Preparation method for titanium silicalite molecular sieve and applications

A technology of titanium-silicon molecular sieve and silicon source, applied in the direction of molecular sieve catalysts, chemical instruments and methods, crystalline aluminosilicate zeolites, etc., can solve the problems of increasing catalyst costs, wasting gold, and catalyst deactivation

Active Publication Date: 2013-11-20
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this system, although the traditional titanium silicate molecular sieve (TS-1) has stronger hydrophobicity compared with other supports, it can promote the desorption of the product propylene oxide and improve the stability and activity of the catalyst, but the catalyst still has significant The inactivation problem of (Document 1: J.Catal.2012,287,178–189)
Although there are recent reports on the preparation of highly stable supported gold catalysts using solid-state grinding, the catalysts require the use of expensive precursors, and this preparation method cannot selectively deposit gold particles near the active site titanium of titanium-silicon molecular sieves. , a part of the gold was wasted, and the cost of the catalyst was also invisibly increased (Document 2: Appl. Catal. B: Environ. 2010, 95, 430–438)

Method used

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  • Preparation method for titanium silicalite molecular sieve and applications
  • Preparation method for titanium silicalite molecular sieve and applications
  • Preparation method for titanium silicalite molecular sieve and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of Ti-Si Molecular Sieve TS-1 with Micropores Blocked by Template Agent

[0064] Take 1.5g of Tween-20 and 25g of deionized water in a beaker and mix and stir to obtain a mixed solution 1. Take 66g of ethyl orthosilicate and 26g of tetrapropylammonium hydroxide into solution 1 and stir for 30 minutes to obtain mixed solution 2. 20 mL of isopropanol and 0.22 g of n-butyl titanate were mixed and stirred for 1 hour to obtain a mixed solution 3. Solution 3 was added to solution 2 at a rate of 0.5 ml / min and stirred for 1 hour to obtain solution A. The mixed solution A was dealcoholized at 80°C for 2 hours. The solution after alcohol removal was placed in an autoclave, crystallized at 160°C for 18 hours, taken out, washed and dried.

Embodiment 2

[0066] Preparation of Ti-Si Molecular Sieve TS-1 with Micropores Blocked by Template Agent

[0067] Take 10g of Tween-20 and 100g of deionized water in a beaker and mix and stir to obtain a mixed solution 1. Take 66g of ethyl orthosilicate and 52g of tetrapropylammonium hydroxide into solution 1 and stir for 30 minutes to obtain mixed solution 2. 20 mL of isopropanol and 3.08 g of n-butyl titanate were mixed and stirred for 1 hour to obtain a mixed solution 3 . Solution 3 was added to solution 2 at a rate of 0.1 ml / min and stirred for 1 hour to obtain solution A. The mixed solution A was dealcoholized at 80°C for 6 hours. The solution after alcohol removal was placed in an autoclave, crystallized at 180 degrees for 48 hours, taken out, washed and dried.

Embodiment 3

[0069] Get 0.5g of the carrier in Example 1 and place it in a 250mL beaker, add 10mL concentration of chloroauric acid solution of 0.001mol / L to it, stir for 30 minutes, adjust the pH to 7 with 1mol / L sodium hydroxide, and age for 6 hours; after centrifugation and washing, the catalyst was vacuum-dried overnight at 30°C to obtain a catalyst with a low loading of 0.1%.

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Abstract

The invention discloses a titanium silicalite molecular sieve, a preparation method therefor and applications. The titanium silicalite molecular sieve is uncalcined titanium silicalite molecular sieve TS-1. The invention also discloses a new catalyst applied to systems of direct preparation of epoxypropane from propylene through gas-phase epoxidation. The catalyst employs the uncalcined titanium silicalite molecular sieve TS-1 as a carrier and loads the carrier with metal particles.

Description

technical field [0001] The invention relates to a catalyst, in particular to a titanium-silicon molecular sieve TS-1 whose micropores are blocked, a preparation method thereof and the use of the propylene oxide system in the direct gas-phase epoxidation of propylene. Background technique [0002] Propylene oxide (PO) is an important chemical intermediate and the third largest organic chemical product in propylene derivatives after polypropylene and acrylonitrile. It is widely used in the production of polyether, propylene glycol, polyurethane, etc., and is also the main raw material of the fourth-generation detergent non-ionic surfactant, oilfield demulsifier, pesticide emulsifier, etc., and has broad development prospects. At present, the main methods of producing PO in industry are chlorohydrin method and co-oxidation method. However, the chlorohydrin method produces a large amount of waste water and chlorine-containing by-products in the production process, and is highly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07D303/04C07D301/08
CPCY02P20/52
Inventor 周兴贵冯翔段学志钱刚陈文尧
Owner EAST CHINA UNIV OF SCI & TECH
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