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A kind of preparation method of epoxy plasticizer

A plasticizer and epoxy technology, applied in the field of preparation of epoxidized soybean oil, can solve problems such as explosion danger, and achieve the effects of short reaction time, low energy consumption and good product quality

Active Publication Date: 2017-08-25
中山联成化学工业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] If a mixture of high-concentration hydrogen peroxide and high-concentration formic acid is used to react with soybean oil as a one-time addition of reagents, the heat of reaction will cause the reaction in the kettle to release heat too quickly. If the equipment cannot transfer heat in a timely manner, there is a chance of explosion hazard.
[0006] In addition, in the traditional production process of preparing epoxidized soybean oil, a large amount of wastewater treatment is required. Alkaline neutralization and removal of formic acid-containing wastewater will generate a large amount of waste solids and other sewage treatment burdens.

Method used

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  • A kind of preparation method of epoxy plasticizer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Take 120g of formic acid with a mass concentration of 90% and 500g of hydrogen peroxide with a mass concentration of 50%, mix evenly, and put it into the reactor together with 880g of soybean oil with an iodine value of 130gI / 100g, stir rapidly, and the reaction temperature gradually increases, and the temperature rises to 60 ℃, open the external cooling circulation pipe, and the internal heating pipe, the reaction solution is introduced into the cooling circulation pipe for reaction, the reaction temperature is controlled at 70 ~ 85 ℃, the reaction is 4 hours, and the sampling test epoxy value is 7.0% (g O / 100g oil ) to finish the reaction, centrifuge the water phase, and dehydrate to obtain epoxy soybean oil.

Embodiment 2

[0029] Take 140g of formic acid with a mass concentration of 90% and 365g of hydrogen peroxide with a mass concentration of 70%, mix evenly, and put it into the reactor together with 880g of soybean oil with an iodine value of 130gI / 100g, stir rapidly, and the reaction temperature gradually increases, and the temperature rises to 70 ℃, open the external cooling circulation pipe, and the internal heating pipe, introduce the reaction liquid into the cooling circulation pipe for reaction, control the reaction temperature 70 ~ 85 ℃, react for 4 hours, take a sample to test the epoxy value, greater than 7.0%, end the reaction, carry out The water phase is separated by centrifugation and dehydrated to obtain epoxidized soybean oil.

Embodiment 3

[0031] Take 50 g of formic acid with a mass concentration of 96% and 400 g of hydrogen peroxide with a mass concentration of 70%, mix evenly, and put it into the reactor together with 880 g of soybean oil with an iodine value of 130 gI / 100 g, stir rapidly, and the reaction temperature gradually increases, and the temperature rises to 60 ℃, open the external cooling circulation pipe, and the internal heating pipe, introduce the reaction liquid into the cooling circulation pipe for reaction, control the reaction temperature 70 ~ 85 ℃, react for 4 hours, take a sample to test the epoxy value, greater than 7.0%, end the reaction, carry out The water phase is separated by centrifugation and dehydrated to obtain epoxidized soybean oil.

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Abstract

The invention discloses a method for preparing an epoxy plasticizer. The method comprises the following steps: mixing high-concentration hydrogen peroxide and high-concentration formic acid at normal temperature, thereby obtaining a high-concentration peroxide formic acid mixture; adding the mixture and soybean oil into reaction equipment once, carrying out self-initiation reaction to release heat to the temperature of 60-70 DEG C, controlling the reaction temperature to 70-90 DEG C, reacting for 3-4 hours until the epoxide number is more than 7.0 percent, stopping the reaction, centrifugally separating the aqueous phase, performing dewatering and filtration on the crude oil phase, thereby obtaining the product. The method disclosed by the invention is short in reaction time, high in product selectivity, high in conversion rate and few in ring-opening reaction byproducts, the epoxide number of the product is more than 7.0 percent, the iodine value is less than 2gI / 100g, and the epoxide number retention rate is more than 99 percent; and moreover, the operations of alkali wash / washing / standing are not needed in the product preparation process, wastewater containing formic acid is distilled and recycled by a distillation tower, wastewater treatment is not needed, the wastewater is avoided, the waste solid treatment problem is solved, and the method is low in energy consumption, small in wastewater amount, short in manufacture procedure and high in product quality.

Description

[0001] 【Technical field】 [0002] The invention relates to a preparation method of epoxy plasticizer, in particular to a preparation method of epoxy soybean oil. [0003] 【Background technique】 [0004] At present, the traditional production process for preparing epoxidized soybean oil has insufficient heat removal capacity during the reaction process due to the proportion of reaction reagents and equipment defects. Therefore, the only way to slowly add hydrogen peroxide and use low-concentration reagents is to control the reaction speed and reduce the reaction rate. chance of overheating. This method is likely to cause prolonged reaction time, increased by-products, and reduced product quality. As described in the Chinese patent CN103305347A, the preparation step is to slowly add hydrogen peroxide with a mass concentration of 60% to 70% under vigorous stirring, and finally obtain a methyl epoxy product with an epoxy value of more than 4.5% and an iodine value of 2.8gI / 100g or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/42C11C3/00
CPCC11C3/00
Inventor 郑晓娜蔡满富吴遵承
Owner 中山联成化学工业有限公司
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