Synthesis method of bis(2-ethylhexyl)peroxydicarbonate

A technology of peroxydicarbonate and ethylhexyl, which is applied in the preparation of peroxy compounds, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of long reaction time, high risk, poor mixing efficiency, etc. Improve the conversion rate and selectivity, reduce the risk of the reaction, the effect of extremely efficient heat and mass transfer

Active Publication Date: 2019-09-20
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional production process is mostly batch reaction, and hydrogen peroxide, solid alkali, water and chlorinated ester are used as raw materials to produce EHP. The existing problems are as follows: for safety, a large amount of water is added, energy consumption is high, danger is high, and reaction time is long , produces a lot of waste water, and the reaction process is not easy to control
[0004] Chinese patent CN 105198783A discloses a kind of production method of bis(2-ethylhexyl) peroxydicarbonate, the method is 27% hydrogen peroxide, mass fraction is 32% ionic membrane liquid caustic soda and ch

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  • Synthesis method of bis(2-ethylhexyl)peroxydicarbonate

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Embodiment 1

[0033] A kind of synthetic method of peroxydicarbonate two (2-ethylhexyl) ester, comprises the following steps:

[0034] (1) the hydrogen peroxide that concentration is 40% and the sodium hydroxide solution that concentration is 55% mix in the first microchannel continuous flow reactor, and the internal diameter size of the first microchannel continuous flow reactor is 1mm, and length is 2.5m, The temperature is 12°C, and the reaction time in the first microchannel continuous flow reactor is 1min;

[0035] (2) The material obtained in step (1) is mixed and reacted with chloroester in the second microchannel continuous flow reactor, and the time of mixed reaction is 4min; the mol ratio of chloroester to hydrogen peroxide is 1:0.9, hydrogen peroxide and hydrogen Sodium oxide molar ratio is 1:2, and the internal diameter size of the second microchannel continuous flow reactor is 1mm, is formed by the connection of 10 microchannel mixer substrates, and the length of every microcha...

Embodiment 2

[0038] A kind of synthetic method of peroxydicarbonate two (2-ethylhexyl) ester, comprises the following steps:

[0039] (1) the hydrogen peroxide that concentration is 30% and the sodium hydroxide solution that concentration is 55% mix in the first microchannel continuous flow reactor, and the internal diameter size of the first microchannel continuous flow reactor is 2mm, and length is 1m, temperature is 10°C, and the reaction time in the first microchannel continuous flow reactor is 1.5min;

[0040] (2) The material obtained in step (1) is mixed with chloroester in the second microchannel continuous flow reactor, and the time of the mixed reaction is 3min; the mol ratio of chloroester to hydrogen peroxide is 1:0.8, hydrogen peroxide and hydrogen Sodium oxide molar ratio is 1:1.8, and the internal diameter size of the second microchannel continuous flow reactor is 2mm, is formed by the connection of 8 microchannel mixer substrates, and the length of every microchannel mixer ...

Embodiment 3

[0043] A kind of synthetic method of peroxydicarbonate two (2-ethylhexyl) ester, comprises the following steps:

[0044] (1) the hydrogen peroxide that concentration is 50% and the sodium hydroxide solution that concentration is 45% mix in the first microchannel continuous flow reactor, and the internal diameter size of the first microchannel continuous flow reactor is 0.5mm, and length is 2.0m , the temperature is 15°C, and the reaction time in the first microchannel continuous flow reactor is 1min;

[0045] (2) The material chloroester obtained in step (1) is mixed and reacted in the second microchannel continuous flow reactor, and the time of mixed reaction is 5min; the mol ratio of chloroester and hydrogen peroxide is 1:0.6, and hydrogen peroxide and hydrogen The sodium molar ratio is 1:2.2, and the inner diameter of the second microchannel continuous flow reactor is 0.5mm, which is connected by 6 microchannel mixer substrates, and the length of each microchannel mixer sub...

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Abstract

The invention belongs to the technical field of chemical engineering, and specifically relates to a synthesis method of bis(2-ethylhexyl)peroxydicarbonate. According to the method, hydrogen peroxide and sodium hydroxide are mixed in a first micro-channel continuous flow reactor; then the mixture is mixed with chlorinated esters in a second micro-channel continuous flow reactor to carry out reactions; the temperature of the first micro-channel continuous flow reactor is 15 to 30 DEG C; the second micro-channel continuous flow reactor is formed by connecting 3 to 10 micro-channel mixer substrates; and the temperature of the second micro-channel continuous flow reactor is controlled in a range of 30 to 40 DEG C. The heat-mass transfer efficiency of the synthesis method is high; the temperature is controlled in different sections; the product decomposition caused by uncontrolled temperature, increased side reactions, and the like is prevented; and at the same time, the energy consumption and danger coefficient are reduced. The reaction conversion rate of the synthesis method is 99.2% or more, and the selectivity is 98.5% or more.

Description

technical field [0001] The invention belongs to the technical field of chemistry and chemical engineering, and in particular relates to a synthesis method of bis(2-ethylhexyl) peroxydicarbonate. Background technique [0002] Di(2-ethylhexyl) peroxydicarbonate, also known as initiator EHP, dioctyl peroxydicarbonate, referred to as EHP, is easily decomposed into free radicals under heat or light conditions, so it can be widely used as a free radical type The initiator of the reaction, such as polyethylene, PVC, polyvinyl acetate, etc. in the production. EHP was used as an initiator for the polymerization of vinyl chloride. Its advantages are high initiation rate, short polymerization time, low polymerization temperature, less usage, good product quality and low residual toxicity. [0003] The traditional production process is mostly batch reaction, and hydrogen peroxide, solid alkali, water and chlorinated ester are used as raw materials to produce EHP. The existing problems...

Claims

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Application Information

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IPC IPC(8): C07C407/00C07C409/32B01J19/00B01J4/00
CPCB01J4/001B01J19/0093C07C407/00C07C409/32
Inventor 陈唐建翟志强崔黎明
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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