Synthetic method of methyl ethyl ketone peroxide with no three wastes produced

A technology of methyl ethyl ketone peroxide and a synthesis method, applied in the field of methyl ethyl ketone peroxide synthesis, can solve problems such as three wastes, and achieve the effects of solving the problems of three wastes, stable reaction process, and eliminating potential safety hazards

Active Publication Date: 2019-05-24
淄博圣马化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at the technical defects of the prior art, and provides a method for synthesizing methyl ethyl ketone peroxide without producing three wastes, so as to solve the technical problem that the conventional synthesis method of methyl ethyl ketone peroxide will produce three wastes

Method used

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  • Synthetic method of methyl ethyl ketone peroxide with no three wastes produced
  • Synthetic method of methyl ethyl ketone peroxide with no three wastes produced
  • Synthetic method of methyl ethyl ketone peroxide with no three wastes produced

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] In a 250ml four-necked bottle equipped with stirring, a thermometer, and a dropping funnel, sequentially add 90g (1.323mol) of 50% hydrogen peroxide and 15.0g of 99.5% dimethyl phthalate. Under the condition of stirring, control the temperature of the reaction system at 20-22°C through an external constant temperature water bath, and then slowly add 50.5g (0.700mol) of methyl ethyl ketone to the system through the dropping funnel, and the dropping time is maintained at 2.0h After the dropwise addition, continue to stir and react at this temperature for 1.0h. After the reaction is completed, add 45g of ethylene glycol and 0.004g of product stabilizer to the system under stirring conditions, and continue stirring for 10 minutes until the stabilizer is completely Dissolved to obtain 200 g of the product with an active oxygen content of 9.81%.

Embodiment 2

[0023] In a 250ml four-necked bottle equipped with stirring, a thermometer, and a dropping funnel, sequentially add 15.0g of 99.5% dimethyl phthalate, 50.5g (0.700mol) of methyl ethyl ketone, complete the addition, start stirring, and Under stirring conditions, drop 0.3g of 60-65% nitric acid into the system, then pass through an external constant temperature water bath, control the temperature of the reaction system at 20-22°C, and then slowly add 90g (1.323 mol) 50% hydrogen peroxide, the dropping time is maintained at about 2.0h. After the dropping is completed, continue to stir and react at this temperature for 1.0h, then stop stirring, keep warm for 0.5h, and separate out about 33.0g of water. , start stirring again, under stirring condition, add ethylene glycol 50.0g, product stabilizer 0.004g to the system, continue to stir for 10 minutes, dissolve completely to stabilizer, obtain product amount 172.8g, active oxygen content 9.82%.

Embodiment 3

[0025] In a 250ml four-necked bottle equipped with stirring, a thermometer, and a dropping funnel, sequentially add 15.0g of 99.5% dimethyl phthalate, 50.5g (0.700mol) of methyl ethyl ketone, complete the addition, start stirring, and Under the condition of stirring, add 0.3g of 95-98% sulfuric acid dropwise, then through an external constant temperature water bath, control the temperature of the reaction system at 20-22°C, then slowly add 90g (1.323mol) of 50 % hydrogen peroxide, the dropping time is maintained at about 2.0h. After the dropping is completed, continue to stir and react at this temperature for 1.0h, then stop stirring, keep the temperature for 0.5h, until the system has clear layers and 37.0g of water is separated, start again Stir, under stirring condition, add ethylene glycol 54.0g, product stabilizer 0.004g to the system, continue to stir for 10 minutes, until stabilizer dissolves completely, obtain product 172.3g, active oxygen content 9.82%.

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Abstract

The invention provides a synthetic method of methyl ethyl ketone peroxide with no three wastes produced. According to the technical scheme, hydrogen peroxide and butanone are subjected to reaction through reverse dropping of butanone by using dimethyl phthalate as a solvent; after reaction, a hydrophilic solvent is added into the reaction product so that a finished liquid is homogenous. The synthetic method has the advantages that the technical prejudice, where mixing butanone and a solvent is before the adding of an acid catalyst and the dropping of hydrogen peroxide, in the traditional synthetic method is broken through; the method, where hydrogen peroxide is used as a base material and acidity of the hydrogen peroxide is utilized to allow autonomous catalysis, is utilized, adding otheracids is not required by the method, butanone is subjected as a raw material to reaction with dimethyl phthalate acting as a solvent, no water is required after reaction, a fixed quantity of one solvent is added to the system before a stabilizer mixture is added, and mixing well is just required; the reaction process is very stable, no three wastes are produced during the synthesis of the finishedproduct, and the finished product has very good stability and good service performance.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for synthesizing methyl ethyl ketone peroxide without generating three wastes. Background technique [0002] Methyl ethyl ketone peroxide is an initiator of unsaturated polyester resin, which has an important influence on the properties of unsaturated polyester resin. Unsaturated polyester resin is an important class of polymer materials, with an output of one million tons and a wide range of applications, including more than a dozen fields such as aircraft, high-speed rail, ships, yachts, wind power, and FRP anti-corrosion materials. In the synthesis of polyester resin materials, more than 90% of the varieties use methyl ethyl ketone peroxide as the initiator. It can be seen that the demand for methyl ethyl ketone peroxide products in the polyester industry is not only very large, but also very dependent. [0003] The traditional synthetic method of methyl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/22
Inventor 谭立哲王云峰孙营梁岳
Owner 淄博圣马化工有限公司
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