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Method for preparing precious metal-containing titanium silicalite

A technology for titanium silicalite and precious metal, applied in the field of preparing precious metal-containing titanium silicalite, can solve the problems such as the need to be improved in activity and activity stability, and achieve the effects of overcoming the aggregation of precious metals, good dispersibility and stability, and improved synergy.

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

[0036] 20 grams of titanium-silicon molecular sieve TS-1 and ammonium nitrate palladium complex are added to the tetrapropylammonium hydroxide aqueous solution containing cetyltrimethylammonium bromide and hydrazine hydrate and stirred uniformly, wherein titanium-silicon molecular sieve ( Gram): cetyltrimethylammonium bromide (mole): tetrapropylammonium hydroxide (mole): hydrazine hydrate (mole): ammonium nitrate palladium complex (gram, in palladium): water (gram )=100:0.2:0.05:0.05:0.02:650. 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, dry it naturally at room temperature until the water content is less than 10% by weight, wash with water, filter, and then dry it at 150°C , and calcined at 450°C for 3 hours to obtain noble metal-containing titanium silicalite material A. Its 960cm -1 Absorption peak at and 550cm -1 Absorption peak intensity ratio I...

Embodiment 2

[0038] 20 grams of titanium-silicon molecular sieve TS-1 and palladium chloride are added to the aqueous sodium hydroxide solution containing polyvinylpyrrolidone and hydrazine hydrochloride and stirred evenly, wherein titanium-silicon molecular sieve (gram): polyvinylpyrrolidone (mol): sodium hydroxide (mol): hydrazine hydrochloride (mol): palladium chloride (gram, calculated as palladium): water (gram) = 100: 0.01: 1.5: 0.5: 4.0: 3500. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 180°C and autogenous pressure for 24 hours, take out the resultant, dry it naturally at room temperature until the water content is less than 10% by weight, wash with water, filter, and then dry it at 150°C , and calcined at a temperature of 550° C. for 3 hours to obtain the noble metal-containing titanium silicalite material B. Its 960cm -1 Absorption peak at and 550cm -1 Absorption peak intensity ratio I 960 / I 550 The data are listed i...

Embodiment 3

[0040] 20 grams of titanium-silicon molecular sieve TS-1 and ammonium chloride palladium complex are added to the aqueous urea solution containing tetradecyltrimethylammonium bromide and hydrazine hydrate and stirred evenly, wherein titanium-silicon molecular sieve (gram): ten Tetraalkyltrimethylammonium bromide (mol): urea (mol): hydrazine hydrate (mol): ammonium chloride palladium complex (gram, in palladium): water (gram)=100: 0.04: 1.0: 0.5:1.0:1200. Then put it into a stainless steel sealed reaction kettle, hydrothermally treat it at a temperature of 120°C and autogenous pressure for 144 hours, take out the resultant, dry it naturally at room temperature until the water content is less than 10% by weight, wash with water, filter, and then dry it at 150°C , and calcined at 580° C. for 3 hours to obtain the noble metal-containing titanium silicalite material C. Its 960cm -1 Absorption peak at and 550cm -1 Absorption peak intensity ratio I 960 / I 550 The data are listed...

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PUM

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Abstract

The invention discloses a method for preparing precious metal-containing titanium silicalite. The method comprises the following processes of: adding a titanium silicalite and a precious metal source into alkali source aqueous solution which contains a protective agent and a reducing agent for mixing uniformly; performing hydro-thermal treatment, and naturally drying, washing and filtering a product; and afterdrying and roasting the product. Compared with the prior art, the catalytic oxidative activity and the activity stability of the precious metal-containing titanium silicalite prepared bythe method are both improved obviously in an oxidizing reaction.

Description

technical field [0001] The invention relates to a method for modifying a titanium-silicon molecular sieve, in particular to a method for modifying a titanium-silicon molecular sieve with a noble metal compound to prepare a noble metal-containing titanium silicalite. 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 effe...

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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