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Process for producing oxime

A technology of ammoximation reaction and titanosilicate, applied in oxime preparation, organic chemistry, etc., can solve problems such as complexity, long catalyst preparation process, unsatisfactory conversion rate selectivity, etc., and achieve low cost and high yield rate effect

Inactive Publication Date: 2011-08-17
SUMITOMO CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, in the method disclosed in Patent Document 1, since the performance of the catalyst is insufficient, it is unsatisfactory in the conversion rate of ketone and the selectivity rate of oxime
In addition, the method disclosed in Patent Document 2 is unsatisfactory in terms of cost because the preparation process of the catalyst is long and complicated.

Method used

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  • Process for producing oxime
  • Process for producing oxime
  • Process for producing oxime

Examples

Experimental program
Comparison scheme
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Embodiment 1

[0060] (preparation of catalyst)

[0061] Put 9.1 kg of piperidine, 25.6 kg of pure water, 6.2 kg of boric acid, 0.54 kg of tetra-n-butyl orthotitanate, and fumed silica ("CAB-O-SIL M-7D" manufactured by CABOT) in an autoclave. 4.5kg, in an air environment, stirred at room temperature to prepare a gel, and aged for 1.5 hours. The autoclave was sealed, and the temperature was raised to 170° C. over 10 hours while stirring, and then kept at the same temperature for 168 hours to carry out hydrothermal synthesis to obtain a suspension. The suspension was filtered, and the filter residue was washed with water until the pH of the washing liquid was close to 10, and then dried at 50° C. to finally obtain a white powder in a water-containing state.

[0062] 3.5 L of 13% by weight nitric acid was added to 350 g of this water-containing white powder, and the mixture was refluxed for 20 hours. Next, filter, wash the filter residue with water until the washing solution is nearly neutral...

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Abstract

To provide a method for inexpensively producing an oxime in high yield by carrying out ammoximation reaction of a ketone by using a catalyst which has excellent properties and can be prepared advantageously in cost. The method for producing the oxime involves subjecting the ketone to the ammoximation reaction with a peroxide and ammonia in the presence of a titanosilicate exhibiting an X-ray diffraction pattern having peaks at the following positions shown as lattice plane spacings: lattice spacing d( 1 / 2 A): 13.2+-0.6; 12.3+-0.3; 11.0+-0.3; 9.0+-0.3; 6.8+-0.3; 3.9+-0.2; 3.5+-0.1; and 3.4+-0.1.

Description

technical field [0001] The present invention relates to a method for preparing oximes by ammoximation reaction of ketones. Oximes can be used as raw materials for amides or lactams, and the like. Background technique [0002] As one of the methods for producing oximes, there is known a method of subjecting ketones to ammoximation reaction using titanosilicate as a catalyst. For example, JP-A-62-59256 (Patent Document 1) discloses a method of performing the above-mentioned ammoximation reaction using titanium silicate (titanium silicalite TS-1) having an MFI structure as a catalyst. In addition, International Publication No. 03 / 074421 pamphlet (Patent Document 2) discloses a method of performing the above-mentioned ammoximation reaction using a titanosilicate having a MWW structure as a catalyst. [0003] [Patent Document 1] JP-A-62-59256 [0004] [Patent Document 2] International Publication No. 03 / 074421 Pamphlet [0005] However, in the method disclosed in Patent Docum...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/04C07C251/32
CPCC07C249/06C07C249/14C07C251/32
Inventor 老川幸深尾正美
Owner SUMITOMO CHEM CO LTD