Method for preparing and modifying titanium silicalite molecular sieve catalyst and application of titanium silicalite molecular sieve catalyst in ketone oximation

Abstract

The invention discloses a method for preparing and modifying a titanium silicalite molecular sieve catalyst and application of the titanium silicalite molecular sieve catalyst in ketone oximation. The method comprises the following steps: (1) adding seed crystal into a titanium source, a silicon source, a first template agent, a first alkali source, water and additive which serve as raw materials to prepare a titanium silicalite molecular sieve A by adopting a hydrothermal synthesis method; (2) modifying the titanium silicalite molecular sieve A by using an acidic mixed solution to obtain a molecular sieve B; (3) modifying the molecular sieve B by using a second template agent and a second alkali source or mixed liquid of the second template agent and ammonium salt to obtain a molecular sieve C. The titanium silicalite molecular sieve catalyst prepared by the method can be applied to ketone oximation. According to the method, the synthesis cost of the titanium silicalite molecular sieve can be reduced, non-framework titanium in the molecular sieve can be effectively removed, and the catalyzing performance of the molecular sieve synthesized by a low-price system in a ketone oximation reaction can be remarkably improved.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical synthesis, and in particular relates to a preparation method of a titanium-silicon molecular sieve catalyst with high performance in ketone ammonia oximation. Background technique [0002] Titanium-silicon molecular sieve is a new type of heteroatom molecular sieve developed in the early 1980s. It has a regular and orderly channel structure and a large pore volume and specific surface area. Under mild reaction conditions, titanium-silicon molecular sieves in H 2 o 2 It exhibits unique selective oxidation catalytic performance in the oxidation reaction process of a series of organic compounds in which the aqueous solution is the oxidant. In the mid-1980s, the Italian Montedipe Company first used cyclohexanone, ammonia and H 2 o 2 As a raw material, cyclohexanone oxime is selectively produced by TS-1 catalysis at normal pressure and low temperature. This new process has the advantages...

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Problems solved by technology

However, because the fluorine-containing compounds used in the modification process will cause a certain degree of environmental pollution, its application is greatly restricted.

Patent application CN103214001 discloses a preparation method of a high-performance titanium-silicon molecular sieve catalyst. After the micron-sized titanium-silicon molecular sieve is synthesized by hydrothermal crystallization, it is treated with an alkaline solution and then prepared with a titanium source, an organic template agent and an alkali source. The titanium-containing modifying solution is used to modify it, and finally obtain a high-performance titanium-silicon molecular sieve catalyst. This method solves the problems of high cost, low catalytic activity and poor stability in the preparation of titanium-silicon molecular sieves in the prior art to a certain extent. And the modification process is complicated to operate, which is not conducive to industrial application

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