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Method for synthesis of trimethylolpropane diallyl ether

A technology of methylolpropane diallyl ether and trimethylolpropane, which is applied in the field of synthesis of chemical intermediates, can solve the problems of incomplete utilization of raw materials, low product purity, unfavorable economic benefits, etc., and facilitates industrial production , The process conditions are not high, and the operation is simple and convenient

Inactive Publication Date: 2012-09-12
GUANGDONG UNIV OF PETROCHEMICAL TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional domestic synthesis process has problems such as high pressure requirements, incomplete utilization of raw materials, long production time, low production efficiency and low product purity, which is not conducive to the improvement of economic benefits of enterprises, and cannot meet the domestic demand for high-quality trimethylol Propane Diallyl Ether Demand

Method used

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  • Method for synthesis of trimethylolpropane diallyl ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 80mL 1,4-dioxane, 134g (1 mol) trimethylolpropane, 7.16g PEG-6000 to a 500ml four-neck flask with a thermometer, condenser, constant pressure dropping funnel and stirrer (m PEG-6000 :m 三羟甲基丙烷 =0.05:1), start stirring, and heat up the water bath. After it is completely dissolved, add 160g of NaOH (4mol) crystals, the temperature continues to rise, and maintain the required reaction temperature in a water bath of 80°C. Increase the stirring intensity, then drop in 168.3g (2.2mol) propene chloride, and when propene chloride is added dropwise to nearly half, increase the rate of propene chloride addition. The total time for the dropwise addition was 4 hours. After the dropwise addition, the reaction was continued at 80° C. for 3 hours, the heating was stopped, and the stirring was turned off. The reacted solid-liquid mixture was cooled to room temperature, then filtered with a circulating water vacuum pump, and the filtrate was collected. Rotary evaporation was carri...

Embodiment 2

[0035] Add 80mL 1,4-dioxane, 134g (1 mol) trimethylolpropane, 4.07g PEG-6000 to a 500ml four-necked flask with a thermometer, condenser, constant pressure dropping funnel and stirrer (m PEG-6000 :m 三羟甲基丙烷 =0.03:1), start stirring, heat up the water bath, after it is completely dissolved, add 160g NaOH (4mol) crystals, the temperature continues to rise, and keep the temperature constant under the condition of 80°C water bath. Increase the stirring intensity, then drip 168.3g (2.2mol) propene chloride, and when propene chloride is added dropwise to nearly half, increase the rate of propene chloride addition. The total time for the dropwise addition was 4.5 hours. After the dropwise addition, the reaction was continued at 80° C. for 4 hours, the heating was stopped, and the stirring was turned off. The reacted solid-liquid mixture was cooled to room temperature, then filtered with a circulating water vacuum pump, and the filtrate was collected. Rotary evaporation was carried o...

Embodiment 3

[0037] Add 60mL 1,4-dioxane, 134g (1 mol) trimethylolpropane, 7.16g PEG-6000 to a 500ml four-necked flask with a thermometer, condenser, constant pressure dropping funnel and stirrer (m PEG-6000 :m 三羟甲基丙烷=0.05:1), start stirring, heat up the water bath, after it is completely dissolved, add 160g NaOH (4mol) crystals, the temperature continues to rise, and keep the temperature constant under the condition of 80°C water bath. Increase the stirring intensity, then drip 168.3g (2.2mol) propene chloride, and when propene chloride is added dropwise to nearly half, increase the rate of propene chloride addition. The total time for the dropwise addition was 4.5 hours. After the dropwise addition, the reaction was continued at 80° C. for 4 hours, the heating was stopped, and the stirring was turned off. The reacted solid-liquid mixture was cooled to room temperature, then filtered with a circulating water vacuum pump, and the filtrate was collected. Rotary evaporation was carried ou...

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Abstract

The invention discloses a method for synthesis of trimethylolpropane diallyl ether. The method comprises the following steps that dioxane, trimethylolpropane and PEG-600 are added into a reactor; the mixed raw materials are heated with stirring so that the mixed raw materials are dissolved completely; solid NaOH is added into the solution; the solution is heated to a temperature of 80 DEG C; chloropropene is dropwisely added into the heated solution with stirring; the solution undergoes an etherification reaction and then is subjected to reduced pressure distillation; and dioxane and a trimethylolpropane diallyl ether product are recovered at different temperatures. Trimethylolpropane diallyl ether content of the trimethylolpropane diallyl ether product obtained by the method is more than 92%. The method provided by the invention has a high yield, high purity, a low production cost and simple processes and can satisfy industrial production demands.

Description

technical field [0001] The invention belongs to the field of synthesis of chemical intermediates, in particular to a synthesis method of trimethylolpropane diallyl ether. Background technique [0002] As a class of very important organic intermediates, trimethylolpropane diallyl ethers have been widely used. At present, these compounds are mainly used in various coatings and semi-finished products of organic synthesis, or as raw materials for inorganic pigment dispersants. This type of compound has a double bond and an ether bond in its molecular structure, utilizes its own ether bond to be oxidized to overcome the obstacle of oxygen inhibition in the double bond free radical reaction, and can obviously enhance the speed of the free radical reaction, and this type of compound It has self-drying performance. When it participates in the manufacture of synthetic resins in the form of monomers, it can endow the coatings made of these resins with self-drying and quick-drying pro...

Claims

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Application Information

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IPC IPC(8): C07C43/178C07C41/16
Inventor 刘卫兵范绍波张庆
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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