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Titanium-silicon molecular sieve/tripolite composite catalyst and preparation

A technology of titanium-silicon molecular sieves and composite catalysts, which is applied in molecular sieve catalysts, physical/chemical process catalysts, organic chemical methods, etc., can solve the problems of high use cost, difficult separation, small particles, etc., and achieve easy operation control and improved catalytic performance , the effect of mild reaction conditions

Inactive Publication Date: 2008-09-17
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to overcome the problems of small particles, high cost of use and difficult separation in industrial applications of conventional titanium-silicon molecular sieves, it can also significantly improve the diffusion of reactants and products in the pores of the catalyst, and increase the reaction rate and product selectivity.

Method used

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  • Titanium-silicon molecular sieve/tripolite composite catalyst and preparation
  • Titanium-silicon molecular sieve/tripolite composite catalyst and preparation
  • Titanium-silicon molecular sieve/tripolite composite catalyst and preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Put 10g of diatomaceous earth in a 100mL Erlenmeyer flask, add 100mL of 40% sulfuric acid, install a reflux device at the mouth of the bottle, heat it to 80°C in a water bath, keep it warm for 4 hours, cool to room temperature, and titrate to the pH value with 20% sodium hydroxide solution for 10. Continue to heat up to 90°C, keep warm for 0.5h, then cool to room temperature, wash with deionized water until neutral, then wash with 100mL absolute ethanol, filter, dry the filter cake in an oven at 110°C for 14h, The heating rate of h was raised from room temperature to 1000°C and kept at this temperature for 4h.

[0028] Mix 3.6g of TS-1 and 5.4g of treated diatomaceous earth evenly, press into tablets, and crush to 20-40 mesh. The hydroxylation reaction of phenol is carried out in a fixed-bed glass reactor with an inner diameter of 15mm, and the amount of catalyst is 7g. It is placed in the constant temperature section of the reactor, and both ends are closed with broke...

Embodiment 2

[0030]The difference from Example 1 is that the calcination time of diatomaceous earth at 1000° C. is extended to 12 hours, and other conditions are the same as in Example 1. Catalyst evaluation conditions are shown in Example 1, and reaction evaluation results are shown in Table 1.

Embodiment 3

[0032] The difference from Example 1 is that the chemically treated diatomaceous earth is not subjected to roasting heat treatment after drying, and other conditions are the same as in Example 1. Catalyst evaluation conditions are shown in Example 1, and reaction evaluation results are shown in Table 1.

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Abstract

The invention discloses a Ti-Si molecular sieve / diatomite composite catalyst and a preparation method thereof, which is characterized in that: the catalyst is formed by compounding Ti-Si molecular sieve (such as TS-1 and TS-2) and diatomite with particular chemical property which is treated in a particular way, and is modified chemically by transition metal oxide after molding; the preparation method comprises the following steps: (1) after being treated with acid solution and alkaline solution, the diatomite needs heat treatment in high temperature to obtain particular chemical property; (2) the molding Ti-Si molecular sieve / diatomite composite catalyst is modified chemically by transition metal oxide (such as lanthanum and nickel). The composite catalyst can be used as the catalyst of selective oxidation reaction of the organic compound (such as the catalytic hydroxylation reaction of phenol) on fixed bed liquidoid, which uses hydrogen peroxide as the oxidant. The Ti-Si molecular sieve / diatomite composite catalyst has the advantages of high catalytic activity, high stability, long service life and easy separation, recovery and regeneration of the catalyst. When using the catalyst in the hydroxylation reaction of phenol of fixed bed liquidoid, under the reaction conditions of 84 DEG C, atmospheric pressure and 8.46h<-1> space velocity, the conversion rate of phenol is greater than 33%, the selectivity of diphenol reaches 99.9%, and the effective use rate of hydrogen peroxide is greater than 85%.

Description

[0001] The present invention relates to a preparation method of a supported titanium-silicon molecular sieve, more specifically to a preparation method of a titanium-silicon molecular sieve / diatomite composite catalyst, which can be used in a fixed-bed liquid phase with hydrogen peroxide as an oxidant The selective oxidation reaction of organic compounds, such as the catalytic hydroxylation of phenol, not only has high catalytic activity, but also has high stability and long service life, and the catalyst is easy to separate, recover and regenerate. Background technique [0002] Since the advent of ZSM-5 zeolite molecular sieves in the 1970s, molecular sieves containing heteroatoms such as Cr, Ti, Zr, Be, P, and V have been successfully synthesized one after another. Among them, the research on zeolite molecular sieves containing Ti has developed rapidly in recent years. Since Taramasso et al. used tetrapropylammonium hydroxide (TPAOH) as template and tetraethyl titanate as tit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J21/08C07B33/00
CPCY02P20/584
Inventor 卢冠忠杨云飞郭杨龙郭耘王艳芹王筠松张志刚刘晓晖龚学庆
Owner EAST CHINA UNIV OF SCI & TECH
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