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A kind of hierarchical porous 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 affecting the activity of molecular sieves and low crystallinity of titanium-silicon molecular sieves, and achieve high selective oxidation activity, uniform particle size distribution, and specific surface area big effect

Active Publication Date: 2018-11-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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, and the titanium-silicon molecular sieves prepared by direct silanization treatment and precrystallization-silanization treatment have low crystallinity, and silanization reagents can affect the activity of molecular sieves, etc.

Method used

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  • A kind of hierarchical porous titanium-silicon molecular sieve and synthesis method thereof
  • A kind of hierarchical porous titanium-silicon molecular sieve and synthesis method thereof
  • A kind of hierarchical porous 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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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 王宝荣彭欣欣朱斌林民舒兴田
Owner CHINA PETROLEUM & CHEM CORP