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Method for preparing environment-friendly plasticizer by high concentration hydrogen peroxide epoxidized oil

An environmentally friendly plasticizer and hydrogen peroxide technology, applied in the direction of fatty acid production, fatty acid chemical modification, etc., can solve the problems of long reaction time, low epoxy value, low conversion rate, etc., to achieve shortened reaction time, high epoxy value, and low cost low effect

Inactive Publication Date: 2014-09-03
JIANGNAN UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, in the field of epoxidized fatty acid methyl ester industrialization, the oxygen source used is still low-concentration hydrogen peroxide, and its main disadvantages are that the reaction requires a relatively high temperature (generally above 70°C), and the reaction time is long (generally 8-10 h). Low and poor selectivity, the epoxy value of the product is low (only about 3.5%), and the iodine value is high (up to about 8 g / 100g)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Add 30 g of fatty acid methyl ester with an iodine value of 102 g / 100 g and 1.8 g of formic acid with a mass fraction of 88% to a three-necked flask equipped with a thermometer, a stirrer and a dropping funnel, and heat it in a water bath to 40°C. Slowly add 7 g of 70% H 2 o 2 , maintain the reaction temperature at 60°C, and after 4 hours of complete reaction, transfer the reaction mixture to a separatory funnel, keep it warm and let it stand for 40 minutes to separate layers; the upper layer is the oil phase, and the lower layer is the water phase. The pH is near neutral. The oil phase was distilled under reduced pressure at 85°C to obtain the product epoxy fatty acid methyl ester.

[0016] The epoxy value of the product obtained is 4.64%, and the iodine value is 1.4 g / 100g. The conversion rate reached 98.6%, and the selectivity reached 73.2%.

Embodiment 2

[0018] Add 30 g of cottonseed oil with an iodine value of 113 g / 100 g and 2 g of formic acid with a mass fraction of 88% to a three-necked flask equipped with a thermometer, a stirrer and a dropping funnel, and heat it in a water bath to 40°C. Add dropwise 7.9g of 70% H with stirring 2 o 2 , maintain the reaction temperature at 60°C, and after 4 hours of complete reaction, transfer the reaction mixture to a separatory funnel, keep it warm and let it stand for stratification; the upper layer is the oil phase, and the lower layer is the water phase. After separating the oil phase, wash the oil phase with water until the pH The value is near neutral. The oil phase was distilled under reduced pressure at 85° C. to obtain the product epoxy cottonseed oil.

[0019] The epoxy value of the product obtained is 5.84%, and the iodine value is 2.8 g / 100g. The conversion rate reaches 97.5%, and the selectivity reaches 84.1%

Embodiment 3

[0021] Add 30 g of fatty acid methyl esters with an iodine value of 102 g / 100 g and 2 g of formic acid with a mass fraction of 88% to a three-necked flask equipped with a thermometer, a stirrer and a dropping funnel, and heat it in a water bath to 40°C. Under vigorous stirring, 8 g of 60% H 2 o 2 , maintain the reaction temperature at 60°C, and after 4 hours of complete reaction, transfer the reaction mixture to a separatory funnel, keep it warm and let it stand for stratification; the upper layer is the oil phase, and the lower layer is the water phase. After the oil phase is separated, wash the oil phase with water until The pH is near neutral. The oil phase was distilled under reduced pressure at 85°C to obtain the product epoxy fatty acid methyl ester.

[0022] The epoxy value of the product obtained is 4.75%, and the iodine value is 2.2 g / 100g. The conversion rate reached 97.8%, and the selectivity reached 75.6%.

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Abstract

The invention relates to a method for preparing an environment-friendly plasticizer by high concentration hydrogen peroxide epoxidized oil, and belongs to the chemical technical field. The epoxidized environment-friendly plasticizer is generated by reaction under a heating condition by using fatty acid methyl ester, cottonseed oil or soybean oil as a raw material, high concentration hydrogen peroxide (60-70%) as an oxygen source and formic acid as a catalyst. The epoxide number of final product can reach over 4.5%, and the iodine value is below 2.8g / 100g. With the adoption of high concentration hydrogen peroxide, the reaction time can be shortened by over 50% compared with that of low concentration hydrogen peroxide (35-50%). The method is simple in process, the effective yield of the reaction kettle in unit volume can be improved by over 15%, and the energy consumption is reduced, so that the method is more low-carbon and environment-friendly. Fatty acid methyl ester is originated from products of leftovers of vegetable oil and fat, drainage oil and waste cooking oil after methyl esterification or is replaced by cottonseed oil or soybean oil to obtain epoxy cottonseed oil or epoxy soybean oil. The method provided by the invention can be widely applied to epoxidizing process of vegetable oil and fat and has good application prospect.

Description

technical field [0001] The invention discloses a method for preparing an environment-friendly plasticizer by epoxidizing grease with high-concentration hydrogen peroxide, belongs to the technical field of chemical industry, and is suitable for the deep processing and development of various unsaturated fatty acid esters. Background technique [0002] At present, in the plastic processing industry, phthalate plasticizers are still the most widely used type of plasticizers. However, due to the potential harm of such plasticizers to human health, countries have successively introduced laws to restrict the use of such products. Epoxy vegetable oil plasticizer (such as epoxy soybean oil, epoxy fatty acid methyl ester) is a new type of environmentally friendly plasticizer, its toxicity is extremely small, and it is allowed to be used as an additive for food and pharmaceutical packaging materials in many countries. plasticizer. This kind of plasticizer can not only replace the mai...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C11C3/00
Inventor 蒋平平郑佳伟王富才彭敏佳吴江浩
Owner JIANGNAN UNIV
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