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A kind of synthetic method of dimethylglyoxime

A technology of diacetyl oxime and diacetyl, which is applied in the field of synthesis of diacetyl oxime, can solve the problems of complicated operation, carcinogenicity, environmental pollution and the like, and achieves the effects of improving production efficiency and reducing reaction steps.

Active Publication Date: 2018-08-24
SHANXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] This method has the following disadvantages: (1) the raw material is highly corrosive (sulfuric acid, hydrochloric acid), inflammable and explosive (ethyl nitrite), carcinogenic (sodium nitrite); (2) the involved reaction is a homogeneous reaction, and the step The reaction requires product separation, and the operation is cumbersome; (3) The discharge of three wastes is large and the environmental pollution is serious
However, so far, research work on this aspect has not been reported

Method used

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  • A kind of synthetic method of dimethylglyoxime
  • A kind of synthetic method of dimethylglyoxime

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Set the constant temperature reaction temperature to 40°C, add 0.5gTS-1, 0.5g diacetyl, and 5.0g ethanol into the there-necked flask, and use a constant pressure dropping funnel to mix 1.1g concentrated ammonia solution (25%) and 1.3g hydrogen peroxide ( 30%) was added three times within 1 h. When the dropwise addition was started, the reaction time was 2h.

Embodiment 2

[0036] Titanium silicate molecular sieve TS-1 is selected as 0.8g, and the others are the same as in Example 1.

Embodiment 3

[0038] Titanium silicate molecular sieve TS-1 is selected as 1.0 g, and the others are the same as in Example 1.

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Abstract

The invention relates to a novel method for synthesizing dimethylglyoxime. The method comprises the following steps: 1) setting the thermostatic reaction temperature to 10-70 DEG C, and adding a catalyst into a solvent ethanol-butanedione mixed liquid, wherein the ethanol is 10-20 times by mass of the butanedione; and 2) adding stronger ammonia water and oxydol into the mixed liquid in the step 1) by 1-3 times within 0.5-1 hour, and reacting for 0.5-6 hours, wherein the mole ratio of the butanedione, oxydol and ammonia water is 1:(2-3.5):(2-4), and the catalyst is a titanium silicon molecular sieve and is 1-4 times by mass of the butanedione. Compared with the prior art, the reaction steps are reduced, thereby implementing one-step synthesis of dimethylglyoxime; the solid powder catalyst can be easily separated from the reaction system, and can be recycled, thereby enhancing the dimethylglyoxime production efficiency to some extent; and the used raw materials have low toxicity and no harm, and the reaction byproduct is water and is almost not hazardous to the environment, thereby satisfying the requirements of green chemical industry.

Description

technical field [0001] The invention relates to a compound with nitrogen and oxygen combination, in particular to a synthesis method of dimethylglyoxime. Background technique [0002] 2,3-Butanedione dioxime (2,3-Butanedione dioxime) is an important chemical reagent, which has important uses in practical production and scientific research. Diacetyl oxime is often used as a chelating agent for the analysis and determination of nickel and palladium; separation of nickel from cobalt and other metals, separation of palladium from tin, gold, rhenium, iridium; and cyanide, nickel, palladium, cobalt, iron Photometric determination of metal ions such as (II) and rhenium (VII). In addition, since the nitrogen atom in the dimethylglyoxime complex is sp2 hybridized, its structure is similar to some biologically important macrocyclic ligands (such as vitamin B12 and myoglobin), and its metal complexes can be used as Model compounds are used in the study of enzymes and catalysts. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C249/04C07C251/38
CPCC07C249/04C07C251/38
Inventor 高鹏飞赵永祥王永钊徐亚琳王永福
Owner SHANXI UNIV