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Synthetic method of titanium-containing mesoporous materials

A technology of mesoporous materials and synthesis methods, applied in chemical instruments and methods, molecular sieves and alkali exchange compounds, inorganic chemistry, etc., can solve the problems of single pore size of composite materials, environmental and cost burdens, and complicated preparation steps of preparation methods, etc. Achieve uniform distribution of species, reduce cost and environmental burden, and achieve the effect of good catalytic oxidation function

Active Publication Date: 2012-12-12
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, 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 preparation steps in the preparation method are relatively complicated, have environmental and cost burdens

Method used

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  • Synthetic method of titanium-containing mesoporous materials
  • Synthetic method of titanium-containing mesoporous materials
  • Synthetic method of titanium-containing mesoporous materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] First, add 50 grams of tetraethyl orthosilicate to the aqueous solution of tetrapropylammonium hydroxide and stir it ultrasonically to make it evenly mixed. Liquid is added to the aqueous solution of cetyltrimethylammonium bromide and ultrasonically stirred to make it evenly mixed, in which tetraethylorthosilicate, tetrabutyl titanate, tetrapropylammonium hydroxide, cetyltrimethyl The molar ratio of ammonium bromide and water is 1: 0.02: 0.45: 0.15: 85; the above system is transferred to a stainless steel sealed reaction kettle, first crystallized at 100 °C and autogenous pressure for 5 hours, and then at 120 °C and autogenous pressure After crystallization under pressure for 48 hours, the obtained crystallized product was filtered, washed, dried at 110°C for 120 minutes, and then calcined at 550°C for 3 hours to obtain titanium-containing mesoporous material A.

[0040] The XRD crystal phase diagram of A is as follows figure 1 The nitrogen adsorption isotherm is shown...

Embodiment 2

[0045] First add 50 grams of tetramethyl orthosilicate to the aqueous solution of tetrapropylammonium hydroxide and stir it ultrasonically to make it evenly mixed, then slowly add an appropriate amount of tetraethyl titanate into it under normal temperature and pressure ultrasonic stirring, and then The mixed liquid is added to the aqueous solution of the surfactant tetradecyltrimethylammonium bromide and stirred ultrasonically to make it evenly mixed. Among them, tetramethyl orthosilicate, tetraethyl titanate, tetrapropylammonium hydroxide, surface active The molar ratio of agent and water is 1:0.008:0.15:0.05:25. Put this mixed solution into a stainless steel sealed reaction kettle, crystallize at 100°C and autogenous pressure for 72 hours, filter and wash the crystallized product obtained, and dry at 110°C for 120 minutes, then bake at 550°C for 3 hours, a titanium-containing mesoporous material B was obtained, and the sample was characterized by X-ray diffraction, Fourier ...

Embodiment 3

[0047] First add 50 grams of tetraethyl orthosilicate to the aqueous solution of ethylamine and stir it ultrasonically to make it evenly mixed, then slowly add an appropriate amount of tetrabutyl titanate to it under ultrasonic stirring at normal temperature and pressure, and then add the mixed solution to the Ultrasonic stirring in the aqueous solution of cetyltrimethylammonium bromide makes it evenly mixed, wherein the molar ratio of tetraethyl orthosilicate, tetrabutyl titanate, ethylamine, surfactant and water is 1:0.4: 0.35:0.25:150. Put this mixed solution into a stainless steel sealed reaction kettle, first crystallize at 100°C and autogenous pressure for 5 hours, then crystallize at 160°C and autogenous pressure for 24 hours, filter the obtained crystallized product, wash with water, and dry at 110°C ℃ drying for 120 minutes, and then roasting at a temperature of 550 ℃ for 3 hours to obtain a titanium-containing mesoporous material C, which is characterized by X-ray di...

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Abstract

The invention provides a synthetic method of titanium-containing mesoporous materials, which is characterized by comprising the following steps of: adding a silicon source to the water solution of an The invention provides a synthetic method of titanium-containing mesoporous materials, which is characterized by comprising the following steps of: adding a silicon source to the water solution of anorgano-alkali compound in a dropping manner under the ultrasonic agitation; after homogeneous mixing, adding a titanium source to the mixture; after the hydrolysis is completed, mixing the obtained miorgano-alkali compound in a dropping manner under the ultrasonic agitation; after homogeneous mixing, adding a titanium source to the mixture; after the hydrolysis is completed, mixing the obtained mixture with the water solution of a surface active agent to obtain a mixture with the mole ratio of silicon source: titanium source: organic base: surface active agent: water=1:(0.001-0.5) :(0.05-0.8)xture with the water solution of a surface active agent to obtain a mixture with the mole ratio of silicon source: titanium source: organic base: surface active agent: water=1:(0.001-0.5) :(0.05-0.8):(0.01-0.5) :(5-250); putting the mixture into a sealed reaction kettle for hydrothermal crystallization; and then collecting the obtained titanium-containing mesoporous material. The titanium-contain:(0.01-0.5) :(5-250); putting the mixture into a sealed reaction kettle for hydrothermal crystallization; and then collecting the obtained titanium-containing mesoporous material. The titanium-containing mesoporous material synthesized by the method has good catalytic oxidation function and better effect on the reactions in the presence of large molecules.ing mesoporous material synthesized by the method has good catalytic oxidation function and better effect on the reactions in the presence of large molecules.

Description

technical field [0001] The invention relates to a synthesis method of an inorganic material, and more specifically to a synthesis method of a titanium-containing mesoporous material. Background technique [0002] Titanium-silicon molecular sieve is a new molecular sieve containing heteroatom titanium, which was 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. Among them, TS-1 molecular sieve is a new type of titanium-silicon 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 only has a microporous (about 0.55 nanometer) structure, and it is difficult for...

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