Method for preparing peroxidized dicarbonate (2-ethylhexyl) ester (EHP) by continuous flow

A technology of dicarbonic acid peroxide and ethylhexyl, applied in the chemical industry, can solve problems such as poor quality stability and reproducibility, uneven temperature distribution, and high labor intensity of workers, so as to achieve stable product quality, low labor intensity, The effect of stable production process

Inactive Publication Date: 2015-02-25
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The industrial production of bis(2-ethylhexyl) peroxydicarbonate (EHP) adopts batch operation mode, the labor intensity of workers is high, the process conditions are greatly affected by human factors, and the quality stability and reproducibility are poor
At the same time, due to the larger structural size of the reactor equipment, the concentration of substances in the reaction process, and the uneven temperature distribution, resulting in insufficient active oxygen in the finished product of bis(2-ethylhexyl) peroxydicarbonate (EHP), which reduces the product quality. quality

Method used

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  • Method for preparing peroxidized dicarbonate (2-ethylhexyl) ester (EHP) by continuous flow

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] (1) solid sodium hydroxide is added into deionized water to be mixed with a 10% sodium hydroxide aqueous solution;

[0030] (2) will 1 # The flow rate of the metering pump is set to 360ml / min, 2 # The flow rate of the metering pump is set to 40ml / min, and 1 # Metering pump, 2 # Metering pump, so that sodium hydroxide aqueous solution and 27.5wt% hydrogen peroxide enter 1 at a steady flow rate respectively # React in the reactor, add the brine of 5wt% concentration simultaneously to control reaction temperature at 10 ℃, then enter 2 # reactor;

[0031] (3) Setting 3 # The flow rate of the metering pump is 130ml / min, 3 # metering pump in 1 # Metering pump, 2 # The metering pump is turned on after 60 seconds, so that the 2-ethylhexyl chloroformate solution of 98wt% purity enters the 2 # The reactor reacts with the product of sodium hydroxide aqueous solution and hydrogen peroxide, adding brine to control the reaction temperature at 25°C;

[0032] (4) The product ...

Embodiment 2

[0034] (1) solid sodium hydroxide is added into deionized water to be mixed with a 15% sodium hydroxide aqueous solution;

[0035] (2) will 1 # The flow rate of the metering pump is set to 420ml / min, 2 # The flow rate of the metering pump is set to 70ml / min, and 1 # Metering pump, 2 # Metering pump, so that sodium hydroxide aqueous solution and 27.5wt% concentration of hydrogen peroxide enter 1 at a steady flow rate respectively # React in the reactor, add the brine of 7wt% concentration simultaneously to control reaction temperature at 15 ℃, then enter 2 # reactor;

[0036] (3) Setting 3 # The flow rate of the metering pump is 180ml / min, 3 # metering pump in 1 # Metering pump, 2 # After the metering pump is turned on for 80 seconds, the chloroformate-2-ethylhexyl ester solution with a purity of 98wt% enters the 2 # The reactor reacts with the product of sodium hydroxide aqueous solution and hydrogen peroxide, adding brine to control the reaction temperature at 30°C; ...

Embodiment 3

[0039] (1) adding solid potassium hydroxide to deionized water to prepare an aqueous potassium hydroxide solution with a concentration of 12.5%;

[0040] (2) will 1 # The flow rate of the metering pump is set to 460ml / min, 2 # The flow rate of the metering pump is set to 80ml / min, and 1 # Metering pump, 2 # Metering pump, so that potassium hydroxide aqueous solution and 27.5wt% concentration of hydrogen peroxide enter 1 at a steady flow rate respectively #React in the reactor, add the brine of 10wt% concentration simultaneously to control reaction temperature at 12 ℃, then enter 2 # reactor;

[0041] (3) Setting 3 # The flow rate of the metering pump is 170ml / min, 3 # metering pump in 1 # Metering pump, 2 # The metering pump is turned on after 50 seconds, so that the 2-ethylhexyl chloroformate solution of 98wt% purity enters the 2 # The reactor reacts with the product of potassium hydroxide aqueous solution and hydrogen peroxide, adding brine to control the reaction t...

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Abstract

The invention provides a method for preparing peroxidized dicarbonate (2-ethylhexyl) ester (EHP) by a continuous flow. The method comprises the following steps: preparing an alkaline aqueous liquid; carrying out reaction on the alkaline aqueous liquid and hydrogen peroxide in a reactor; adding a chloroformic acid-2-ethyl caproate liquid to react with a product of the alkaline aqueous liquid and hydrogen peroxide; and further carrying out full reaction on the product to obtain a product by virtue of a delayed pipeline, wherein the reaction process is carried out in a micro-reactor. The solvent or emulsion type peroxidized dicarbonate (2-ethylhexyl) ester (EHP) prepared by the method provided by the invention is stable in product quality and good in repeatability. As reaction is carried out in the micro-reactor, the process flow is simplified, so that the reaction is continuously carried out under mild, safe and environment-friendly conditions. Therefore, the product content and yield are greatly improved, and the yield can reach over 98%.

Description

technical field [0001] The present invention relates to a kind of preparation method of initiator bis(2-ethylhexyl) peroxydicarbonate (EHP) used for high polymer synthesis, in particular to a kind of continuous flow preparation of bis(2-ethylhexyl) peroxydicarbonate The method of hexyl) ester (EHP), belongs to the field of chemical industry. Background technique [0002] Microreactors, that is, microchannel reactors, are microreactors with characteristic sizes between 10 and 300 microns manufactured by precision processing technology. The microreactor can make the channel of the reaction fluid at the micron level, and can contain millions of microchannels. At the same time, due to its internal microstructure, the microreactor device has a large specific surface area, which can reach the ratio of the stirred tank. Hundreds or even thousands of times the surface area. Microreactors have excellent heat and mass transfer capabilities, which can achieve instant uniform mixing o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/32C07C407/00
Inventor 沈智陈唐建侯永正翟少华肖毅
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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