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Method for preparing di(2-ethylhexyl) peroxydicarbonate

A technology of dicarbonic acid peroxide and ethylhexyl, which is applied to the preparation of peroxy compounds, chemical instruments and methods, and the preparation of organic compounds, etc., can solve the problems of shortened operation difficulty, obvious amplification effect, and low decomposition temperature, and achieve reduction Effects of response time, high operational safety, and short response times

Active Publication Date: 2019-01-25
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] But the synthesis of di(2-ethylhexyl) peroxydicarbonate mostly adopts ethylhexanol and phosgene to react (2-ethyl)hexyl chloroformate at present, and then makes by peroxidation reaction, and phosgene is high Toxic substances, potential safety hazards
In addition, due to the high activity of bis(2-ethylhexyl) peroxydicarbonate, low decomposition temperature, easy decomposition and even explosion, the existing kettle technology has the disadvantages of high raw material consumption, unstable reaction and low yield, and traditional The reaction cycle in the reactor is long, the amplification effect is obvious, and safety accidents are prone to occur
The traditional pipeline microreactor increases the energy consumption due to the excessive length of the pipeline, and the excessive pressure drop of the pipeline increases the difficulty of operation. At the same time, the service life of the pump is shortened if the pressure drop is too large. At the same time, there are serious safety hazards if the pressure drop is too large.

Method used

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  • Method for preparing di(2-ethylhexyl) peroxydicarbonate
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  • Method for preparing di(2-ethylhexyl) peroxydicarbonate

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Effect test

Embodiment 1

[0033] Prepare 20wt% hydrogen peroxide aqueous solution and 15wt% sodium hydroxide aqueous solution respectively, pump the 20wt% hydrogen peroxide aqueous solution and 15wt% sodium hydroxide aqueous solution into the first micro-mixer of the micro-reaction device, mix thoroughly and enter The reaction was carried out in the first microreactor, the volume of the first microreactor was 3mL, the reaction temperature T1: 20°C, the residence time t1: 1min, and the reaction liquid A was obtained. Reaction solution A and 98wt% chloroester aqueous solution are pumped into the second micro-mixer of micro-reaction device respectively, after fully mixing, enter in the second micro-reactor and react, the volume of the second micro-reactor is 24mL, reaction temperature T2 : 25° C.; residence time t2: 6 min, to obtain reaction solution B. The molar ratio of the reaction is: chloroester: hydrogen peroxide: sodium hydroxide=1: 0.6: 1.2. The inner diameters of the reaction tubes of the first ...

Embodiment 2

[0035] Identical with embodiment 1, difference only is: the volume of the first microreactor is 1.5mL, and the volume of the second microreactor is 24mL, and the reaction residence time t1:0.5min in the first microreactor obtains diperoxide Bis(2-ethylhexyl)carbonate, the reaction yield is 93.2%.

Embodiment 3

[0037] Identical with embodiment 1, difference only is: the volume of the first microreactor is 6mL, and the volume of the second microreactor is 24mL, and the reaction residence time t1:2min in the first microreactor obtains dicarbonate peroxide (2-Ethylhexyl) ester, the reaction yield is 97.0%.

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Abstract

The invention discloses a method for preparing di(2-ethylhexyl) peroxydicarbonate. The method includes the following steps: (1) pumping a hydrogen peroxide aqueous solution and a sodium hydroxide aqueous solution into a first microreactor of a micro-reaction device for reaction to obtain a reaction solution A; (2) pumping the reaction solution A obtained in the step (1) and 2-ethylhexyl chloroformate separately into a second microreactor of the micro-reaction device for reaction to obtain a reaction solution B; (3) making the reaction solution B obtained in the step (2) react in a self-made reactor continuously and introducing the reaction solution into a separation tank for static stratification to obtain an upper oil phase to obtain the di(2-ethylhexyl) peroxydicarbonate. The method hasthe advantages of simple process, continuous production, fast reaction, high yield, low cost, good operability, high operation safety, high selectivity and direct amplification for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for continuously preparing di(2-ethylhexyl) peroxydicarbonate by using a microchannel reaction device combined with a self-made reactor. Background technique [0002] Bis(2-ethylhexyl) peroxydicarbonate (EHP) is a colorless transparent liquid, which is a highly active initiator. Compared with other peroxydicarbonate initiators, its transportation and storage stability Preferably, because it is insoluble in water, it is not easy to produce a water phase polymer when the polymerization reaction is initiated, the tendency of sticking to the kettle is small, and the heat release of the polymerization reaction is uniform, and it is easy to obtain a uniform reaction. Therefore bis(2-ethylhexyl) peroxydicarbonate has become one of the most promising initiators. [0003] But the synthesis of di(2-ethylhexyl) peroxydicarbonate mostly adopts ethylhexanol an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C407/00C07C409/32
CPCC07C407/00C07C409/32
Inventor 郭凯方正赵学祥黄达何伟欧阳平凯
Owner NANJING UNIV OF TECH
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