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Method used for preparing methylethyl ketone peroxide by taking acidic ion exchange resin as catalyst

The technology of ion exchange resin and methyl ethyl ketone peroxide is applied in the field of preparation of methyl ethyl ketone peroxide, which can solve the problems of low active oxygen content in the product, high cost of waste acid treatment, serious corrosion of strong acid, etc. high conversion rate

Active Publication Date: 2016-01-13
兰州助剂厂有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In the process of producing methyl ethyl ketone peroxide (referred to as MEKP), it has been prepared from butanone (referred to as MEK) and hydrogen peroxide under the catalysis of sulfuric acid and phosphoric acid at home and abroad, but the disadvantages are: strong acid corrodes the equipment seriously, The cost of waste acid treatment is high; the catalyst is dissolved in the reactant, which is not easy to separate and cannot be reused; the active oxygen content of the product is not high, only about 10%

Method used

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  • Method used for preparing methylethyl ketone peroxide by taking acidic ion exchange resin as catalyst
  • Method used for preparing methylethyl ketone peroxide by taking acidic ion exchange resin as catalyst
  • Method used for preparing methylethyl ketone peroxide by taking acidic ion exchange resin as catalyst

Examples

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Effect test

Embodiment 1

[0023] Example 1. At room temperature, add 5.67g of 30wt% hydrogen peroxide, 0.2g of Amberlyst-15 and 4.6g of dibutyl phthalate into a two-necked flask, stir and mix evenly, and adjust the temperature to about 20°C; slowly drop Add 3.6g butanone, react for 40min, then transfer to the separation funnel and let stand for 30min, separate the water phase and the oil phase, the oil phase is MEKP, the mass is 7.9g. The content of active oxygen in the oil phase was determined by chemical titration method to be 10.73%.

Embodiment 2

[0024] Example 2. At room temperature, add 5.67g of 30wt% hydrogen peroxide, 0.2g of Amberlyst-15 and 4.6g of dibutyl phthalate into a two-necked flask, stir and mix evenly, adjust the temperature to about 30°C, and slowly Add 3.6g butanone dropwise, react for 40min, then transfer to a separating funnel, let stand for 30min, separate the water phase and the oil phase, the oil phase is MEKP with a mass of 7.3g. The content of active oxygen in the oil phase was determined by chemical titration method to be 11.15%.

Embodiment 3

[0025] Example 3. At room temperature, add 5.67g of 30wt% hydrogen peroxide, 0.2g of Amberlyst-15 and 4.6g of dibutyl phthalate into a two-necked flask, stir and mix evenly, adjust the temperature to 30°C, and drop slowly during stirring Add 3.6g butanone, react for 60min, then transfer to a separating funnel, let it stand for 30min, separate the water phase and the oil phase, the oil phase is MEKP, the mass is 7.9g. The active oxygen content in the oil phase was determined to be 11.41% by chemical titration.

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Abstract

The invention provides a method used for preparing methylethyl ketone peroxide by taking an acidic ion exchange resin as a catalyst. According to the method, butanone and hydrogen peroxide are taken as raw materials, the acidic ion exchange resin is taken as the catalyst, dibutyl phthalate is taken as a diluent, after constant temperature stirring reaction, an obtained mixture is allowed to stand for separation, and an obtained oil phase is methylethyl ketone peroxide. According to the method, the heterogeneous catalyst is adopted, so that the catalyst and the reaction materials can be separated easily, and the catalyst can be recycled for a plurality of times; reaction is stable, the temperature is increased slowly, and reaction is continuous and stable; product active oxygen content is 13%, and economic value is high; application of strong such as sulfuric acid is avoided, so that corrosion on equipment is less, environment pollution is not caused, and environmental benefit is relatively high.

Description

technical field [0001] The invention relates to a method for preparing methyl ethyl ketone peroxide, in particular to a method for preparing methyl ethyl ketone peroxide by using an acidic ion exchange resin as a catalyst. Background technique [0002] Organic peroxides can be divided into hydrocarbyl peroxides, percarboxylic acids, acyl peroxides, ester peroxides, ketone peroxides, etc. according to the different functional groups of the substituents. Among them, methyl ethyl ketone peroxide (referred to as MEKP) As an important organic peroxide, it is widely used as an initiator for unsaturated olefin polymerization, a catalyst for organic reactions and a curing agent for unsaturated polyester resins. . [0003] In the process of producing methyl ethyl ketone peroxide (referred to as MEKP), it has been prepared from butanone (referred to as MEK) and hydrogen peroxide under the catalysis of sulfuric acid and phosphoric acid at home and abroad, but the disadvantages are: st...

Claims

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Application Information

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IPC IPC(8): C07C409/20C07C407/00
CPCY02P20/582Y02P20/584
Inventor 査飞潘姣蒋旭
Owner 兰州助剂厂有限责任公司
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