Method for synthesizing mesoporous titanium-silicon molecular screen material

A technology of titanium-silicon molecular sieve and synthesis method, which is applied in the direction of molecular sieve compounds, molecular sieve catalysts, chemical instruments and methods, etc., which can solve the problems of single pore size, environmental and cost burden, and complicated preparation steps of the preparation method, and achieve good sample uniformity , reduce cost and environmental burden, good catalytic activity and activity stability

Active Publication Date: 2011-08-10
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Method for synthesizing mesoporous titanium-silicon molecular screen material
  • Method for synthesizing mesoporous titanium-silicon molecular screen material
  • Method for synthesizing mesoporous titanium-silicon molecular screen material

Examples

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Effect test

Embodiment 1

[0044] First add 50 grams of tetraethylorthosilicate to the aqueous solution composed of tetrapropylammonium hydroxide and cetyltrimethylammonium bromide, and stir them under normal pressure and 40℃ ultrasonically to make them evenly mixed. Add tetrabutyl titanate slowly and dropwise to it to obtain a mixture, in which the moles of tetraethyl orthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, cetyltrimethylammonium bromide and water The ratio is 1: 0.02: 0.25: 0.15: 95; transfer the above system to a stainless steel sealed reactor, first crystallize at a temperature of 100°C and autogenous pressure for 5 hours, and then crystallize at a temperature of 120°C and autogenous pressure For 48 hours, the obtained crystallized product was filtered, washed with water, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain mesoporous titanium silicate molecular sieve material A.

[0045] The X-ray diffraction spectrum (XRD) of A is as figure 1 As ...

Embodiment 2

[0049] First add 50 grams of tetraethylorthosilicate to the aqueous solution composed of tetrapropylammonium hydroxide and cetyltrimethylammonium bromide, and ultrasonically stir them under normal pressure and 35°C to make them evenly mixed. Slowly add tetrabutyl titanate dropwise to it under ultrasonic stirring to obtain a mixture, including tetraethyl orthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, and cetyltrimethylammonium bromide The molar ratio with water is 1:0.08:0.45:0.05:35. Put this mixture into a stainless steel sealed reactor and crystallize at a temperature of 100°C and autogenous pressure for 72 hours. The resulting crystallized product is filtered, washed with water, and dried at 110°C for 120 minutes, and then at a temperature of 550°C After firing for 3 hours, a mesoporous titanium silicate molecular sieve material B was obtained. The sample was characterized by X-ray diffraction, Fourier infrared spectroscopy, and visible-ultraviolet spectr...

Embodiment 3

[0051] First add 50 grams of tetraethylorthosilicate to the aqueous solution composed of tetrapropylammonium hydroxide and cetyltrimethylammonium bromide, and stir them under normal pressure and 55℃ ultrasonically to make them evenly mixed. Slowly add tetrabutyl titanate dropwise to it under ultrasonic stirring to obtain a mixture, including tetraethyl orthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, and cetyltrimethylammonium bromide The molar ratio with water is 1:0.04:0.18:0.22:120. Put this mixture into a stainless steel sealed reactor, firstly crystallize at a temperature of 100°C and autogenous pressure for 5 hours, and then crystallize at a temperature of 120°C and autogenous pressure for 24 hours, filter the resulting crystallized product and wash with water , Dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain mesoporous titanium silicate molecular sieve material C. The sample was characterized by X-ray diffraction, Fourie...

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Abstract

The invention provides a synthesis method of mesoporous Ti-HMS material and is characterized in that silica resource, titanium resource, organic alkali compound and surfactant are evenly mixed together by ultrasonic blending technology and that the mixture is used for obtaining product through hydrothermal crystallization. The synthesis method of the invention simplifies the synthesis technique, has easy and convenient operation, easily controllable process, good repeatedly preparation capacity but no special equipment requirement, and is applicable to industrial production; meanwhile the mesoporous Ti-HMS material prepared by the method has good catalytic oxidation function and promotes better effect in particular on the reaction of macromolecule.

Description

Technical field [0001] The present invention relates to a method for synthesizing titanium-containing materials, and further relates to a method for synthesizing mesoporous titanium silica molecular sieve materials. Background technique [0002] Titanium-silicon molecular sieve is a new type of titanium-containing heteroatom molecular sieve developed in the early 1980s. At present, Ti-ZSM-5 with MFI structure, namely TS-1, MEL structure TS-2, and TS-48 with larger pore structure have been synthesized. Among them, TS-1 molecular sieve is a new type of titanium silicate molecular sieve with excellent directional oxidation catalytic performance formed by introducing transition metal element titanium into the molecular sieve framework with ZSM-5 structure. TS-1 not only has the catalytic oxidation effect of titanium, but also has the shape-selective effect and excellent stability of ZSM-5 molecular sieve. However, Ti-ZSM-5 has a microporous (about 0.55 nanometers) structure, and it...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89C01B39/08C01B37/00
Inventor 林民史春风龙军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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