Method for preparing molecular sieve based catalyst

A molecular sieve and catalyst technology, applied in the field of molecular sieve catalyst and molecular sieve catalyst preparation, can solve the problems of poor catalyst stability, uneven distribution of catalyst active centers, fast deactivation rate, etc., to reduce production cost and production cycle, and achieve excellent selectivity. and stability, the effect of solving mass transfer problems

Inactive Publication Date: 2017-01-11
QINGDAO WINCHANCE TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the uneven distribution of catalyst active centers and poor surface hydrophobicity of Ti-HMS catalytic materials, when organic...

Method used

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  • Method for preparing molecular sieve based catalyst
  • Method for preparing molecular sieve based catalyst
  • Method for preparing molecular sieve based catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] At room temperature and under stirring, add a mixed solution of silicon source tetraethyl orthosilicate, bis(triethoxysilyl)methane and trimethoxysilane, which accounts for 70% of the total amount to be added, to the template agent 16 Alkyltrimethylammonium bromide, mineralizer tetraethylammonium hydroxide and water mixed solution for hydrolysis to form a colorless and transparent solution I; the remaining 30% silicon source tetraethyl orthosilicate, di( Triethoxysilyl)methane and trimethoxysilane are mixed and then fully mixed with titanium source tetrabutyl titanate to form a mixed solution II; at -5°C and under rapid stirring, slowly add solution II to the solution In Ⅰ, a light yellow transparent solution was formed, and continued to stir for 1 hour, which was recorded as solution Ⅲ; solution Ⅲ was transferred to a stainless steel autoclave for crystallization treatment, the crystallization temperature was 140°C, and the crystallization time was 72 hours. The crysta...

Embodiment 2

[0020] Compared with Example 1, only in the molecular sieve preparation process, the amount of tetrabutyl titanate added was reduced. The composition relationship of the amount of each substance is [(CH 3 ) 3 CH 3(CH 2 ) 15 N + ]Br - : [(CH 3 CH 2 ) 4 NH 4 ] + Oh - :Si(OC 2 h 5 ) 4 :(C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 : CH 3 Si(OCH 3 ) 3 :Ti(OC 4 h 9 ) 4 :H 2 O =0.3:0.4:1:0.3:0.1:0.03:10 (molar ratio).

[0021] The ultraviolet-visible (UV-Vis) spectrum of the molecular sieve catalyst has a strong absorption peak around 215 nm, and no absorption peak exists at other wavelengths. Its infrared (FT-IR) spectrum is at 960cm -1 There is an obvious absorption peak. More than 95% of the pores have a pore size greater than 2 nm.

Embodiment 3

[0023] Compared with Example 1, only in the molecular sieve preparation process, reduce (C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 added amount. The composition relationship of the amount of each substance is [(CH 3 ) 3 CH 3 (CH 2 ) 15 N + ]Br - : [(CH 3 CH 2 ) 4 NH 4 ] + Oh - :Si(OC 2 h 5 ) 4 :(C 2 h 5 O) 3 Si-CH 2 -Si(OC 2 h 5 ) 3 : CH 3 Si(OCH 3 ) 3 :Ti(OC 4 h 9 ) 4 :H 2 O =0.3:0.4:1:0.2:0.1:0.04:10 (molar ratio).

[0024] The ultraviolet-visible (UV-Vis) spectrum of the molecular sieve catalyst has a strong absorption peak around 215 nm, and no absorption peak exists at other wavelengths. Its infrared spectrum (FT-IR) is at 960cm -1 There is an obvious absorption peak. More than 95% of the pores have a pore size larger than 2 nm.

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Abstract

The invention relates to a method for preparing a molecular sieve based catalyst. The method comprises the following steps: mixing and hydrolyzing a silicon source, a template agent, a mineralizer, water and ethanol at normal temperature; slowly adding a mixture of a titanium source and the residual silicon source into the hydrolyzed silicon hydroxide solution under rapid stirring, and forming gel; transferring the gel into a crystallization kettle for crystallization; washing, filtering and roasting a crystallized molecular sieve so as to remove the template agent, wherein the calcination temperature is 500-600 DEG C, and the calcination time is 4-6 hours to obtain the composite porous molecular sieve based catalyst. The catalyst is simple in preparation process and high in production efficiency; and moreover, because the molecular sieve structure contains organic functional groups and composite pores with hydrophobic property and carbon deposition resistance, the catalyst is excellent in hydrophobic property and mass transfer performance and high in activity, selectivity and stability, and can be used in the process of producing corresponding epoxides through olefin epoxidation by taking H2O2, ethylbenzene hydroperoxide, isopropylbenzene hydroperoxide, tert-butyl hydroperoxide and the like as oxidizing agents.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of a molecular sieve catalyst, in particular to a method for combining four-coordination active titanium species and Si-(CH 2 ) n1 -Si, Si-O-Si(R 4 ) n2 and Ti-O-Si(R 4 ) n2 In situ assembly into molecular sieve catalysts with composite pore structures. Background technique [0002] Titanium porous molecular sieve materials have good catalytic activity for the selective oxidation of hydrocarbons, the ammoxidation of ketones / aldehydes and the hydroxylation of aromatics, etc., and can be used as catalysts for olefin epoxidation and other reactions, and have broad industrial application prospects . [0003] After searching, the patent US4410501 disclosed the synthesis method of TS-1 molecular sieve for the first time. In the method, a titanium-silicon mixed colloid solution is prepared by using an aqueous solution of tetrapropylammonium hydroxid...

Claims

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Application Information

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IPC IPC(8): B01J29/89C01B39/08C01B39/04C07D301/14C07D303/04
CPCB01J29/89C01B39/04C01B39/085C01P2002/82C01P2002/84C07D301/14C07D303/04
Inventor 苏建丽
Owner QINGDAO WINCHANCE TECH
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