A kind of production method of epoxidized soybean oil

A technology of epoxidized soybean oil and production method, which is applied in the direction of organic chemistry, can solve the problems of difficult control of reaction temperature, high cost of sewage treatment, slow epoxidation speed, etc., to reduce sewage production, save sewage treatment burden, and react The effect of less by-products

Active Publication Date: 2019-08-30
广东宏力达合成材料科技有限公司
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Problems solved by technology

[0004] CN86104989A discloses a kind of production method of epoxy soybean oil, this method reacts 7~8 hours with soybean oil, 39% hydrogen peroxide, concentrated sulfuric acid, glacial acetic acid, one-step synthesis product epoxy soybean oil, epoxy value is at 6.0-6.4, The epoxy group generated by this method is easy to open the ring, especially in the later stage of epoxidation, because the concentration of oxidant hydrogen peroxide decreases, the epoxidation speed is slow, the production cycle is long, and the reaction temperature is not easy to control
Among them, the specific steps of series connection epoxidation treatment are as follows: (1) Add soybean oil, hydrogen peroxide, formic acid and concentrated sulfuric acid into the first reaction kettle connected in series according to the ratio and keep stirring, and react under the condition of 60-80°C. After 2.5-4.0 hours, remove the water layer to obtain epoxidized soybean oil A; (2) mix epoxidized soybean oil A, hydrogen peroxide, formic acid and concentrated sulfuric acid in a mass ratio of 1: 0.84-0.90: 0.03-0.10: 0.004 -0.006 is added to the second reaction kettle and continuously stirred, wherein the concentration of hydrogen peroxide is 23-26%, under the condition of 70-80°C, react for 2-3.5 hours, and divide and remove the water layer to obtain epoxidized soybean oil B; (3 ) adding epoxidized soybean oil B, hydrogen peroxide, formic acid and concentrated sulfuric acid to the third reaction kettle in a mass ratio of 1:0.5-0.9:0.04-0.10:0.003-0.006, wherein the concentration of hydrogen peroxide is 50% , under the condition of 65-75 ℃, react for 2-3.5 hours, divide and remove the water layer to obtain the crude product of epoxidized soybean oil; the water consumption of this invention is large, the subsequent sewage treatment cost is high, and the epoxidation temperature is relatively high, and the epoxidation The speed is fast, which is conducive to the epoxidation reaction to the target product, but at the same time, the high temperature will accelerate the occurrence of side reactions such as hydrolysis, which will affect the quality of the product
[0006] At present, the non-solvent synthesis of epoxidized soybean oil still has low epoxy value of the product (the bottleneck of epoxy value in the domestic industry is 6.5g / 100gESO), many by-products, relatively complicated post-treatment, high reaction temperature, and long reaction time and the high cost of the catalyst

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  • A kind of production method of epoxidized soybean oil
  • A kind of production method of epoxidized soybean oil

Examples

Experimental program
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Effect test

Embodiment 1

[0033] (1) Take 100g of hydrogen peroxide, 3g of formic acid, 0.1g of phosphotungstic heteropolyacid and 0.2g of manganese benzoate with a concentration of 55%, add them to the autoclave successively, stir for 2h at a speed of 200rpm, cool to 50°C, and obtain peroxyformic acid mixture;

[0034] (2) in the formic acid peroxide mixture that step (1) obtains, slowly drip 120g soybean oil, control the flow rate of soybean oil, make it drop completely in 0.8h; During the dropping process, feed 10L oxygen, control The stirring speed is 200rpm, the temperature is 60°C, the pressure is 0.9Mpa, the reaction is 2h, and the crude epoxy soybean oil is obtained;

[0035] (3) The crude epoxidized soybean oil obtained in step (2) is subjected to alkali washing, water washing, and vacuum distillation according to conventional technical means to obtain the finished epoxidized soybean oil.

Embodiment 2

[0037] (1) Take 65% hydrogen peroxide 100g, 10g formic acid, 0.3g phosphotungstic heteropoly acid and 0.6g manganese benzoate, add them to the autoclave successively, stir for 1h at a speed of 450rpm, cool to 60°C, and get peroxyformic acid mixture;

[0038] (2) In the peroxyformic acid mixture obtained in step (1), slowly add 180g of soybean oil dropwise, control the flow rate of soybean oil, and make it drop completely within 1h; during the dropwise addition, feed 50L of oxygen and control the stirring The speed is 450rpm, the temperature is 60°C, the pressure is 1.2Mpa, the reaction is 1h, and the crude product of epoxidized soybean oil is obtained;

[0039] (3) The crude epoxidized soybean oil obtained in step (2) is subjected to alkali washing, water washing, and vacuum distillation according to conventional technical means to obtain the finished epoxidized soybean oil.

Embodiment 3

[0041](1) Take 100g of hydrogen peroxide, 8g of formic acid, 0.05g of phosphotungstic heteropolyacid and 0.25g of manganese benzoate at a concentration of 60%, add them to the autoclave successively, stir for 1h at a speed of 300rpm, and cool to 55°C to obtain peroxyformic acid mixture;

[0042] (2) in the formic acid peroxide mixture that step (1) obtains, slowly drip 160g soybean oil, control the flow rate of soybean oil, make it drop completely in 0.5h; During the dropping process, feed 15L oxygen, control The stirring speed is 450rpm, the temperature is 60°C, the pressure is 1.0Mpa, the reaction is 1.5h, and the crude epoxy soybean oil is obtained;

[0043] (3) The crude epoxidized soybean oil obtained in step (2) is subjected to alkali washing, water washing, and vacuum distillation according to conventional technical means to obtain the finished epoxidized soybean oil.

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Abstract

The invention discloses a production method of epoxidized soybean oil. The invention adopts a two-step synthesis method, and the method includes the steps of: (1) adding hydrogen peroxide, formic acidand a catalyst into a high-pressure reaction kettle, conducting stirring and cooling to obtain peroxyformic acid; (2) adding soybean oil dropwise into the peroxyformic acid obtained by step (1), introducing oxygen, performing stirring and carrying out pressurizing reaction to obtain a crude epoxidized soybean oil product; and (3) conducting alkali washing, water scrubbing and reduced pressure distillation on the crude epoxidized soybean oil product obtained by step (2) to obtain an epoxidized soybean oil finished product. Compared with the prior art, the method provided by the invention has the advantages of low cost, good reaction temperature controllability, fast reaction speed and few by-product, and the obtained product has good quality.

Description

technical field [0001] The invention belongs to the technical field of inorganic chemical synthesis, and in particular relates to a production method of epoxidized soybean oil. Background technique [0002] Epoxidized soybean oil is a non-toxic non-benzene environment-friendly plastic additive-plasticizer widely used at present. It has dual properties of plasticization and heat stability, and is non-toxic, safe and environmentally friendly, so it is favored by the plastic products industry. Favored, widely used in plastics, coatings, new polymer materials, rubber and other industrial fields. With the improvement of environmental protection awareness in all countries in the world, the toxicity of plasticizers has attracted more and more attention; plasticizer phthalate products are suspected of causing cancer, and many developed countries have banned them from being used in medical treatment, food packaging, and daily necessities. , toys and other plastic products. Moreover...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/42C07D301/16
Inventor 徐文惠
Owner 广东宏力达合成材料科技有限公司
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