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Ti-beta molecular sieve and synthesis method and application thereof

A molecular sieve and reaction technology, applied in the field of Ti-beta molecular sieve and its synthesis, can solve the problems of reduced selective oxidation activity, too large Ti-β particles, complex structure, etc., and achieve small particle size, few skeleton defects and good catalysis performance effect

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

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Problems solved by technology

However, the structure of the new template is complex and difficult to synthesize; while the particles of Ti-β prepared under neutral conditions are too large, resulting in a decrease in its selective oxidation activity

Method used

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  • Ti-beta molecular sieve and synthesis method and application thereof
  • Ti-beta molecular sieve and synthesis method and application thereof
  • Ti-beta molecular sieve and synthesis method and application thereof

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preparation example Construction

[0029] On the other hand, the present invention also provides a kind of synthetic method of Ti-beta molecular sieve, comprises the following steps:

[0030] (1) Mix the silicon source, titanium source, mineralizer, structure-directing agent, water and optional alkali source evenly to obtain a molar ratio of OH - : SiO 2 : TiO 2 :A:R:H 2 O=(0.15-3):1:(0.001-0.1):(0.001-5):(0.3-5):(3-300) reaction mixture; wherein, the structure directing agent is selected from tetraethyl At least one of ammonium hydroxide, tetraethylammonium fluoride, tetraethylammonium chloride, tetraethylammonium bromide, tetraethylammonium iodide, diethylamine and triethylamine, the mineral The mineralizing agent is a mixture containing at least one halogen ion compound and at least one alkali metal compound; A represents the molar number of the mineralizing agent in the reaction mixture, and R represents the molar number of the structure-directing agent in the reaction mixture;

[0031] (2) crystallize th...

Embodiment 1

[0058] Under stirring conditions, ethyl orthosilicate, tetrabutyl titanate, tetraethylammonium hydroxide and deionized water were mixed at 60 °C to obtain SiO 2 :TiO 2 : Structure directing agent: H 2 Alkaline mixed solution of O=1:0.02:1.1:20, then mineralizer: SiO 2 = 0.6, hydrofluoric acid: sodium chloride = 1.2 molar ratio, mineralizer is added to the alkaline mixture and stirred evenly to obtain OH - :SiO2 2 =0.77 Ti-beta molecular sieve precursor.

[0059] After transferring the colloid to a pressure-resistant closed reactor, the temperature of the crystallization system was raised to 135°C under stirring conditions, and the temperature was kept at autogenous pressure for 10 days to obtain a mixture of crystallization products; the mixture was filtered and washed with water for several After one pass; drying at a temperature of 110°C for 8 hours and then calcining at a temperature of 550°C for 4 hours to obtain a Ti-β molecular sieve. The XRD spectrum of the molecul...

Embodiment 2

[0061] Under stirring conditions, mix methyl orthosilicate, tetrapropyl titanate, tetraethylammonium fluoride, deionized water and external alkali source sodium carbonate at 40°C to obtain SiO 2 :TiO 2 : Structure directing agent: H 2 Alkaline mixed solution of O=1:0.01:0.4:5, then mineralizer: SiO 2 =0.01, fluorosilicic acid: sodium fluoride = 0.5 molar ratio, add mineralizer to the alkaline mixture and stir evenly to obtain OH - :SiO2 2 =0.4 Ti-beta molecular sieve precursor.

[0062] After transferring the colloid to a pressure-resistant closed reactor, the temperature of the crystallization system was raised to 120°C under stirring conditions, and the temperature was kept at autogenous pressure for 25 days to obtain a mixture of crystallization products; the mixture was filtered and washed with water for several After one pass; drying at 90° C. for 12 hours and then calcination at 450° C. for 10 hours to obtain Ti-β molecular sieve.

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Abstract

The invention discloses an aluminum-free Ti-beta molecular sieve and a synthesis method thereof. The aluminum-free Ti-beta molecular sieve has a flakey morphology, the length and width size is not more than 490 nm, and the thickness is not more than 100 nm; the Q4 / Q3 is not less than 30. The synthesis of the molecular sieve includes the following steps: (1) evenly mixing a silicon source, a titanium source, a mineralizer, a structural guide agent, water and an optional alkali source, to obtain a reaction mixture with a certain molar ratio; (2) crystallizing the reaction mixture obtained in the step (1) for 0.5-40 days in a pressure-proof airtight container at the temperature of 110-230 DEG C and at self-generated pressure, to obtain a crystallized product; and (3) recycling the crystallized product obtained in the step (2). The aluminum-free Ti-beta molecular sieve obtained by the synthesis method has relatively good catalytic properties in reactions for preparing cyclohexene oxide through catalytic oxidation of cyclohexene and preparing epoxyoctane through catalytic oxidation of 1-octylene.

Description

technical field [0001] The invention relates to a Ti-beta molecular sieve and its synthesis 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-beta 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, and the channels in the [100] and [010] directions are straight channels with a diameter of about 0.66×0.67 nm; the channels in the [001] direction are composed of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08B01J29/89C07D301/12C07D303/04
Inventor 王宝荣朱斌舒兴田彭欣欣林民
Owner CHINA PETROLEUM & CHEM CORP
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