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

A molecular sieve and seed crystal technology, applied in the field of Ti-beta molecular sieve and its synthesis, can solve the problems of large particle size, aluminum removal, and long molecular sieve crystallization time.

Active Publication Date: 2019-02-01
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the dealuminated β molecular sieve is used as the seed crystal, the crystallization time of the molecular sieve is long, the crystallized product has many defects, and the dealumination process is difficult to control. It can increase the acidity of molecular sieves and reduce the selectivity of oxidation products; the structure of the new template is complex and difficult to synthesize; when synthesized under neutral conditions, the amount of mineralizer HF is large and toxic, and the synthesis of Ti-β under neutral conditions Long period and large particles will reduce 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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Under stirring conditions, mix ethyl orthosilicate, tetrabutyl titanate, all-silicon β molecular sieve seed crystals, tetraethylammonium hydroxide and deionized water at 60°C to obtain a molar ratio of SiO 2 :TiO 2 : Seed crystal: Structure directing agent: H 2 O=1:0.03:0.8:1.3:20 alkaline mixed solution, and then press the mineralizer: SiO 2 =0.8 molar ratio, add sodium fluoride to the above mixed solution and stir to obtain OH - :SiO 2 About 1.3 Ti-β molecular sieve precursor.

[0063] After transferring the colloid to a pressure-resistant closed reactor, under agitation, the crystallization system was heated to 135°C and kept at a constant temperature under autogenous pressure for 10 days to obtain a mixture of crystalline products; this mixture was filtered and washed with water. After all; drying at a temperature of 110°C for 6 hours and then roasting at a temperature of 550°C for 5 hours to obtain Ti-β molecular sieve. The XRD spectrum of the molecular sieve is as fol...

Embodiment 2

[0065] Under stirring conditions, mix methyl orthosilicate, tetrapropyl titanate, all-silicon β molecular sieve seed crystals, diethylamine, deionized water, and external alkali source ammonia at 40°C to obtain a molar ratio of SiO 2 :TiO 2 : Seed crystal: Structure directing agent: H 2 O=1:0.01:0.02:0.25:5 alkaline mixed solution, and then according to mineralizer: SiO 2 = 0.015 molar ratio, add sodium hydroxide to the above mixed solution and stir to obtain OH - :SiO 2 =0.35 Ti-β molecular sieve precursor.

[0066] After transferring the colloid to a pressure-resistant closed reactor, under stirring, the crystallization system was heated to 110°C and kept at a constant temperature under autogenous pressure for 15 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 12 hours and then calcining at a temperature of 450°C for 10 hours to obtain Ti-β molecular sieve.

Embodiment 3

[0068] Under stirring conditions, mix silica gel, tetraethyl titanate, all-silicon β molecular sieve seed crystals, tetraethylammonium fluoride, deionized water, and additional alkali source sodium hydroxide at 80°C to obtain a molar ratio of SiO 2 :TiO 2 : Seed crystal: Structure directing agent: H 2 O=1:0.06:1.5:2.5:50 alkaline mixed solution, and then press the mineralizer: SiO 2 =2 molar ratio, add sodium bromide to the above mixed solution and stir to obtain OH - :SiO 2 = 2 Ti-β molecular sieve precursor.

[0069] After transferring the colloid to a pressure-resistant closed reactor, under stirring conditions, the crystallization system was heated to 190°C and kept at a constant temperature under autogenous pressure for 0.5 days to obtain a mixture of crystalline products; this mixture was filtered and washed with water. After all; drying at a temperature of 130°C for 2 hours and then roasting at a temperature of 600°C for 3 hours to obtain Ti-β molecular sieve.

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Abstract

The invention discloses a Ti-beta molecular sieve and a synthesis method and application thereof. The synthesis method of the Ti-beta molecular sieve includes the following steps that 1, a silicon source, a titanium source, a seed crystal, an alkali metal compound mineralizer, a structure-directing agent, water and an optional alkali source are mixed evenly, and a reaction mixture in a certain molar ratio is obtained, wherein the seed crystal is an all-silicon beta molecular sieve; 2, the reaction mixture obtained in the step 1 is crystallized for 0.1-20 days at the temperature of 90-230 DEG C and the self-generated pressure in a pressure-resistant closed vessel, and a crystallization product is obtained; 3, the crystallization product obtained in the step 2 is recovered. According to the technical scheme, by adding the seed crystal and the alkali metal compound mineralizer, the Ti-beta molecular sieve which has few framework defects, is uniform in particle size and has good catalytic performance in a macromolecule reaction is prepared under the alkaline condition.

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] Beta molecular sieve is a symbiosis of stacking faults composed of three closely related polymorphs. It has a three-dimensional twelve-membered ring pore structure, in which the pores in the [100] and [010] directions are straight pores, and their pore diameters are about 0.66×0.67nm; the pores in the [001] direction are composed of [100] and [010] ] The cross of straight channels in two d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04B01J29/70C07D301/19C07D303/06
Inventor 王宝荣林民彭欣欣朱斌舒兴田
Owner CHINA PETROLEUM & CHEM CORP
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