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A kind of method for modification of extruded titanium-silicon molecular sieve

A technology of titanium-silicon molecular sieve and extrusion molding, which is applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of limited diffusion of macromolecules and low titanium content in the outer surface skeleton, and avoid large Molecular diffusion limitation, enhanced catalytic activity, enhanced activity effect

Active Publication Date: 2018-10-19
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to solve the problems of low titanium content in the outer surface of the extruded titanium-silicon molecular sieve TS-1, and the restriction of macromolecular diffusion. The activity of TS-1 in catalyzing macromolecular reactions further expands the application of TS-1

Method used

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  • A kind of method for modification of extruded titanium-silicon molecular sieve
  • A kind of method for modification of extruded titanium-silicon molecular sieve
  • A kind of method for modification of extruded titanium-silicon molecular sieve

Examples

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Effect test

Embodiment 1

[0040] Mix 20g of titanium-silicon molecular sieve TS-1 powder prepared according to Comparative Example 1 of the present invention and 1.0g of starch evenly, add 10g of 25wt% silica sol, stir evenly, and quickly put it into -18°C for 10h in a sealed freezer, take out the freezer The product was thawed at 25°C, put into an extruder to extrude, and then dried and roasted to obtain a strip-shaped titanium-silicon molecular sieve. Add 8.0mL tetrabutyl titanate dropwise into 20mL isopropanol, react at 25°C for 40min, add 5mL 1.2mol / L tetrapropylammonium hydroxide, 67mL water and 7.7g Tween 40 to the solution successively, React at 25°C for 40 minutes to obtain titanium source hydrolyzate; mix 8g of strip-shaped titanium-silicon molecular sieve TS-1 with 70mL of titanium source hydrolyzate, put it in a crystallization kettle, and treat it at 170°C for 48h to separate the solid. Washed, dried, and baked at 550°C for 6h, the obtained sample was designated as TS-1-E.

Embodiment 2

[0042] Mix 20g of titanium-silicon molecular sieve TS-1 powder prepared according to Comparative Example 1 of the present invention and 1.5g of polymethylacrylate evenly, add 20g of 25wt% silica sol, stir evenly, and quickly put it into -18°C for 5h in a sealed freezer , take out the frozen product and thaw it at 30°C, put it into an extruder and extrude it, and then dry and roast it to obtain a strip-shaped titanium-silicon molecular sieve. Add 6.6mL of tetrabutyl titanate dropwise into 20mL of isopropanol, react at 25°C for 30min, add 5.2mL of 1.2mol / L tetrapropylammonium hydroxide, 68mL of water and 10.8g of Tween 20 to the solution successively, React at 25°C for 30 minutes to obtain titanium source hydrolyzate; mix 8g strip-shaped titanium-silicon molecular sieve TS-1 with 60mL titanium source hydrolyzate, put it in a crystallization kettle, treat at 170°C for 60h, separate the solid, and The solid was washed, dried, and calcined at 550°C for 6 hours, and the obtained sam...

Embodiment 3

[0044] Mix 20g of titanium-silicon molecular sieve TS-1 powder prepared according to Comparative Example 1 of the present invention and 2.0g of polyacrylic acid evenly, add 16g of 25wt% silica sol, stir evenly, quickly put it into -4°C and seal and freeze for 24h, take out The frozen product was thawed at 30°C, put into an extruder to extrude into a rod, and then dried and roasted to obtain a strip-shaped titanium-silicon molecular sieve. Add 6.0mL of titanium tetrachloride dropwise into 16mL of isopropanol, react at 25°C for 10min, add 2.2mL of 1.2mol / L tetrapropylammonium hydroxide, 58mL of water and 2.0g of Tween 60 to the solution successively. React at 20°C for 20 minutes to obtain a titanium source hydrolyzate; mix 8g of strip-shaped titanium-silicon molecular sieve TS-1 with 50mL of titanium source hydrolyzate, put it in a crystallization kettle, and treat it at 170°C for 48h to separate the solid. Washed, dried, and baked at 540°C for 5h, the obtained sample was design...

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Abstract

The invention provides a method for modifying an extrusion moulding titanium silicalite molecular sieve. The method comprises the following specific steps: adding a titanium source into an alcohols solvent dropwise, sequentially adding a quaternary ammonium base, water and a protective agent, reacting for 10-60 minutes at the temperature of 20-30 DEG C to obtain a modified solution, mixing the modified solution and a strip titanium silicalite molecular sieve TS-1 obtained through extrusion moulding, putting the mixture in a crystallization kettle, processing for 12-48 hours at the temperature of 100-190 DEG C, separating a solid, washing the solid, and carrying out drying and roasting to obtain the strip titanium silicalite molecular sieve with high titanium content on the outer surface. The method solves the problems that the titanium content of a framework on the outer surface of the extrusion moulding titanium silicalite molecular sieve TS-1 is low and the large molecule is difficult to diffuse, the TS-1 with high titanium content of the framework on the outer surface is prepared, then the diffusion path of a reactant is shortened, the activity of the TS-1 in catalysis of a macromolecule reaction is improved, and the application of the TS-1 is further expanded.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a method for preparing a shaped titanium-silicon molecular sieve which has excellent catalytic performance for selective oxidation of macromolecules and whose outer surface contains relatively high skeleton titanium content. Background technique [0002] Since the synthesis of titanium-silicon molecular sieve TS-1 was first reported in US Patent US4410501 in 1983, its oxidation system with hydrogen peroxide has shown catalytic activity for olefin epoxidation, aromatic hydrocarbon hydroxylation, and ketone ammoxidation. Moreover, the by-product is water, which belongs to an environmentally friendly process, so it has attracted widespread attention. [0003] However, due to the limited pore size (0.56nm×0.53nm) of TS-1 on the diffusion of reactants and products, TS-1 has excellent performance in catalyzing small molecule oxidation reactions (such as propylene epoxidati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89
CPCB01J29/89B01J2229/18
Inventor 左轶郭新闻刘民马梦瞳刘准
Owner DALIAN UNIV OF TECH
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