Preparation method for precious-metal-containing titanium silicalite material

A titanium silicalite and precious metal technology, which is applied in the field of preparation of precious metal-containing titanium silicalite materials, can solve problems such as the need to be improved in activity and activity stability, and achieve good catalytic activity stability, good dispersibility and stability, and synergistic effect. improved effect

Active Publication Date: 2012-07-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it still needs to be improved in terms of activity and activity stability

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add tetrapropylammonium hydroxide aqueous solution containing palladium acetate and Tween 80 into tetraethyl orthosilicate and tetrabutyl titanate mixture and stir well, wherein the molar composition is silicon source: titanium source: protective agent: organic Alkali: 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 add hydrazine hydrate equimolar to the above-mentioned palladium source, then transfer the result to a stainless steel sealed reactor for hydrothermal treatment at a temperature of 170°C and autogenous pressure for 36 hours, take out the result and dry it naturally at room temperature until the water content is less than 10 % by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain noble metal-containing titanium-silicon material A. The X-ray diffraction spectrum of the material has the spectrum ...

Embodiment 2

[0036] Add the tetrapropylammonium hydroxide aqueous solution containing palladium ammonium chloride and Span 60 into the mixed solution of tetraethyl orthosilicate and tetrabutyl titanate and stir well, wherein the molar composition is silicon source: titanium source: protective 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 add 2 times the hydrazine hydrochloride with the above-mentioned palladium source (mole), then transfer the result to a stainless steel sealed reaction vessel and treat it for 48 hours at a temperature of 120°C and autogenous pressure, and take out the result and dry it naturally at room temperature to the water content Less than 10% by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain the noble metal-containing titanium-silicon material B. The X-ray diffraction spec...

Embodiment 3

[0038] A mixed aqueous solution of tetrapropylammonium hydroxide and triethanolamine containing palladium nitrate and cyclodextrin was added to tetraethyl orthosilicate and TiCl 4 Stir and mix in the mixed solution, wherein the molar composition silicon source: titanium source: protective agent: organic base (the molar ratio of tetrapropyl ammonium hydroxide and triethanolamine is 1): palladium source: water=100: 0.03: 0.5: 0.05 :0.02:550, 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 hydrazine hydrate equimolar to the above-mentioned palladium source, then transfer the result to a stainless steel sealed reaction kettle for 36 hours at a temperature of 100°C and autogenous pressure, take out the result and let it dry naturally at room temperature until the water content is less than 10 % by weight, washed with water, filtered, dried at 150°C, and calcined at 550°C for 3 hours to obtain the noble metal-c...

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PUM

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Abstract

The invention relates to a preparation method for a precious-metal-containing titanium silicalite material, which is characterized in that alkali source aqueous solution containing a precious metal source and protective agent is added first into titanium source and silicon source mixed liquid and is evenly agitated, reducing agent is added and is evenly mixed, and then the mixture is transferred to a reactor for hydro-thermal treatment; and the obtained product after the hydro-thermal treatment is naturally dried first and is washed, and then the washed product is dried again and is sintered.Compared with the prior art, the catalytic oxidization activity and the activity stability of the prepared precious-metal-containing titanium silicalite material in oxidization reaction are obviouslyimproved.

Description

technical field [0001] The invention relates to a preparation method of a titanium-silicon material, in particular to a preparation method of a noble metal-containing titanium silicalite material. 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 molec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89B01J37/16B01J37/10B01J37/04C07B33/00
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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