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Ti-beta molecular sieve obtained by modifying full-silicon beta molecular sieve, preparation method and applications thereof

A beta molecular sieve, modified technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve problems such as inability to remove aluminum, and achieve the effect of high selectivity and good catalytic performance

Active Publication Date: 2017-01-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when there is skeleton aluminum in the molecular sieve, the dealumination treatment cannot completely remove the aluminum

Method used

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  • Ti-beta molecular sieve obtained by modifying full-silicon beta molecular sieve, preparation method and applications thereof
  • Ti-beta molecular sieve obtained by modifying full-silicon beta molecular sieve, preparation method and applications thereof
  • Ti-beta molecular sieve obtained by modifying full-silicon beta molecular sieve, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] Under stirring conditions, mix ethyl orthosilicate, tetrabutyl titanate, tetraethylammonium hydroxide and deionized water at 40°C to obtain a molar ratio of SiO 2 : TiO 2 : Structure directing agent: H 2 O=0.2:0.025:1.5:20 modifying solution, and then according to the molar ratio of all-silicon β molecular sieve, structure-directing agent and mineralizing agent as 1:1.5:1.2, the all-silicon β molecular sieve and mineralizing agent Sodium fluoride was added to the aforementioned modification solution, and after stirring evenly, the precursor of Ti-β molecular sieve was transferred to a pressure-resistant stainless steel reaction kettle; under stirring conditions, it was heated to 145°C and crystallized under autogenous pressure for 5 days.

[0065] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted Ti-β molecular sieve was recovered, dried at 110°C for 6 hours, and then calcined at 550°C for 5 hours to obtain the...

Embodiment 2

[0067] Under stirring conditions, mix methyl orthosilicate, tetrapropyl titanate, tetraethylammonium fluoride and deionized water at 30°C to obtain a molar ratio of SiO 2 : TiO 2 : Structure directing agent: H 2 O=0.08:0.002:0.8:10 modifying solution, and then according to the molar ratio of all-silicon β molecular sieve to structure-directing agent and mineralizer is 1:0.8:0.008, the all-silicon β molecular sieve and mineralizer Potassium fluoride was added to the aforementioned modifying liquid, and after stirring evenly, the precursor of Ti-β molecular sieve was transferred to a pressure-resistant stainless steel reactor; under stirring conditions, it was heated to 120°C and crystallized under autogenous pressure for 18 days.

[0068] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted Ti-β molecular sieve was recovered, dried at 90°C for 2 hours, and then calcined at 450°C for 10 hours to obtain the Ti-β molecular s...

Embodiment 3

[0070] Under stirring conditions, mix silica gel, tetraethyl titanate, triethylamine and deionized water at 60°C to obtain a molar ratio of SiO 2 : TiO 2 : Structure directing agent: H 2 O=0.3:0.05:2::30 modifying solution, and then according to the molar ratio of all-silicon β molecular sieve to structure-directing agent and mineralizer as 1:2:1.5, the all-silicon β molecular sieve and mineralization Lithium fluoride is added to the above-mentioned modification solution, and after stirring evenly, the Ti-β molecular sieve precursor is transferred to a pressure-resistant stainless steel reaction kettle; under stirring conditions, it is heated to 170°C and crystallized under autogenous pressure for 1 day .

[0071] After the stainless steel pressure-resistant reactor was lowered to room temperature, the obtained unroasted Ti-β molecular sieve was recovered, dried at 130°C for 12 hours, and then calcined at 600°C for 3 hours to obtain the Ti-β molecular sieve. SEM results suc...

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Abstract

The invention discloses a Ti-beta molecular sieve obtained by modifying a full-silicon beta molecular sieve, a synthesis method and applications thereof, wherein the preparation method comprises: (1) uniformly mixing a silicon source, a titanium source, a structure guiding agent, an alkali metal compound mineralization agent, a full-silicon beta molecular sieve and water to obtain a reaction mixture having a certain molar ratio; (2) crystallizing the reaction mixture obtained in the step (1) for 0.5-30 days in a pressure-resistant closed container at a temperature of 80-200 DEG C under an autogenous pressure to obtain a crystallized product; and (3) recovering the crystallized product obtained in the step (2). According to the present invention, the Ti-beta molecular sieve prepared according to the technical scheme has the good catalytic performance in the macromolecular oxidation reaction, and the selectivity of the oxidation product is high.

Description

technical field [0001] The invention relates to a Ti-β molecular sieve and its synthesis method and application, in particular to a Ti-β molecular sieve prepared by modification of all-silicon β molecular sieve and its preparation method and application. 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-β with BEA structure, Ti-ZSM-12 with MTW structure, and Ti-MCM-22 with MWW structure, etc. [0003] β molecular sieves are stacking fault symbiosis composed of three structurally distinct but closely related polymorphs. It has a three-dimensional twelve-membered ring channel structure, in which the channels in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/70C07D301/12C07D303/06
Inventor 王宝荣林民朱斌彭欣欣舒兴田
Owner CHINA PETROLEUM & CHEM CORP