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Titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction

A titanium-silicon molecular sieve, TS-1 technology, applied in the direction of molecular sieve catalysts, physical/chemical process catalysts, catalyst activation/preparation, etc., can solve the problems of difficult separation and recycling, poor repeatability and stability, and high synthesis cost. Reduce production costs, improve activity, and improve activity

Inactive Publication Date: 2010-06-30
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0018] In order to solve the problems in the prior art that the particles are small, difficult to separate and recycle, in addition, the synthesis cost is high, the glue making process requires strict and complex requirements, poor repeatability and stability, etc., the present invention provides a new catalyst for ketone Titanium-silicon molecular sieve TS-1 catalyst for oximation reaction, using cheap inorganic titanium source and inorganic silicon source hydrothermally synthesized titanium-silicon molecular sieve TS-1 raw powder, the synthesis process is simple, greatly reducing its production cost; the prepared titanium Silicon molecular sieve TS-1 catalyst has large particles (2um-10um), which is easy to separate and recover after reaction, and can increase the reuse rate; it is especially suitable for modifying the original powder of titanium silicon molecular sieve TS-1 after hydrothermal crystallization again It is suitable for the ammoximation reaction of ketones with hydrogen peroxide as the oxidant, without by-products, and is an environmentally friendly process, which is beneficial to industrial applications

Method used

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  • Titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction
  • Titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction
  • Titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0048] The preparation of TS-1 was carried out according to Comparative Example 1. Dissolve 2gTPAOH in 100ml of deionized water, mix evenly, take 30ml of the interpretation solution and mix it with 2g of TS-1, move it to a sealed crystallization kettle, react for 48 hours at a temperature of 170°C and autogenous pressure, take it out, filter, After washing with deionized water to neutrality, drying at 120°C for 12h, and calcining at 550°C for 6h, the TPAOH-modified TS-1 catalyst was prepared.

Embodiment 2

[0050] The preparation of TS-1 was carried out according to Comparative Example 2. Ammonia water (mass fraction 25%, 1.29mol / L) is diluted to 10 times solution with deionized water, after getting 30ml of explaining solution and 2g TS-1 mix uniformly, move to sealed crystallization kettle, in 170 ℃ React at temperature and autogenous pressure for 48 hours, take it out, filter, wash with deionized water until neutral, dry at 120°C for 12 hours, and roast at 550°C for 5 hours to prepare ammonia modified TS-1 catalyst.

Embodiment 3

[0052] The preparation of TS-1 was carried out according to Comparative Example 1. Dissolve 7.76g of urea in 100ml of deionized water, mix evenly, take 30ml of the interpretation solution and mix it with 2g of TS-1, move it to a sealed crystallization kettle, react for 48 hours at a temperature of 170°C and autogenous pressure, take it out, and After filtering, washing with deionized water until neutral, drying at 120°C for 12h, and then calcining at 550°C for 5h, the urea-modified TS-1 catalyst was prepared

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Abstract

The invention relates to a titanium-silicon molecular sieve TS-1 catalyst for catalyzing ketone oximation reaction. In order to solve the problems of small particles, difficult separation and reutilization, high synthesis cost, strict and complex requirements in the process of gluing, poor repeatability and stability and the like in the prior art, the invention provides a new titanium-silicon molecular sieve TS-1 catalyst for the catalyzing ketone oximation reaction, which is prepared from the following steps: mixing the titanium-silicon molecular sieve TS-1 with one or more solutions of organic amine, ammonium salt, ammonia water and urea, carrying out crystallization again under the self-generating hydro-thermal pressure, and filtering, washing, drying and roasting to obtain the product. The prepared titanium-silicon molecular sieve TS-1 catalyst has large particles and easy separation and recovery after reaction, can improve the reutilization ratio, is especially suitable for ketone oximation reaction using hydrogen peroxide as an oxidizing agent, and can not produce byproducts, thereby protecting the environment and being beneficial to industrial application.

Description

technical field [0001] The invention relates to a titanium silicon molecular sieve TS-1 catalyst used for catalyzing the oximation reaction of ketones. Background technique [0002] Titanium-silicon molecular sieves had related patent reports as early as 1967, but they were not taken seriously because the author did not give sufficient data to characterize the crystal structure. Until the early 1980s, Italian Taramasso et al. patented GB207107A (1981) and USP4,410,501 ( 1983) publicly reported the synthesis of MFI-type structure TS-1 molecular sieve, followed by Ti-ZSM-11, Ti-Beta, Ti-MOR, Ti-ITQ-7 and Ti-MWW with microporous structure and mesoporous structure Ti-MCM-41, Ti-HMS, Ti-MSU and Ti-SBA-15, etc., this type of molecular sieve can selectively oxidize a variety of organic compounds, such as: olefin epoxidation, alcohol oxidation, alkane partial oxidation, phenol Hydroxylation, aromatic hydrocarbon epoxidation, ketone oximation, etc. In particular, titanium-silicon m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J37/10C07C249/04C07C251/44C07C251/38
Inventor 周继承张红莉黄先亮
Owner XIANGTAN UNIV
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