Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow

A new technology of tert-butyl decanoate and peroxidation, which is applied in the chemical industry, can solve the problems of insufficient active oxygen, poor quality stability and reproducibility, and uneven temperature distribution of tert-butyl peroxyneodecanoate. Low labor intensity, stable product quality and stable flow rate

Inactive Publication Date: 2015-05-06
LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The industrial production of tert-butyl peroxyneodecanoate (BNP) adopts intermittent 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 large structural size inside the reactor equipment, the concentration of substances in the reaction process, and the temperature distribution are uneven, resulting in insufficient active oxygen in the finished product of tert-butyl peroxyneodecanoate (BNP), which reduces the product quality.

Method used

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  • Method for preparing tert-butyl peroxyneodecanoate (BNP) through continuous flow

Examples

Experimental program
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Effect test

Embodiment 1

[0029] (1) adding solid sodium hydroxide to deionized water to prepare a 32% sodium hydroxide aqueous solution;

[0030] (2) will 1 # The flow rate of the metering pump is set to 430ml / min, 2 # The flow rate of the metering pump is set to 120ml / min, and 1 # Metering pump, 2 # Metering pump, so that sodium hydroxide aqueous solution and tert-butyl hydroperoxide aqueous solution of 70wt% concentration 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 170ml / min, 3 # metering pump in 1 # Metering pump, 2 # Open after metering pump opens 50 seconds, make the neodecanoyl chloride solution of 98wt% purity enter 2 with steady flow rate # The reactor reacts with the products of sodium hydroxide aqueous solution and tert-butyl hydroperoxide aqueous solution, adding brine to control the...

Embodiment 2

[0034] (1) adding solid sodium hydroxide to deionized water to prepare a 40% aqueous sodium hydroxide solution;

[0035] (2) will 1 # The flow rate of the metering pump is set to 320ml / min, 2 # The flow rate of the metering pump is set to 80ml / min, and 1 # Metering pump, 2 # Metering pump, so that the sodium hydroxide aqueous solution and the tert-butyl hydroperoxide aqueous solution of 72wt% concentration 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 150ml / min, 3 # metering pump in 1 # Metering pump, 2 # The metering pump is turned on after 70 seconds, so that the neodecanoyl chloride solution of 98wt% purity enters the 2 # The reactor reacts with the products of sodium hydroxide aqueous solution and tert-butyl hydroperoxide aqueous solution, adding brine to control the...

Embodiment 3

[0039] (1) adding solid potassium hydroxide to deionized water to prepare a 40% potassium hydroxide aqueous solution;

[0040] (2) will 1 # The flow rate of the metering pump is set to 340ml / min, 2 # The flow rate of the metering pump is set to 110ml / min, and 1 # Metering pump, 2 # Metering pump, make potassium hydroxide aqueous solution and tert-butyl hydroperoxide aqueous solution of 75wt% concentration enter 1 at a steady flow rate respectively # React in the reactor, add the brine of 10wt% concentration simultaneously to control reaction temperature at 10 ℃, then enter 2 #reactor;

[0041] (3) Setting 3 # The flow rate of the metering pump is 140ml / min, 3 # metering pump in 1 # Metering pump, 2 # After the metering pump is turned on for 40 seconds, the neodecanoyl chloride solution with a purity of 98wt% enters the 2 # The reactor reacts with the products of potassium hydroxide aqueous solution and tert-butyl hydroperoxide aqueous solution, adding brine to control...

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Abstract

The invention provides a method for preparing tert-butyl peroxyneodecanoate (BNP) through a continuous flow, wherein the method includes an alkaline aqueous solution is prepared, the alkaline aqueous solution and a tert-butyl hydrogen peroxide aqueous solution are subjected to a reaction in a reactor, a neodecanoyl chloride solution and the product of the alkaline aqueous solution and the tert-butyl hydrogen peroxide aqueous solution are subjected to a reaction, and the product is subjected to further full reaction through a delay pipeline to obtain the product, wherein the reaction process is carried out in a micro-reactor. With adopting of the prepared solvent-type or emulsion-type tert-butyl peroxyneodecanoate (BNP), the product quality is stable, and the reproducibility is good; because the reaction is carried out in the micro-reactor, the process flow is simplified, the reaction is continuously carried out under mild, safe and environmental-protection conditions, the amount and the yield of the product are greatly improved, and the yield can reach above 98%.

Description

technical field [0001] The present invention relates to a kind of preparation method of initiator tert-butyl peroxyneodecanoate (BNP) used for high polymer synthesis, particularly a kind of method for preparing tert-butyl peroxyneodecanoate (BNP) by continuous flow, belonging to 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 of materials and efficient heat transfer, so m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C409/38C07C407/00
Inventor 沈智陈唐建侯永正翟少华肖毅
Owner LINZIZHENGHUA ACCESSORY INGREDIENT ZIBO
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