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A kind of synthetic method of dimethyl azobisisobutyrate

A technology of dimethyl azobisisobutyrate and a synthesis method, which is applied in the direction of organic chemistry and the like, can solve the problems of unsuitable industrial scale production, difficult to handle discharge, human body and environmental hazards, etc., and achieves thorough product separation and reaction. The effect of short time, environmentally friendly and non-toxic raw materials

Active Publication Date: 2019-06-21
邢保林
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The two methods in the traditional process have long synthetic routes, and the solvents used are toxic benzene or halogenated aromatic hydrocarbons, which are very harmful to human body and environment
And it needs to feed chlorine gas or hydrogen chloride gas, the reaction is violent and difficult to control, and safety accidents such as kettle leakage often occur. After the hydrolyzed crude product is frozen, a small amount of it dissolves in water and is difficult to recover, and the yield is low; the waste water produced is strongly acidic, and it is difficult to treat it up to the standard Emissions, environmental protection pressure is very high, not suitable for industrial scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, and the reaction temperature is 25°C. After the dropwise addition, keep warm for reaction 8 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of phosphorus trichloride solution was 95%; the molar ratio of raw materials was azobisisobutyronitrile:methanol:isophor Alone: ​​phosphorus trichloride=1:2:3.2:2;

[0031] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 30°C, and wait for the azo After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 6 for hydrolysis; the weight ratio of azoiminomethyl ether hydrochloride solid mat...

Embodiment 2

[0037] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, the reaction temperature is 10°C, and keep warm after the dropwise addition 15 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of the phosphorus trichloride solution was 97%; the molar ratio of the raw materials was azobisisobutyronitrile:methanol: Isophorone: phosphorus trichloride=1:2:5.8:2.8;

[0038] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 20°C, and wait for the azoimine methyl ether hydrochloride solid material to After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 4 for hydrolysis; the weight ratio of a...

Embodiment 3

[0044] (1) Condensation: Add the measured azobisisobutyronitrile, methanol, and isophorone into the reaction vessel, start stirring, add phosphorus trichloride solution dropwise, the reaction temperature is 30°C, and keep warm after the dropwise addition 10 hours; the feed liquid was centrifuged to obtain azoimine methyl ether hydrochloride solid material; the mass concentration of the phosphorus trichloride solution was 95%; the molar ratio of the raw materials was azobisisobutyronitrile:methanol: Isophorone: phosphorus trichloride=1:3.5:5.8:2.8;

[0045] (2) Hydrolysis: Add the measured pure water into the hydrolysis container, add the solid material of azoimine methyl ether hydrochloride obtained in step (1) into the hydrolysis container under stirring, control the temperature at 10°C, and wait for the azoimine methyl ether hydrochloride solid material to After adding iminomethyl ether hydrochloride, adjust the pH value of the system to 7 for hydrolysis; the weight ratio of...

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PUM

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Abstract

The invention discloses a dimethyl 2,2'-azobis(2-methylpropionate) synthesis method. The dimethyl 2,2'-azobis(2-methylpropionate) synthesis method comprises the following steps: (1) condensing: adding azodiisobutyronitrile, methyl alcohol and isophorone into a reactor, adding a phosphorus trichloride solution to react, centrifuging to obtain an azoimide methyl ether hydrochloride solid material; (2) hydrolyzing: adding pure water into a hydrolysis container, adding the azoimide methyl ether hydrochloride solid material into the hydrolysis container to hydrolyze; (3) splitting a phase: putting the hydrolyzed material liquid into a phase split container, splitting the phase by using a phase transfer agent hexadecyl trimethyl ammonium chloride; (4) recrystallizing; (5) drying. The process route and the raw materials are optimally designed, the raw materials are environmentally friendly and toxic-free, the reaction is stable and easy to control, and the reaction safety is greatly improved; the product separation is more thorough, and the product yield is greatly improved; the wastewater discharge is reduced, and the environmental protection pressure is effectively relieved; the reaction time is short, the energy consumption is low, and the production cost is greatly lowered.

Description

technical field [0001] The invention relates to a method for synthesizing dimethyl azobisisobutyrate, which belongs to the technical field of chemical synthesis. Background technique [0002] The full name of POP is grafted polyether polyol, referred to as grafted polyether. It is a polymer obtained by grafting and copolymerizing compounds containing vinyl monomers in polyether. The polyurethane foam produced by it has a high load-bearing capacity. and good rebound performance. The output of graft polyether in developed countries accounts for more than 1 / 5 of the general polyether. In recent years, my country's demand for POP has been increasing. However, in the production process of POP, the properties of the initiator and its decomposition products will directly affect the production process and product characteristics of the polymer. After the commonly used polymerization initiator azobisisobutyronitrile (AIBN) is decomposed, its product is highly toxic solid tetrameth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C245/04
CPCC07C245/04
Inventor 邢保林
Owner 邢保林
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