Synthesis method of Ti-Beta molecular sieve

A molecular sieve and anion technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of poor stability and hydrophobicity, and achieve the effects of improving catalytic activity, wide silicon-titanium ratio, and wide range

Inactive Publication Date: 2013-11-20
SHANXI DATONG UNIV
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  • Abstract
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  • Application Information

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Problems solved by technology

However, there are many defects in the unit cell structure in the synthesized Ti-Beta molecular sieve, resulting in poor stability and hydrophobicity.
[0006] There is also an indirect synthesis method for preparing Ti-Beta molecular sieves. For example, U.S. Patent U.S. 5695736 discloses an indirect synthesis method of gas-solid same-crystal substitution. In this method, Beta molecular sieves are first dealuminated to generate skeleton vacancies, and then dealuminated Beta molecular sieves are combined with TiCl 4 The steam reaction allows Ti to enter the framework of Beta molecular sieves. However, the gas-solid isomorphic substitution generally must be carried out at a relatively high temperature (673K), and TiCl 4 It is easy to hydrolyze to form acid mist of HCl and easily produce TiO 2 species

Method used

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  • Synthesis method of Ti-Beta molecular sieve
  • Synthesis method of Ti-Beta molecular sieve
  • Synthesis method of Ti-Beta molecular sieve

Examples

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Embodiment 1

[0020] , Preparation of structure directing agent N, N-diethylpiperidine quaternary ammonium base

[0021] Dissolve 43.6 g (0.38 mol) of N-ethylpiperidine in 140 ml of acetone, add excess bromoethane (63.4 g, 0.58 mol), stir at room temperature for 30 h, filter out the solid, wash with acetone, and vacuum After drying, 79.6 g (0.356 mol) of N, N-diethylpiperidine bromide were obtained. Its chemical structure was confirmed by NMR spectrum, IR spectrum and elemental analysis. Dissolve 79.6 g (0.356 mol) N, N-diethylpiperidine bromide in 700 g deionized water, add excess silver oxide (Ag 2 (0) 124.6 g (0.54 mol), after stirring the mixture at room temperature for 24 hours, the mixture was filtered to obtain an aqueous solution of N, N-diethylpiperidine quaternary ammonium base, which was then rotary evaporated at 50 ° C for 3.5 hours, passed through 0.1 mol · L -1 The concentration of the solution was determined by hydrochloric acid titration, and the concentration of N, N-d...

Embodiment 2

[0025] , Preparation of structure directing agent N, N-diethylpiperidine quaternary ammonium base

[0026] Dissolve 51.6 g (0.45 mol) of N-ethylpiperidine in 150 ml of acetone, add excess bromoethane (81.75 g 0.75 mol), stir at room temperature for 18 h, filter out the solid, wash with acetone, and dry in vacuo , to obtain 96.6 g (0.432 mol) of N, N-diethylpiperidine bromide. Its chemical structure was confirmed by NMR spectrum, IR spectrum and elemental analysis. Then 96.6 g (0.432 mol) of N, N-diethylpiperidine bromide was dissolved in 1000 g of deionized water, 149.9 g (0.65 mol) of excess silver oxide was added, and the mixture was stirred at room temperature for 24 hours. After stirring, the mixture was filtered to obtain an aqueous solution of N, N-diethylpiperidine quaternary ammonium base, which was then rotary evaporated at 50 °C for 4 hours, passed through 0.1 mol L -1 The concentration of the solution was determined by hydrochloric acid titration, and the concen...

Embodiment 3

[0030] , Preparation of structure directing agent N, N-diethylpiperidine quaternary ammonium base

[0031] Dissolve 36.7 g (0.32 mol) of N-ethylpiperidine in 100 ml of acetone, add excess bromoethane (50.3 g, 0.46 mol), stir at room temperature for 36 h, filter out the solid, wash with acetone, and dry in vacuo , to obtain 64.8 g (0.29 mol) of N, N-diethylpiperidine bromide. Its chemical structure was confirmed by NMR spectrum, IR spectrum and elemental analysis. Then 64.8 g (0.29 mol) of N, N-diethylpiperidine bromide was dissolved in 500 g of deionized water, 117.6 g (0.51 mol) of excess silver oxide was added, and the mixture was stirred at room temperature for 24 hours. After stirring, the mixture was filtered to obtain an aqueous solution of N, N-diethylpiperidine quaternary ammonium base, which was then rotary evaporated at 50 °C for 3 hours, passed through 0.1 mol L -1 The concentration of the solution was determined by hydrochloric acid titration, and the concentra...

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Abstract

The invention discloses a synthesis method of a Ti-Beta molecular sieve. The method includes: taking N, N-diethylpiperidine quaternary ammonium base as a structure directing agent, mixing a silicon source, a titanium source, a fluorine anion (F<->) source with N, N-diethylpiperidine quaternary ammonium base (R) and water, then subjecting the reaction mixture to hydrothermal crystallization for 3-25 days at 120-180DEG C, then washing, drying and roasting the product, thus obtaining the Ti-Beta molecular sieve. During synthesis of the invention, the range of the gel Si-Ti ratio is wide, and the synthesized Ti-Beta molecular sieve has a wide Si-Ti ratio. No miscellaneous crystal is generated, and the synthesized Ti-Beta molecular sieve does not contain aluminum and non-framework titanium. Especially, the Ti-Beta molecular sieve with a higher framework titanium content can be synthesized, thus being conducive to enhancing the catalytic activity.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemistry and catalytic chemistry, and specifically relates to a preparation method of Ti-Beta molecular sieve. Background technique [0002] Titanium-containing molecular sieve is a very good liquid-phase selective oxidation catalyst, which combines the catalytic oxidation of titanium and the shape-selective effect of molecular sieves, and can catalyze the partial oxidation of alkanes, epoxidation of olefins, oxidation of alcohols, and the hydroxyl of phenol and benzene Catalysis and ammonia oxidation of cyclohexanone, etc., thus aroused extensive attention of catalytic workers. They have done a lot of research in this field and synthesized various types of titanium silicon molecular sieves. [0003] Ti-Beta molecular sieve is the only titanium-containing molecular sieve with a three-dimensional twelve-membered ring channel system. Ti-Beta molecular sieve has high catalytic activity. In addi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 刘建红晋春郭永吕存琴孟双明杨国臣乔永生
Owner SHANXI DATONG UNIV
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