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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 unsatisfactory pore structure adjustability, low crystallinity of crystallized products, etc., and achieve good macromolecular reaction performance and pore channels The effect of adjustable structure and 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 reagents, the crystallinity of the crystallized product is low, and the adjustability of the pore structure 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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] 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.

[0074] After the pre-crystallization is complete, press n 硅烷化试剂 :n SiO2 =0.12, n 硅烷化试剂 :n 表面活性剂 =1 molar ratio, N-phenyl-3-aminopropyltrimethoxysilane and hexyltrimethylammonium chloride are added to the pre-crystallized titanium-silicon molecular sieve nanoclusters, and after stirring evenly, the obtained titanium-silicon The molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, the temperature was raised to 170°C and crystallized under autogenous pressure for 8h.

[0075] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtaine...

Embodiment 2

[0077] Under stirring conditions, white carbon black, tetrapropyl ammonium hydroxide, tetrapropyl titanate and deionized water were mixed to obtain a molar ratio of SiO 2 : Structure directing agent: TiO 2 :H 2 O=1:0.5:0.03:100 homogeneous mixture; press n again 硅烷化试剂 :n SiO2 =0.2, n 硅烷化试剂 :n 表面活性剂 =0.5 molar ratio, N-phenyl-3-aminopropyltrimethoxysilane and octyltriethylammonium chloride are added to the titanium-silicon molecular sieve precursor gel, after stirring evenly, the obtained titanium-silicon molecular sieve The precursor was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, the temperature was raised to 190°C and crystallized under autogenous pressure for 24h.

[0078] 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 poro...

Embodiment 3

[0080] Under stirring conditions, mix silica gel, tetraethylammonium hydroxide, tetraethyl 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.

[0081] After the pre-crystallization is complete, press n 硅烷化试剂 :n SiO2 =0.25, n 硅烷化试剂 :n 表面活性剂 =0.2 molar ratio, N-phenyl-3-aminopropyltrimethoxysilane and phenyltriethoxyammonium chloride were added to the precrystallized titanium-silicon molecular sieve nanoclusters, and after stirring evenly, the obtained The titanium-silicon molecular sieve precursor was transferred to a pressure-resistant stainless steel reactor; the temperature was raised to 210 ° C under stirring conditions and crystallized under autogenous pressure for 12 hours.

[0082] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted titaniu...

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Abstract

The invention discloses a method for preparing a multilevel-pore titanium-silicon molecular sieve. The method includes the following steps that 1, a silicon source, a structure-directing agent, a titanium source and water are mixed to be even in a certain proportion, then a silylating reagent and a surfactant are added, or after pre-crystallization is carried out for 0.5 hour to 48 hours at the temperature of 30 DEG C to 90 DEG C, a silylating reagent and a surfactant are added, and the mixture containing the silylating reagent and the surfactant is obtained; 2, the mixture obtained in the step 1 is crystallized for 1 hour to 240 hours in a pressure-proof closed container at the temperature of 110 DEG C to 230 DEG C under the self-generated pressure, and the crystallized product is obtained; 3, the crystallized product obtained in the step 2 is recycled. By means of the technical scheme, the multilevel-pore titanium-silicon molecular sieve which is large in mesoporous volume, adjustable in pore channel structure and good in macromolecule reaction performance 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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