Compound titanium silicon molecular sieve with middle and micro pore, its preparation and use

A silicon molecular sieve and composite titanium technology, which is applied in molecular sieve catalysts, refined hydrocarbon oil, chemical instruments and methods, etc., can solve the problems of long crystallization and harsh synthesis conditions, and achieve mild synthesis conditions, stability and catalytic oxidation ability. , the effect of good catalytic oxidation performance

Inactive Publication Date: 2006-10-11
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the above two molecular sieves need to be crystallized at a relatively high temperature (above 100°C) for a long time (1-10 days) to obtain, and the synthesis conditions are relatively harsh.
[0011] So far, there has been no report on the self-assembly of TS-1 nanoparticles and long-chain alkylamines at room temperature (5-40°C) to prepare mesoporous composite titanium-silicon molecular sieves with microporous molecular sieve structural units in the pore walls.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029]Add 11.2ml of tetraethylsilicate to 25.6ml of tetrapropylammonium hydroxide solution, stir at room temperature for 1-2 hours; take 0.4ml of tetrabutyl titanate and dissolve in 4ml of isopropanol, mix well and slowly drop into the above solution, subject to no precipitation; then add 4.3ml of deionized water and continue stirring for 0.5-1.5h. The mixture was warmed up to 80 °C, stirred and heated for 1 h, and 15 ml of deionized water was added. The resulting mixture was transferred into a stainless steel crystallization kettle with a polytetrafluoroethylene liner, statically crystallized at 140 °C for 2.5 h, and rapidly cooled to room temperature to obtain a precursor containing TS-1 nanoparticles. Dissolve 2.5g of dodecylamine in 10ml of absolute ethanol, add 15ml of deionized water, stir and mix evenly, drop the precursor obtained above into the mixture, and keep stirring at room temperature for 24h. The product was filtered, washed, dried, and calcined at 640°C for 4...

Embodiment 2

[0031] Add 11.2ml of tetraethylsilicate to 25.6ml of tetrapropylammonium hydroxide solution, stir at room temperature for 1-2 hours; take 0.4ml of tetrabutyl titanate and dissolve in 4ml of isopropanol, mix well and slowly drop into the above solution, subject to no precipitation; then add 4.3ml of deionized water and continue stirring for 0.5-1.5h. The mixture was warmed up to 80 °C, stirred and heated for 1 h, and 15 ml of deionized water was added. The resulting mixture was transferred into a stainless steel crystallization kettle lined with polytetrafluoroethylene, statically crystallized at 100 °C for 6 h, and rapidly cooled to room temperature to obtain a precursor containing TS-1 nanoparticles. Take 2.5g of dodecylamine and dissolve it in 10ml of absolute ethanol, add 15ml of deionized water, stir and mix evenly, drop the precursor obtained above into the mixture, and keep stirring at room temperature for 9h. The product was filtered, washed, dried, and calcined at 640...

Embodiment 3

[0033] Add 11.2ml of tetraethylsilicate to 25.6ml of tetrapropylammonium hydroxide solution, stir at room temperature for 1-2 hours; take 0.4ml of tetrabutyl titanate and dissolve in 4ml of isopropanol, mix well and slowly drop into the above solution, subject to no precipitation; then add 4.3ml of deionized water and continue stirring for 0.5-1.5h. The mixture was warmed up to 80 °C, stirred and heated for 1 h, and 15 ml of deionized water was added. The obtained mixture was transferred into a stainless steel crystallization kettle lined with polytetrafluoroethylene, statically crystallized at 60°C for 48h, and rapidly cooled to room temperature to obtain a precursor containing TS-1 nanoparticles. Take 2.5g of dodecylamine and dissolve it in 10ml of absolute ethanol, add 15ml of deionized water, stir and mix evenly, drop the precursor obtained above into the mixture, and keep stirring at room temperature for 18h. The product was filtered, washed, dried, and calcined at 640°C...

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PUM

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Abstract

The invention provides a middle-microporous compound titanium silicon molecule screen and relative preparation and application. It is characterized in that: it is belong to pure-phase molecule screen, with disordered worm-shape pore passage, while the middle holes are 20-30 and the micro holes are 5-9 and the wall of pore passage is mounted with the first and second structural units of microporous molecule screen. The preparation comprises two steps: first preparing the predecessors of first and second structural units of titanium silicon molecule screen; then using said predecessors to self assemble with long-chain alkylamine to attain said middle-microporous compound titanium silicon molecule screen. The invention has the advantages that: the composite condition is normal, and it has better catalytic oxidization properties in the reactions as oxidation desulfurization, olefin oxidization and styrene oxidization, etc.

Description

technical field [0001] The invention relates to a medium-microporous composite titanium-silicon molecular sieve catalyst which can be used in fuel oxidative desulfurization, olefin epoxidation and styrene oxidation and a preparation method thereof. Background technique [0002] US Patent No. 4,410,501 once disclosed titanium-silicon molecular sieve TS-1 and its preparation method. TS-1 molecular sieve has MFI structure. In the catalytic oxidation system using hydrogen peroxide as oxidant, it has excellent catalytic performance for olefin epoxidation, cyclohexanone ammoxidation, aromatic hydrocarbon oxidation, saturated hydrocarbon oxidation, alcohol oxidation and other reactions. Moreover, the reaction conditions are mild and environmentally friendly. [0003] US Patent No. 4,833,260 discloses an olefin epoxidation process using hydrogen peroxide as an oxidant and TS-1 molecular sieve as a catalyst. The reaction temperature is 0-150° C., the pressure is 1-100 atm., and the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89C01B39/08C07D301/12C07D303/04C10G27/00
Inventor 李钢金长子王祥生王云宫文魁高健郭新闻
Owner DALIAN UNIV OF TECH
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