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A kind of ti-beta molecular sieve and its synthetic method and application

A molecular sieve and reaction technology, which is 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, and difficult synthesis, and achieve small particle size, few skeleton defects, and good catalysis performance effect

Active Publication Date: 2018-09-28
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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  • A kind of ti-beta molecular sieve and its synthetic method and application
  • A kind of ti-beta molecular sieve and its synthetic method and application
  • A kind of ti-beta molecular sieve and its synthetic method and application

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preparation example Construction

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

[0030] (1) Mix the silicon source, titanium source, mineralizer, structure directing agent, water and optional alkali source uniformly 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 agent is a mixture containing at least one halide ion compound and at least one alkali metal compound; A represents the number of moles of mineralizer in the reaction mixture, and R represents the number of moles of structure directing agent in the reaction mixture;

[0031] (2) Crystallize the reaction mixture obtained in st...

Embodiment 1

[0058] Under stirring conditions, mix ethyl orthosilicate, tetrabutyl titanate, tetraethylammonium hydroxide and deionized water at 60℃ to obtain SiO 2 :TiO 2 : Structure Directing Agent: H 2 O=1:0.02:1.1:20 alkaline mixed solution, then according to mineralizer: SiO 2 =0.6, the molar ratio of hydrofluoric acid: sodium chloride = 1.2, add mineralizer to the alkaline mixture and stir to obtain OH - :SiO 2 =0.77 Ti-β molecular sieve precursor.

[0059] After transferring the colloid to a pressure-resistant closed reactor, under agitation, the crystallization system was heated to 135°C and kept constant at autogenous pressure for 10 days to obtain a mixture of crystalline products; this mixture was filtered and washed with water. After all; drying at 110° C. for 8 hours and then roasting at 550° C. for 4 hours to obtain Ti-β molecular sieve. The XRD spectrum of the molecular sieve is as follows figure 1 As shown, the topography of the scanning electron microscope (SEM) is as figure ...

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 O=1:0.01:0.4:5 alkaline mixed solution, and then according to mineralizer: SiO 2 =0.01, fluorosilicic acid: sodium fluoride = 0.5 molar ratio, add mineralizer to the alkaline mixture and stir to obtain OH - :SiO 2 = 0.4 Ti-β molecular sieve precursor.

[0062] After transferring the colloid to a pressure-resistant closed reactor, under stirring, the crystallization system was heated to 120°C and kept at a constant temperature under autogenous pressure for 25 days to obtain a mixture of crystalline products; this mixture was filtered and washed with water. After all; drying at a temperature of 90°C for 12h and then calcining at a temperature of 450°C for 10h 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 silicate molecular sieve refers to a type of heteroatom molecular sieve containing four-coordinated framework titanium. Since Enichem first announced the titanium silicate TS-1 with MFI structure in 1983, people have developed a series of titanium silicate molecular sieves with different framework structures. For example, 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] β molecular sieve is a symbiosis of stacking faults composed of three closely related polymorphs. It has a three-dimensional twelve-membered ring pore structure. The pores in the [100] and [010] directions are straight pores with a pore diameter of about 0.66×0.67 nm; the pores in the [001] direction are composed of two [100] and [010] A sinusoidal channel with a hole diameter of about 0.5...

Claims

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Application Information

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Patent Type & Authority Patents(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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