In-situ supported forming preparation method of titanium silicon molecular sieve composite catalyst

A composite catalyst, titanium silicon molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc. The problem of high cost is to achieve the effect of enhancing the catalytic efficiency, reducing the possibility of catalyst deactivation, and increasing the specific surface area.

Inactive Publication Date: 2015-04-22
河北美邦工程科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The particle size of TS-1 before molding is small, the loss in the reaction is very serious, and the life of the catalyst is very short, only 34h
The service life of the microsphere TS-1 catalyst prepared by spray molding is increased to more than 148h, but its catalytic performance in the ammoximation reaction of cyclohexanone will be greatly reduced
[0003] Based on the above preparation methods, the prior art TS-1 catalyst mo

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Introduce porous material into silica gel: TiCl 4 : TPABr: Isopropanol: Ammonia: Distilled water with a molar ratio of 1:0.2:0.5:2:5:200 In the hydrothermal synthesis system of TS-1 with MFI topology, the porous material accounts for 8% of the total material weight %;

[0029] (2) Aging the hydrothermal synthesis system obtained in step (1) at 100°C for 24 h, so that the TS-1 with MFI topological structure precipitates crystal nuclei on the surface of the porous material and in the pores, grows in situ, and loads the porous material On, obtain TS-1 composite catalyst intermediate product 1;

[0030] (3) The intermediate product 1 obtained in step (2) was crystallized at 120°C for 240 hours to obtain a mixture of TS-1 composite catalysts. The mixture was separated and dried to obtain TS-1 composite catalyst intermediate product 2:

[0031] (4) The intermediate product 2 obtained in step (3) is in N 2 Calcined at 400°C in atmosphere to make TS-1 composite catalyst....

Embodiment 2

[0035] (1) Introduce porous material into silica sol: TiCl 3 : TPAOH: acetylacetone: ethylamine: distilled water with a molar ratio of 1:0.001:0.5:2:5:200 In the hydrothermal synthesis system of TS-1 with MFI topology, the porous material accounts for 8% of the total material weight %;

[0036] (2) The hydrothermal synthesis system obtained in step (1) was aged at 80°C for 48 h, so that the TS-1 with the MFI topological structure precipitated crystal nuclei on the surface of the porous material and in the pores, and grew in situ, and loaded onto the porous material. In terms of materials, the TS-1 composite catalyst intermediate product 1 was obtained;

[0037] (3) The intermediate product 1 obtained in step (2) was normally crystallized at 150°C for 144 hours to obtain a mixture of TS-1 composite catalysts. The mixture was separated and dried to obtain TS-1 composite catalyst intermediate product 2:

[0038] (4) The intermediate product 2 obtained in step (3) was calcined i...

Embodiment 3

[0042] (1) Introduce porous material into silica: TiOCl 2 : TPABr: Diethylaminoalcohol: Ethylenediamine: Distilled water in a molar ratio of 1:0.001:0.03:2:5:200 In the hydrothermal synthesis system of TS-1 with MFI topology, the porous material accounts for the total material 13.5% by weight;

[0043] (2) Aging the hydrothermal synthesis system obtained in step (1) at 70°C for 72 h, so that the TS-1 with MFI topological structure precipitates crystal nuclei on the surface of the porous material and in the pores, grows in situ, and loads the porous material On, obtain TS-1 composite catalyst intermediate product 1;

[0044] (3) The intermediate product 1 obtained in step (2) was normally crystallized at 180°C for 96 hours to obtain a mixture of TS-1 composite catalysts. The mixture was separated and dried to obtain TS-1 composite catalyst intermediate product 2:

[0045] (4) The intermediate product 2 obtained in step (3) is in N 2 Calcined at 400°C in atmosphere to make TS...

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PUM

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Abstract

The invention relates to an in-situ supported forming preparation method of titanium silicon molecular sieve composite catalyst. The method comprises the steps: (1) introducing a porous system into a TS-1 hydrothermal synthesis system of an MFI topological structure consisting of a silicon source, a titanium source, a template agent, a complexing agent and an alkali source; (2) separating out crystal nucleus from TS-1 on the surface and in pores of the porous material after aging, and loading the crystal nucleus onto the porous material in an in-situ growth manner to obtain an intermediate product 1; (3) crystallizing the intermediate product 1 to obtain a mixture of TS-1 composite catalyst, and separating and drying the mixture to obtain an intermediate product 2; and (4) roasting the intermediate product 2 in a N2 atmosphere to obtain the TS-1 composite catalyst. According to the prepared TS-1 composite catalyst, TS-1 is firmly combined with the porous material, the mechanical strength is high, and the abrasion resistance is good; the TS-1 is in-situ formed in a porous material carrier, so that the specific surface area is increased, and the catalytic efficiency is improved; the process is simple, and the production cost is low; the catalyst is large in particle size and easy to separate, and the service life is prolonged.

Description

technical field [0001] The invention relates to a preparation method of a catalyst, in particular to a preparation method of a titanium-silicon molecular sieve composite catalyst, belonging to the technical field of chemical synthesis. Background technique [0002] Titanium silicate molecular sieve (TS-1) is a commonly used catalyst in the field of chemical synthesis, and TS-1 is usually prepared by hydrothermal synthesis. However, TS-1 prepared by the hydrothermal synthesis method is a fine powder with a grain size ranging from 0.1 to 5 μm, which is difficult to separate from the reaction medium, and cannot meet the requirements of industrial equipment for catalyst strength, life, shape, etc. Therefore, , The molding process of TS-1 is an indispensable step for its industrial application. The traditional TS-1 molding method is secondary molding. Generally, the crystallization solution of the TS-1 precursor synthesized by hydrothermal treatment is washed, centrifuged, roast...

Claims

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Application Information

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IPC IPC(8): B01J29/89C07C249/04C07C251/44
Inventor 刘东张玉妹王素霞
Owner 河北美邦工程科技股份有限公司
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