wash, dry, and roast to obtain an intermediate crystalline material. Transfer the intermediate crystalline material into the above filtrate, add hydrazine hydrate equimolar to the above palladium source at the same time, then hydrothermally treat it at a temperature of 170°C and autogenous pressure for 36 hours, filter the resultant, wash, dry, and roast to obtain the precious metal-co...

Embodiment 2

[0025]Mix tetraethyl orthosilicate and tetraethyl titanate and add them into tetrapropylammonium hydroxide aqueous solution containing ammonium chloride palladium and stir to 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 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, filter the resultant out (the filtrate is for use), wash, dry, and roast to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above-mentioned filtrate, add 2 times the hydrazine hydrochloride of the above-mentioned palladium source (mole), and then perform a hydrothermal treatment at a temperature of 120° C. and an autogenous pressure for 48 hours, and filter, wash...

Embodiment 3

[0027] Tetraethyl orthosilicate and TiCl 4 After mixing, add it to the tetrapropylammonium hydroxide aqueous solution containing palladium carbonate and stir to mix evenly. The molar composition of silicon source: titanium source: alkali source: palladium source: water = 100: 0.03: 0.5: 0.05: 250, silicon source 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 190°C and an autogenous pressure for 8 hours, filter the resultant (the filtrate is ready for use), take it out, wash, dry, and roast to obtain an intermediate crystalline material. Transfer the intermediate crystalline material to the above-mentioned filtrate, add 4 times the hydroxylamine of the above-mentioned palladium source (mole), then hydrothermally treat it for 36 hours at a temperature of 170°C and autogenous pressure, filter the resultant, wash, dry, and roast to obtain Titanium silicon mate...

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Abstract

The invention relates to a method for synthesizing titanium silicon materials containing noble metal, comprising the following steps: adding a titanium source and a silicon source into alkali source water solution to be uniformly mixed after the titanium source and the silicon source are uniformly mixed; carrying out hydrothermal crystallization for 6-240 hours at temperature of 120 DEG C to 200 DEG C; filtering and separating the crystallization products to obtain filtrate, and recovering the crystallization products to obtain intermediate crystalline materials ; transferring the intermediate crystalline materials into the filtrate, adding reducing agent and processing for 2-360 hours in a closed reactor at temperature of 80-200 DEG C; and recovering the products to obtain the silicon materials containing the noble metal titanium. 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 material, in particular to a method for synthesizing a 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 sieve. Using TS-1 ...

Claims

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Application Information

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