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A kind of method for preparing hierarchical porous titanium-silicon molecular sieve

A titanium-silicon molecular sieve and multi-stage pore technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of reducing the crystallinity of molecular sieves and unsatisfactory pore structure adjustability, etc., and achieve less skeleton defects and good macromolecular oxidation performance , the effect of high crystallinity

Active Publication Date: 2019-04-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • 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, and when using these two silylating agents, the crystallinity of molecular sieves will be greatly reduced, and the adjustability of the pore structure introduced by them is not ideal

Method used

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  • A kind of method for preparing hierarchical porous titanium-silicon molecular sieve
  • A kind of method for preparing hierarchical porous titanium-silicon molecular sieve
  • A kind of method for preparing hierarchical porous titanium-silicon molecular sieve

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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 A homogeneous mixture of O=1:0.2:0.025:50; heated to 90°C under stirring conditions and pre-crystallized under autogenous pressure for 24h. Press SiO again 2 : silylating agent = 1: 0.12, n N-苯基三氨基丙基三甲氧基硅烷 :n 六甲基二硅氧烷 =1 molar ratio, N-phenyl-3-aminopropyltrimethoxysilane and hexamethyldisiloxane are added to the pre-crystallized titanium-silicon molecular sieve nanoclusters, and after stirring evenly, the resulting composite silane The chemically treated titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; then the temperature was raised to 170°C and crystallized under autogenous pressure for 8 hours.

[0071] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted t...

Embodiment 2

[0073] Under stirring conditions, white carbon black, tetraethylammonium 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; press SiO again 2 : silylating agent = 1: 0.2, n [3-三甲氧基硅丙基]二甲基十八烷溴化铵 :n 辛基三乙氧基硅烷 =0.5 molar ratio, after adding [3-trimethoxysilylpropyl] dimethyl octadecyl ammonium bromide and octyltriethoxysilane to the mixture, after stirring evenly, the obtained composite silylation treatment The titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; then the temperature was raised to 190°C and crystallized under autogenous pressure for 24h.

[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 550°C for 6 hours to obtain the h...

Embodiment 3

[0076] Under stirring conditions, mix silica gel, tetrabutylammonium hydroxide, tetrapropyl titanate 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; heated to 40°C with stirring and pre-crystallized under autogenous pressure for 48h. Press SiO again 2 : silylating agent = 1: 0.25, n N-苯基三氨基丙基三甲氧基硅烷 :n 甲基三乙氧基硅烷 = 0.2 molar ratio, N-phenyl-3-aminopropyltrimethoxysilane and methyltriethoxysilane were added to the titanium-silicon molecular sieve nanoclusters obtained by precrystallization, and after stirring evenly, the obtained composite silane The chemically treated titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, the temperature was raised to 210 ° C and crystallized under autogenous pressure for 12 hours.

[0077] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obta...

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Abstract

The invention discloses a method for preparing a hierarchical pore titanium silicalite molecular sieve. The method comprises the following steps that 1, after a silicon source, a structure-directing agent, a titanium source and water are mixed to be uniform according to a certain proportion, a silylating reagent is directly added or is added after the mixture is pre-crystallized, and a reaction mixture containing the silylating reagent is obtained, wherein the silylating reagent is a novel silylating reagent; 2, the reaction mixture which contains the silylating reagent and obtained in the step 1 is crystallized in a pressure-resistant closed container under certain conditions, and then an obtained crystallization product is recycled. According to the technical scheme, the hierarchical pore titanium silicalite molecular sieve which is high in relative crystallinity, few in framework defect, good in macromolecule oxidation property and adjustable in pore structure can be prepared.

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 0.51×0.55 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 s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/08
Inventor 王宝荣林民朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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