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Method for preparing hierarchical porous titanium silicalite TS-1

A technology of titanium silicalite, TS-1, applied in the field of preparation of multi-level porous titanium silicalite TS-1, to achieve the effect of reducing synthesis cost, simplifying the preparation process, and eliminating cumbersome processes

Inactive Publication Date: 2011-02-02
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method omits the preparation of carbon templates, it still requires the synthesis of carbon-silicon composites first.

Method used

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  • Method for preparing hierarchical porous titanium silicalite TS-1
  • Method for preparing hierarchical porous titanium silicalite TS-1

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Get 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (weight 30%) of silica sol, and add successively in 8.4g (weight 50%) of caramel solution; take 0.16ml of tetrabutyl titanate solution In 1.6ml of isopropanol (volume ratio is 1:10), mix well and slowly drop into the above solution, the molar ratio composition of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate 0.24:36.5:1:0.02, caramel and silica sol (SiO 2 The mass ratio of 3:1; the resulting mixture was heated to 80° C. and stirred for 2 h; then the mixture was placed at 170° C. for 28 h to obtain a black solid dry glue. Grind the dry glue into powder and put it in the container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; put the crystallization kettle at 170°C for 7d. After washing, filtering and drying the obtained solid, it was calcined at 650° C. for 10 h to obtain the multi-level channel TS-1. In...

Embodiment 2

[0026] Get 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (30% by weight) of silica sol, and add successively in 2.8g (50% by weight) of caramel solution; In 1.6ml of isopropanol (volume ratio is 1:10), mix well and slowly drop into the above solution, the molar ratio composition of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate 0.24:30:1:0.02, caramel and silica sol (based on SiO 2 The mass ratio of 1:1; the resulting mixture was heated to 80° C. and stirred for 2 h; then the mixture was placed at 170° C. for 24 h to obtain a black solid dry glue. Grind the dry glue into powder and put it in the container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; put the crystallization kettle at 170°C for 7d. After washing, filtering and drying the obtained solid, it was calcined at 650° C. for 10 h to obtain the multi-level channel TS-1.

Embodiment 3

[0028] Get 1.5g of tetrapropylammonium bromide, 8ml of deionized water and 3.9ml (30% by weight) of silica sol, and add successively in 5.6g (50% by weight) of caramel solution; In 1.6ml of isopropanol (volume ratio is 1:10), mix well and slowly drop into the above solution, the molar ratio composition of tetrapropylammonium bromide, deionized water, silica sol and tetrabutyl titanate 0.24:33.3:1:0.02, caramel and silica sol (SiO 2 The mass ratio of 2:1; the resulting mixture was heated to 80° C. and stirred for 2 h; then the mixture was placed at 170° C. for 36 h to obtain a black solid dry glue. Grind the dry glue into powder and put it in the container in the middle of the crystallization kettle, add 9ml of ethylenediamine and 12ml of water at the bottom; put the crystallization kettle at 170°C for 7d. After washing, filtering and drying the obtained solid, it was calcined at 650° C. for 10 h to obtain the multi-level channel TS-1.

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Abstract

The invention discloses a method for preparing hierarchical porous titanium silicalite TS-1, which is characterized in that: carbon black is replaced by cheap sugar, and materials such as carbon nanotubes and the like are used as a mesoporous / macroporous template, so the synthesis cost of a molecular sieve is greatly reduced. In the process of preparing dry glue by performing heat treatment on sugar-containing TS-1 molecular sieve synthetic sol, the sugar is heated and part of sugar is carbonized and dehydrated to directly form a hard template, so that high-temperature carbonization under the protection of inert gas is avoided, the complicated process of separately preparing a carbon template and a carbon-silicon complex is saved, and the preparation process of a hierarchical porous zeolite molecular sieve is greatly simplified. The product prepared by the method has the advantages of regular shape and microporous channel of the conventional TS-1, mesopores of 4 to 50nm and macropores of more than 50nm which pass through zeolite, and mutually communicated hierarchical porous channels to overcome the limitation of inherent micropores of the zeolite on catalytic reaction, and can be used for olefin epoxidation, aromatic hydrocarbon hydroxylation, cyclohexanone ammoxidation, oxidation removal of different sizes of sulfides in liquid fuel, and the like.

Description

technical field [0001] The invention relates to a method for preparing a multi-level porous titanium silicalite TS-1. Background technique [0002] Zeolite molecular sieve refers to a kind of microporous crystal of hydrated silicate (including natural and synthetic), which has the characteristics of regular and orderly pore structure, large pore volume and specific surface area, and is widely used in petrochemical, It plays an increasingly important role in many fields such as fine chemical industry, oil and natural gas processing and refining, gas adsorption and separation, environmental protection and so on. [0003] In 1983, the US patent USP 4410501 reported the titanium silicalite molecular sieve TS-1 for the first time. Since the transition metal titanium has a variable valence state, the introduction of titanium endows TS-1 with unique catalytic oxidation properties. With TS-1 as catalyst, H 2 o 2 It is an oxidant reaction system with mild reaction conditions, hig...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 李钢王维海
Owner DALIAN UNIV OF TECH
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