A kind of titanium-containing silicon molecular sieve catalyst and its preparation method and application

A technology of titanium-silicon molecular sieves and catalysts, which is applied in molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of poor catalytic performance and deactivation of titanium-silicon molecular sieves, and achieve good activity and activity stability , energy saving and pollution reduction effect

Active Publication Date: 2020-08-18
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, usually after a period of operation, the catalytic performance of titanium-silicon molecular sieves will deteriorate and deactivation will occur.

Method used

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  • A kind of titanium-containing silicon molecular sieve catalyst and its preparation method and application

Examples

Experimental program
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Effect test

preparation example Construction

[0015] As mentioned above, the present invention provides a method for preparing a titanium-containing silicon molecular sieve catalyst. The method includes: (1) contacting the unloading agent with an organic compound to obtain a contacted product, and the organic compound is selected from sulfone and ketone And one or more of amides, the unloading agent is the unloading agent of the reaction device with titanium silicate molecular sieve as the active component of the catalyst; (2) in the presence of an aqueous solvent, mixing the contacted product alkali source After that, hydrothermal treatment is performed.

[0016] According to the method of the present invention, the purpose of the present invention can be achieved by following the aforementioned scheme. Organic compounds meeting the aforementioned requirements can be used in the present invention. For the present invention, the organic compounds are preferably sulfoxides, sulfones, alkanones and amides. One or more of.

[00...

Embodiment approach

[0050] According to a preferred embodiment of the present invention, preferably the alkali source is ammonia, sodium hydroxide, potassium hydroxide, calcium hydroxide, lithium hydroxide, sodium carbonate, potassium carbonate, tetrapropylammonium hydroxide, tetraethyl One of ammonium hydroxide, tetramethylammonium hydroxide, tetrabutylammonium hydroxide, ethylamine, n-propylamine, n-butylamine, di-n-propylamine, butanediamine, hexamethylenediamine, monoethanolamine, diethanolamine and triethanolamine Or multiple. Various situations are, for example, a mixture of tetraethylammonium hydroxide and n-butylamine, a mixture of ethylenediamine and tetrapropylammonium hydroxide, a mixture of di-n-propylamine and tetrapropylammonium hydroxide, and tetraethylhydroxide. The mixture of ammonium and tetrapropylammonium hydroxide, and the mixture of hexamethylenediamine and tetrapropylammonium hydroxide can be used in the present invention, and there is no special requirement for the above-me...

Embodiment 1

[0066] Under normal pressure at 90℃, mix and contact dimethyl sulfoxide with the unloading agent (SH-1) for 5.5h, where the weight ratio of the unloading agent to dimethyl sulfoxide is 1:10, filter and wash with water Obtain the solid product after contact, and then dry it to constant weight at 180°C;

[0067] After mixing the dried solid and the aqueous ammonia solution at pH 10, hydrothermal treatment at 170℃ for 15h, the mass ratio of solid to ammonia is 50:1, filtering, washing and drying (120℃) to constant weight, and recovering molecular sieve A. The activity, relative crystallinity, and specific surface area of ​​the micropores are shown in Table 1 (the activity determination method is consistent with the method and procedure for measuring the fresh agent, and the cyclohexanone conversion rate measured at the first hour is used as the activity).

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Abstract

The invention belongs to the field of titanium silicon molecular sieve, and more specifically provides a preparation method of a titanium silicon-containing molecular sieve catalyst. The preparation method comprises following steps: 1, a discharge agent is contacted with an organic compound so as to obtain a contact product, wherein the organic compound is one or a mixture of a plurality of ingredients selected from sulphone, ketone, and acidamide, and the discharge agent is a discharge agent of a reaction device taking titanium molecular sieve as a catalyst active component; 2, in the presence of a water-containing solvent, the contact product and an alkali source are mixed and are subjected to hydro-thermal reaction. The catalyst is obtained via the preparation method. The invention alsoprovides applications of the titanium silicon-containing molecular sieve catalyst in oxidation reaction. The relative crystallinity and the micropore specific area of the titanium silicon molecular sieve in the discharge agent are recovered, and the organic compound can be recycled via simple separation, so that environment pollution caused by the preparation process is reduced. High temperatureis not needed in recycling, energy consumption is reduced effectively, and the titanium silicon-containing molecular sieve catalyst is especially suitable for industrial applications.

Description

Technical field [0001] The invention relates to a titanium-containing silicon molecular sieve catalyst, and a preparation method and application thereof. Background technique [0002] Titanium silicate molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. So far, there have been synthesized TS-1 with MFI structure, TS-2 with MEL structure, and TS-48 with larger pore structure. This type of molecular sieve has excellent selective oxidation performance and high catalytic activity for many organic oxidation reactions, such as olefin epoxidation, aromatic hydroxylation, cyclohexanone oximation, alcohol oxidation and other reactions. They are used as redox molecular sieves. The catalyst has good application prospects. [0003] Among them, TS-1 molecular sieve is a new type of titanium silicate molecular sieve with excellent catalytic and selective oxidation performance formed by introducing transition metal element titanium into the molecular sieve ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/89B01J29/90
Inventor 林民史春风朱斌
Owner CHINA PETROLEUM & CHEM CORP
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