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Preparation method and application of anhydrous peroxycarboxylic acid

An anhydrous peroxycarboxylic acid and carboxylic acid technology, applied in electrolysis process, organic chemistry, electrolysis components, etc., can solve the problem of unsuitability for ε-caprolactone, etc., and achieve high reaction yield, mild reaction conditions, and high yield. high rate effect

Active Publication Date: 2022-02-11
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN108047113A has prepared peracetic acid by using acetic acid and hydrogen peroxide, but because the catalyst is sulfuric acid, ε-caprolactone will be polymerized in the presence of sulfuric acid, which is also not suitable for the production of ε-caprolactone

Method used

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  • Preparation method and application of anhydrous peroxycarboxylic acid

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Weigh 500g of methyl butyrate and 25g of 10wt% hydrogen peroxide and add them to the flask. A water separator is installed on the flask, and a condenser is installed on the water separator. Magnetic stirring, control the pressure 5kPa, heat the flask to raise the temperature, the gas phase flows through the water separator after being condensed by the condenser tube, the water is separated through the water separator, and the rest of the condensate flows back into the flask. When the temperature in the flask gradually increased to 28.6°C and remained constant, the heating was stopped, and the vacuum was broken after the system temperature returned to room temperature.

[0037] Transfer all the materials in the above flask to the electrolytic cell, weigh 0.50 g of cobalt acetate, 0.50 g of platinum acetate and 6.48 g of butyric acid into the electrolytic cell, and start stirring to mix the materials in the electrolytic cell evenly. Then, the anode (platinum electrode, 2....

Embodiment 2

[0039] Weigh 500g of ethyl propionate and 166.67g of 50wt% hydrogen peroxide and add them to the flask. A water separator is installed on the flask, and a condenser is installed on the water separator. Magnetic stirring is used to control the pressure to 30kPa, and the flask is heated to raise the temperature. The gas phase is condensed by the condenser tube and then flows through the water separator. The water is separated through the water separator, and the rest of the condensate is returned to the flask. When the temperature in the flask gradually increased to 65.2°C and remained constant, the heating was stopped, and the vacuum was broken after the system temperature returned to room temperature.

[0040] Transfer all the materials in the above flask to the electrolytic cell, weigh 2.50g of silver acetate, 0.50g of ruthenium acetate and 363.03g of propionic acid and add them to the electrolytic cell, start stirring to mix the materials in the electrolytic cell evenly. The...

Embodiment 3

[0042] Weigh 500g of propyl acetate and 41.67g of 30wt% hydrogen peroxide and add them to the flask. A water separator is installed on the flask, and a condenser is installed on the water separator. Magnetic stirring is used to control the pressure to 18kPa, and the flask is heated to raise the temperature. The gas phase is condensed by the condenser tube and then flows through the water separator. The water is separated through the water separator, and the rest of the condensate flows back into the flask. When the temperature in the flask gradually increased to 54.5°C and remained constant, the heating was stopped, and the vacuum was broken after the system temperature returned to room temperature.

[0043]Transfer all the materials in the above-mentioned flask to the electrolytic cell, weigh 0.83g of nickel acetate, 0.50g of iridium acetate and 33.11g of acetic acid into the electrolytic cell, start stirring to mix the materials in the electrolytic cell evenly. Then, the ano...

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Abstract

The invention provides a preparation method and application of anhydrous peroxycarboxylic acid. The preparation method comprises the following steps: carrying out reduced pressure dehydration and pre-concentration on low-concentration hydrogen peroxide, adding a catalyst a and a catalyst b, adding carboxylic acid, and carrying out electrolytic oxidation reaction to synthesize the anhydrous peroxycarboxylic acid. According to the method, the oxidation reaction effect is enhanced through the synergistic effect of electrons and metal salt, no pollution is caused, the requirement of green synthetic chemistry is met, and the prepared peroxycarboxylic acid does not contain water and can be used for preparing epsilon-caprolactone.

Description

technical field [0001] The invention relates to the technical field of peroxycarboxylic acid synthesis, in particular to the preparation of anhydrous peroxycarboxylic acid by an electrochemical method and its application. Background technique [0002] ε-caprolactone, also known as 6-caprolactone, is composed of 5 methylene groups (-CH 2 -) and a seven-membered cyclic lactone composed of an ester group (-COO-). As a synthetic monomer of biodegradable polycaprolactone (PCL), ε-caprolactone has always been a research hotspot in the field of polymer material development. However, my country has been in a relatively backward situation in terms of large-scale production of ε-caprolactone for a long time, which has delayed the development and promotion of downstream products. [0003] There are many ways to synthesize ε-caprolactone, but the most commonly used method is cyclohexanone oxidation, which can be further divided into: peroxyacid oxidation, H 2 o 2 Oxidation method, O...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/07C25B3/23C07D313/04
CPCC25B3/23C25B3/07C07D313/04
Inventor 林龙李文滨翟文超吕英东张涛王磊黎源
Owner WANHUA CHEM GRP CO LTD
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