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Method for synthesizing titanium-silicon materials with mesoporous and microporous structures

A microporous structure, titanium-silicon technology, applied in chemical instruments and methods, crystalline aluminosilicate zeolites, molecular sieves and alkali exchange compounds, etc., can solve the environmental and cost burdens, the complicated preparation method steps, and the single size of the pores of the composite material. and other problems, to achieve the effect of reducing cost and environmental burden, eliminating local concentration unevenness, and improving catalytic performance

Active Publication Date: 2011-06-15
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] CN1226187C has reported the titanium-silicon molecular sieve composite material with above-mentioned two kinds of structures and its preparation method, has certain catalytic activity, but the main problem that it exists is that its mentioned composite material pore size is single (diffraction in X-ray diffraction spectrogram figure The peak position is strictly limited), and the steps in its preparation method are relatively complicated, and there are environmental and cost burdens

Method used

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  • Method for synthesizing titanium-silicon materials with mesoporous and microporous structures
  • Method for synthesizing titanium-silicon materials with mesoporous and microporous structures
  • Method for synthesizing titanium-silicon materials with mesoporous and microporous structures

Examples

Experimental program
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Effect test

Embodiment 1

[0044] First, 30 grams of tetraethyl orthosilicate and appropriate amount of tetrabutyl titanate were added to the aqueous solution of tetrapropylammonium hydroxide respectively, and ultrasonically stirred at normal pressure and 40°C to mix them uniformly to form two kinds of solutions. After mixing the two solutions, add them to the aqueous solution of cetyltrimethylammonium bromide and continue ultrasonic stirring to make them evenly mixed. Among them, tetraethyl orthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, The molar ratio of hexaalkyltrimethylammonium bromide to water is 1:0.02:0.4:0.05:25; the above system is transferred to a stainless steel sealed reaction kettle, and crystallized at a temperature of 100°C and autogenous pressure for 5 hours , and then crystallized at a temperature of 140°C and autogenous pressure for 48 hours, filtered the obtained crystallized product, washed with water, dried at 110°C for 120 minutes, and then calcined at a tempera...

Embodiment 2

[0050] First, add 30 grams of tetraethyl orthosilicate and appropriate amount of tetrapropyl titanate to the aqueous solution of diethanolamine respectively, and stir them ultrasonically at normal pressure and 60°C to form two kinds of solutions, and mix the above two kinds of solutions Then add it to the aqueous solution of cetyltrimethylammonium bromide and continue ultrasonic stirring to make it evenly mixed, in which tetraethyl orthosilicate, tetrapropyl titanate, diethanolamine, cetyltrimethyl The molar ratio of ammonium to water is 1:0.08:0.2:0.2:180. Put this mixed solution into a stainless steel sealed reaction kettle, crystallize at a temperature of 120°C and autogenous pressure for 48 hours, filter the resulting crystallized product, wash with water, and dry at 110°C for 120 minutes, and then at a temperature of 550°C Calcined for 3 hours to obtain titanium silicon material B. The sample is characterized by X-ray diffraction, Fourier transform infrared spectrum and ...

Embodiment 3

[0052] First, add 30 grams of tetramethyl orthosilicate and appropriate amount of tetrabutyl titanate into the aqueous solution of tetrapropylammonium hydroxide respectively, and stir them ultrasonically to make them evenly mixed to form two kinds of solutions. After mixing the above two kinds of solutions, add them to Continue ultrasonic stirring in the aqueous solution of tetradecyl trimethyl ammonium bromide to make it evenly mixed, in which tetramethyl orthosilicate, tetrabutyl titanate, tetrapropyl ammonium hydroxide, tetradecyl trimethyl bromide The molar ratio of ammonium chloride to water is 1:0.4:0.1:0.1:130. Put this mixed solution into a sealed stainless steel reaction kettle, first crystallize at a temperature of 80°C and an autogenous pressure for 5 hours, and then crystallize at a temperature of 160°C and an autogenous pressure for 24 hours, filter the crystallized product obtained, and wash with water , and dried at 110° C. for 120 minutes, and then fired at 550...

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Abstract

The invention provides a method for synthesizing titanium-silicon materials with mesoporous and microporous structures, which is characterized by comprising the following steps of: adding a titanium sThe invention provides a method for synthesizing titanium-silicon materials with mesoporous and microporous structures, which is characterized by comprising the following steps of: adding a titanium source and a silicon source to the water solution of organo-alkali compound respectively under the ultrasonic agitation to obtain two solutions after homogeneous mixing; and then mixing the two solutioource and a silicon source to the water solution of organo-alkali compound respectively under the ultrasonic agitation to obtain two solutions after homogeneous mixing; and then mixing the two solutions evenly under the ultrasonic agitation; mixing the mixture with the water solution of a surface active agent evenly under the ultrasonic agitation to obtain a mixture with the mole ratio of siliconns evenly under the ultrasonic agitation; mixing the mixture with the water solution of a surface active agent evenly under the ultrasonic agitation to obtain a mixture with the mole ratio of siliconsource: titanium source: organic base: surface active agent: water equals to 1: (0.001-0.5) : (0.05-0.8) : (0.05-0.5) : (5-200); putting the mixture into a sealed reaction kettle for hydrothermal cryssource: titanium source: organic base: surface active agent: water equals to 1: (0.001-0.5) : (0.05-0.8) : (0.05-0.5) : (5-200); putting the mixture into a sealed reaction kettle for hydrothermal crystallization; and then collecting the obtained titanium-silicon material. The titanium-silicon material synthesized by the method has good catalytic oxidation property and better effect on the oxidatiotallization; and then collecting the obtained titanium-silicon material. The titanium-silicon material synthesized by the method has good catalytic oxidation property and better effect on the oxidation reactions in the presence of large molecules.n reactions in the presence of large molecules.

Description

technical field [0001] The invention relates to a synthesis method of an inorganic material, and furthermore relates to a synthesis method of a titanium-silicon material with a mesoporous and microporous structure. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. At present, Ti-ZSM-5 with MFI structure, namely TS-1, TS-2 with MEL structure, and TS-48 with larger pore structure have been synthesized. TS-1 molecular sieve is a new type of titanium-silicon molecular sieve with excellent directional oxidation catalytic performance formed by introducing the transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 molecular sieve not only has the catalytic oxidation of titanium, but also It also has the shape-selective effect of ZSM-5 molecular sieve and excellent stability. However, the microporous structure of TS-1 molecular sieve is about 0.55 nanomet...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08C01B39/48
Inventor 林民史春风朱斌舒兴田慕旭宏罗一斌汪燮卿汝迎春
Owner CHINA PETROLEUM & CHEM CORP
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