Hierarchical pore titanium-silicon molecular sieve and synthesis method thereof

A technology of titanium-silicon molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of low crystallinity of titanium-silicon molecular sieve and affect the activity of molecular sieve, and achieve high selective oxidation activity, uniform particle size distribution, and specific surface area big effect

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Even so, only two silylating agents, [3-trimethoxysilylpropyl]dimethyloctadecylammonium bromide and N-phenyl-3-aminopropyltrimethoxysilane, are currently used in multistage The synthesis of porous titanium-silicon molecular sieves

Method used

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  • Hierarchical pore titanium-silicon molecular sieve and synthesis method thereof
  • Hierarchical pore titanium-silicon molecular sieve and synthesis method thereof
  • Hierarchical pore titanium-silicon molecular sieve and synthesis method thereof

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preparation example Construction

[0034] On the other hand, the present invention also provides a kind of synthetic method of hierarchical porous titanium silicon molecular sieve, comprises the following steps:

[0035] (1) Mix the silicon source, the structure directing agent, the titanium source, water, silylating agent with the natural polymer compound and / or the modified natural polymer compound to obtain a reaction mixture, in which SiO 2 :R:TiO 2 :H 2 The molar ratio of O:B is 1:(0.001-5):(0.001-0.1):(5-400):(0.001-0.5), natural polymer compound and / or modified natural polymer compound in the reaction mixture with SiO 2 The weight ratio is 0.001-1; Wherein, R represents the molar number of the structure directing agent in the reaction mixture, and B represents the molar number of the silylating agent in the reaction mixture;

[0036] (2) crystallizing the reaction mixture obtained in step (1) in a pressure-resistant airtight container at 90-230° C. and autogenous pressure for 1-240 hours to obtain a c...

Embodiment 1

[0070] Under stirring conditions, mix ethyl orthosilicate, tetrapropylammonium hydroxide, tetrabutyl titanate and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:0.2:0.025:50 mixture. Press SiO again 2 The molar ratio to silylating agent is 1:0.1, SiO 2 The weight ratio of the natural polymer compound is 1:0.1, add quaternized cellulose and N-phenyl-3-aminopropyltrimethoxysilane to the titanium-silicon molecular sieve precursor gel mixture, and stir evenly Finally, the obtained silylating agent and the titanium-silicon molecular sieve precursor treated with the modified natural polymer compound were transferred to a pressure-resistant stainless steel reaction kettle; under stirring conditions, heated to 170°C and crystallized under autogenous pressure for 24 hours.

[0071] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted titanium-silicon molecular sieve was recovered, ...

Embodiment 2

[0073] Under stirring conditions, mix propyl orthosilicate, tetraethylammonium hydroxide, tetraethyl titanate and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:0.01:0.01:16 mixture. Press SiO again 2 The molar ratio to silylating agent is 1:0.04, SiO 2 The weight ratio of the natural polymer compound is 1:0.05. Add cellulose and trimethylchlorosilane to the titanium-silicon molecular sieve precursor gel mixture. After stirring evenly, the obtained silylating agent and natural polymer compound are treated The titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, it was heated to 190°C and crystallized under autogenous pressure for 48h.

[0074] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted titanium-silicon molecular sieve was recovered, dried at 130°C for 4 hours, and then calcined at 5...

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Abstract

The invention discloses a hierarchical pore titanium-silicon molecular sieve and a synthesis method thereof. The particle size of the hierarchical pore titanium-silicon molecular sieve ranges from 250 nanometers to 350 nanometers, the relative crystallinity is not smaller than 45%, and the specific area is not smaller than 600 m<2>/g. The synthesis method includes the following steps that 1, a silicon source, a structure directing agent, a titanium source, water, a silylating reagent, a natural polymer compound and/or a modified natural polymer compound are mixed to be uniform according to a certain ratio, and a reaction mixture is obtained; 2, the reaction mixture obtained in the step 1 is crystallized for 1-240 h in a pressure-proof sealed container at the temperature of 90-230 DEG C and under self-generated pressure, and a crystallized product is obtained; 3, the crystallized product obtained in the step 2 is recycled. The hierarchical pore titanium-silicon molecular sieve has good catalytic activity in macromolecule reaction 1-octene oxidation.

Description

technical field [0001] The invention relates to a multi-level porous titanium-silicon molecular sieve and a synthesis method thereof. Background technique [0002] Titanium-silicon molecular sieves refer to a class of heteroatom molecular sieves containing four-coordinated titanium framework. Since Enichem first announced the titanium-silicon molecular sieve TS-1 with MFI structure in 1983, people have successively developed a series of titanium-silicon molecular sieves with different skeleton structures. For example, TS-2 with MEL structure, Ti-beta with BEA structure, Ti-ZSM-12 with MTW structure, and Ti-MCM-22 with MWW structure, etc. [0003] TS-1 has a two-dimensional ten-membered ring channel system. The [100] direction is a straight channel with a diameter of 0.51×0.55 nm, and the [010] direction is a sinusoidal channel with a diameter of 0.53×0.56 nm. Due to the introduction of Ti atoms and its special pore structure, TS-1 and H 2 o 2 The formed oxidation system ...

Claims

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Application Information

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IPC IPC(8): C01B39/08
Inventor 王宝荣彭欣欣朱斌林民舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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