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Synthetic method for epoxy soybean oil acrylate

A technology of oil acrylate and epoxidized soybean oil, applied in fatty acid esterification and other directions, can solve the problems of preparing high molecular weight polymers, weak double bond activity, etc., to improve product performance, achieve green, The effect of implementing conditions is simple

Inactive Publication Date: 2014-04-09
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the double bonds naturally present in vegetable oils are weak, and it is difficult to prepare high molecular weight polymers through free radical reactions. In the past, functionalized soybean oil was mainly used.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] a. Put the mixture of refined 50g soybean oil, 12.5g formic acid and 25g petroleum ether in a three-necked reaction flask equipped with electric stirring, dropping funnel and condenser tube, and place it in a constant temperature water bath, mix it evenly and then stir it up To a temperature of 45°C, dropwise add a mixture of hydrogen peroxide and phosphoric acid with a mass ratio of 1.3:0.005;

[0032] b. After the mixture of hydrogen peroxide and phosphoric acid is added dropwise and the temperature is stable, adjust the temperature of the system to a reaction temperature of 55°C, and the reaction time is 3 hours;

[0033] c, after the reaction finishes, transfer the reaction mixture to a separatory funnel and let it stand for stratification, separate the water layer, wash the oil layer with water to neutrality, and distill under reduced pressure to obtain epoxy soybean oil, wherein the epoxy value is 5.3, iodine Value 1.3, acid value 0.3, yield 91%;

[0034] d. Afte...

Embodiment 2

[0038] a, the mixture of 50g soybean oil, 12.5g formic acid and 25g sherwood oil is placed in the three-necked reaction flask that has electric stirring, dropping funnel, condensation pipe, and it is placed in constant temperature water bath, after mixing evenly, stir and rise to At a temperature of 20°C, dropwise add a mixture of 22% hydrogen peroxide and phosphoric acid with a mass ratio of 1.3:0.005;

[0039] b. After the mixture of hydrogen peroxide and phosphoric acid is added dropwise and the temperature is stable, adjust the temperature of the system to a reaction temperature of 30°C, and the reaction time is 4 hours;

[0040] c. After the reaction is over, transfer the reaction mixture to a separatory funnel and let it stand for stratification, separate the water layer, wash the oil layer with water until neutral, and distill under reduced pressure to obtain epoxy soybean oil, wherein the epoxy value is 5.6, and the acid Value 0.5, the yield is 93.3%;

[0041] d, afte...

Embodiment 3

[0045] a. The mixture of 50g soybean oil, 12.5g formic acid and 25g petroleum ether is placed in a three-necked reaction flask with electric stirring, dropping funnel and condenser tube and placed in a constant temperature water bath. After mixing evenly, stir and rise to the temperature At 45°C, add dropwise a mixture of 30% hydrogen peroxide and phosphoric acid with a mass ratio of 1.3:0.005;

[0046] b. After the mixture of hydrogen peroxide and phosphoric acid is added dropwise and the temperature is stable, adjust the temperature of the system to a reaction temperature of 65°C, and the reaction time is 7 hours;

[0047] c. After the reaction is over, transfer the reaction mixture to a separatory funnel and let it stand for stratification. Separate the water layer, wash the oil layer with water until neutral, and distill under reduced pressure to obtain epoxy soybean oil, wherein the epoxy value is 5.69, the acid value 0.7, the yield is 92%;

[0048] d. After the reaction, ...

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Abstract

The invention relates to a synthetic method for epoxy soybean oil acrylate. The synthetic method comprises the following steps of: uniformly mixing the soybean soil, formic acid and solvent at the room temperature, dropping the mixture of hydrogen peroxide and catalyst, stewing and layering the mixture, separating the water layer, using water to wash the oil layer to neutral and decompressing and distilling to obtain the epoxy soybean oil, wherein the epoxy value is higher than 5-8, the acid value is lower than 1, and the yield is 90-95%; adding calcium carbonate or calcium oxide to the remaining formic acid aqueous solution after reaction to obtain and recycle calcium formate; and carrying out an esterification reaction on the epoxy soybean oil to obtain the epoxy soybean oil acrylate, wherein the acid value of the epoxy soybean oil acrylate is lower than 0.5-2, the iodine value of the epoxy soybean oil acrylate is 30-45, and the viscosity of the epoxy soybean oil acrylate is 10000-20000 at 25 DEG C. The synthetic method provided by the invention is clean, safe to carry out, simple to operate, can realize effective utilization of low-concentration hydrogen peroxide, and is convenient to carry out large-scale production.

Description

technical field [0001] The invention relates to a synthesis method of epoxy soybean oil acrylate. Background technique [0002] Soybean oil is mainly a mixture of various saturated and unsaturated fatty acid triglycerides, each molecule contains a double bond, and has long been used as a raw material for alkyd resin coatings. However, the natural double bonds in vegetable oils are less active, and it is difficult to prepare high molecular weight polymers through free radical reactions. In the past, functionalized soybean oil was mainly used. Epoxidized soybean oil has the advantages of abundant resources, low price, non-toxicity, environmental friendliness, thermal stability, light stability, and good solvent resistance, and is widely used in PVC plasticizer stabilizers, food packaging materials, and pharmaceutical products etc. [2]. Acrylated epoxy soybean oil has low viscosity, low irritation and excellent pigment wettability, and can be widely used in the manufacture of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C11C3/08
Inventor 吾满江·艾力夏木西卡玛尔·买买提蔡国星张乐涛努尔买买提·阿布都克力木
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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