Preparation method of hierarchical porous titanium silicon molecular sieve

A titanium-silicon molecular sieve and multi-level pore technology, which is applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the difficulty in the treatment of inorganic salts and inorganic bases, the large loss of molecular sieve quality and crystallinity, and the inability to effectively improve the reaction performance of molecular sieves with macromolecules. and other problems, to achieve the effect of high crystallinity and high macromolecular reactivity

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0009] In summary, either inorganic or organic base treatment alone can construct titanium-silicon molecular sieves with a certain multi-level pore size, but inorganic base treatment has problems such as large loss of molecular sieve quality and crystallinity, difficulty in the treatment of inorganic salts and inorganic bases, etc. ; Although organic base treatment can intr...

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  • Preparation method of hierarchical porous titanium silicon molecular sieve
  • Preparation method of hierarchical porous titanium silicon molecular sieve
  • Preparation method of hierarchical porous titanium silicon molecular sieve

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Embodiment 1

[0077] 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 A homogeneous mixture of O=1:0.2:0.025:50; press SiO again 2 : Silylating agent = 1:0.12 molar ratio, add N-phenyl-triaminopropyltrimethoxysilane to the clarified titanium-silicon molecular sieve precursor gel, after stirring evenly, transfer the obtained titanium-silicon molecular sieve precursor To a pressure-resistant stainless steel reactor; under stirring conditions, heated to 170 ° C and crystallized under autogenous pressure for 8h. After the stainless steel pressure-resistant reactor was lowered to room temperature, the titanium-silicon molecular sieve was recovered, dried at 110°C for 6 hours, and then calcined at 550°C for 4 hours to obtain the hierarchically porous titanium-silicon molecular sieve TS-1 prepared by silanization.

[0078] Under stirring conditions, ...

Embodiment 2

[0080] Under stirring conditions, white carbon black, tetrapropylammonium hydroxide, tetraethyl titanate and deionized water were mixed to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 A homogeneous mixture of O=1:0.5:0.03:100; after pre-crystallization at 90°C for 1, press SiO 2 : Silylating agent = 1:0.2 molar ratio, add hexamethyldisilazane to the titanium-silicon molecular sieve precursor gel obtained by pre-crystallization, stir evenly, transfer the obtained titanium-silicon molecular sieve precursor to a pressure-resistant In a stainless steel reactor; under stirring conditions, heated to 190 ℃ and crystallized under autogenous pressure for 24h. 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 550°C for 6 hours to obtain the hierarchically porous titanium-silicon molecular sieve TS- 1.

[...

Embodiment 3

[0083] Under stirring conditions, mix silica gel, tetraethylammonium hydroxide, titanium tetrachloride and deionized water to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:1:0.05:150 homogeneous mixture; press SiO again 2 : Silylating agent = 1:0.25 molar ratio, add phenyltriethoxysilane to the clarified titanium-silicon molecular sieve precursor gel, stir evenly, transfer the obtained titanium-silicon molecular sieve precursor to the pressure-resistant stainless steel reaction Kettle; under stirring conditions, heated to 210 ° C and crystallized under autogenous pressure for 12h. After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted titanium-silicon molecular sieve was recovered, dried at 150°C for 2 hours, and then calcined at 650°C for 8 hours to obtain the hierarchically porous titanium-silicon molecular sieve TS- 1.

[0084] Under stirring conditions, mix the calcined TS-1, tetrabutylam...

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Abstract

The invention discloses a method for preparing a multi-level porous titanium-silicon molecular sieve, which comprises the following steps: (1) After mixing the silicon source, the structure-directing agent, the titanium source and water uniformly in a certain proportion, directly adding a silylating agent or first After pre-crystallization, a silylating agent is added to obtain a reaction mixture containing a silylating agent; (2) the reaction mixture containing a silylating agent is crystallized under certain conditions in a pressure-resistant airtight container, and then recovered to obtain a crystallized product; (3) the recovered crystallized product is roasted and then treated with alkali to obtain an alkaline mixture; (4) the alkaline mixture is hydrothermally treated in a pressure-resistant airtight container, and the product is recovered. The hierarchically porous titanium-silicon molecular sieve obtained by the technical scheme has the advantages of high crystallinity, high macromolecular reactivity and selectivity, and adjustable pore structure.

Description

technical field [0001] The invention relates to a method for synthesizing a titanium-silicon molecular sieve, in particular to a method for preparing a multi-level porous titanium-silicon molecular sieve. 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. Such as TS-2 of MEL structure, Ti-beta of BEA structure, Ti-ZSM-12 of MTW structure and Ti-MCM-22 of 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 0.51×0.55nm, and the [010] direction is a sinusoidal channel with a diameter of 0.53×0.56nm. Due to the introduction of Ti atoms and its special pore str...

Claims

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Application Information

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