Method for synthesizing Ti-MWW molecular sieve hollow sphere with high external specific surface area

A specific surface area and synthesis method technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of cumbersome method process and achieve the effects of improving uniformity, promoting rapid and high-quality nucleation, and excellent catalytic activity

Inactive Publication Date: 2016-02-17
HUBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses polystyrene microspheres (Chem.Commun.,2000,2161), mesoporous silicon (Chem.Mater.,2002,14,3217), carbon black microspheres (Chem.Mater.,2010,22,2757 ;) etc. as a sacrificial template agent, synthesized silicalite-1, MCM-22 and other molecular sieve hollow spheres, but the process of this method is cumbersome, and the hard template agent must be removed by post-processing such as calcination

Method used

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  • Method for synthesizing Ti-MWW molecular sieve hollow sphere with high external specific surface area
  • Method for synthesizing Ti-MWW molecular sieve hollow sphere with high external specific surface area
  • Method for synthesizing Ti-MWW molecular sieve hollow sphere with high external specific surface area

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Embodiment 1

[0034] At room temperature, add a certain amount of organic amine to a certain amount of water, stir for half an hour, then add titanium source, boron source and stir evenly, then add a certain amount of silicon source to obtain a reaction gel, the gel molar composition is 0.04 TiO 2 : 1.0 SiO 2 : 0.67B 2 o 3 : 1.5 organic amine: 25.0H 2 O. Such as figure 2 As shown, the reaction gel is placed in a closed reactor 3, and the closed reactor 3 is fixed on the horizontal rotating shaft 1 of the homogeneous reactor through a connecting rod 2, and the rotation rate is adjusted to 40 revolutions per minute, and it is first aged at 90°C 14 hours. Then adjust the rotation rate to 60 rpm, crystallize at 185°C for 46 hours, filter, wash and dry to obtain the original powder of Ti-MWW molecular sieve, the titanium source is n-butyl titanate, and the silicon source is silicon dioxide, the boron source is boric acid, and the organic amine is piperidine. Mix the obtained molecular s...

Embodiment 2～10

[0036] Implementation process except following difference, all the other are all the same as embodiment 1, see table 1.

[0037] Table 1

[0038]

[0039] In other embodiments, according to the technical solution provided by the present invention, the ratio of raw materials is adjusted within the given range, and the performance of the obtained product is equivalent, which all conform to the technical idea of ​​the present invention.

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Abstract

The invention belongs to the technical field of chemical synthesis, and particularly relates to a method for synthesizing a Ti-MWW molecular sieve hollow sphere with the high external specific surface area. The method includes the steps that reactive gel is rotated along a horizontal rotating shaft in an airtight reaction still, rotary ageing is conducted for a period of time at a certain temperature first, then rotary crystallization is carried out for a period of time at a certain temperature, and the Ti-MWW molecular sieve hollow sphere can be synthesized by reasonably adjusting the rotating speed. By the adoption of the method, a Ti-MWW molecular sieve of the hollow sphere structure can be synthesized through one step, a sacrificial template in a hard template method does not need to be used, the external specific surface area can reach up to 180-260 m<2> / g, and excellent catalytic activity can be achieved in epoxidation reactions for catalyzing chloropropene, cyclopentene, cyclohexene, cyclooctene and H2O2 (or TBHP).

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing Ti-MWW molecular sieve hollow spheres with high external specific surface area. Background technique [0002] Molecular sieve hollow sphere is an important member of the family of graded pore molecular sieves, with a micropore-macropore composite structure. The macroporous structure can not only shorten the diffusion path of the reaction substrate and accelerate mass transfer, but also greatly improve the carbon deposition problem of traditional microporous molecular sieves and increase the recycling performance of the catalyst. Therefore, the development of microporous-macroporous molecular sieve materials has become a hot and difficult research topic in recent years. [0003] At present, the synthesis method of molecular sieve hollow spheres is the hard template method. This method uses polystyrene microspheres (Chem.Commun.,20...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08
Inventor 周丹章天骏夏清华
Owner HUBEI UNIV
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