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Method for preparing epoxy fatty acid ethylester plasticizer

A technology of epoxy fatty acid ethyl ester and plasticizer, applied in organic chemistry and other directions, can solve the problems of ring-opening reaction of epoxy compounds, increase the cost of sewage treatment, slow acceleration of hydrogen peroxide droplets, etc., to improve the epoxy value and improve the stability. The effect of stability and conversion rate, short reaction time

Inactive Publication Date: 2011-02-09
江苏悦达卡特新能源有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in this epoxy reaction, formic acid plays the role of transferring active oxygen and is recycled. Due to the existence of formic acid, the subsequent treatment process will be increased, especially the cost of sewage treatment.
In addition, due to the violent reaction between formic acid and hydrogen peroxide, hydrogen peroxide is decomposed by a large amount of heat, and the high temperature in the reaction process causes the breakage of unsaturated bonds, which is easy to cause ring-opening reactions in epoxy compounds. The drop causes the drop of epoxy value and the darkening of the color of the plasticizer, which leads to the drop of the epoxy value of the plasticizer and affects the quality of the plasticizer. Therefore, in order to prevent the reaction temperature from being too high, dripping The method of hydrogen peroxide, but the drop rate of hydrogen peroxide is relatively slow, and the reaction time is longer, which causes a large amount of energy consumption, increases the production cost, and the quality of the produced product is unstable

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0010] The present invention prepares the method for epoxy fatty acid ethyl ester plasticizer, and each following component is all by weight percentage, and 70% soybean oil acidified grease and 29% dehydrated alcohol and 1% sulfuric acid catalyst are added in the reactor, react The temperature is controlled at 100°C, the pressure is controlled at 0.4Mpa, and the esterification reaction is carried out with continuous stirring for 1 hour. After the esterification reaction is completed, excess ethanol is recovered, and when the mixed liquid material is cooled to 5°C, it is washed with water at room temperature. The mixed liquid material after washing is left standstill or centrifuged for stratification, emits the glycerin of the lower floor, adds alkali to the mixed liquid material of the upper layer and then neutralizes it, such as adding the sodium hydroxide aqueous solution of concentration 30% (weight), the upper layer The pH value of the mixed liquid material is controlled at...

Embodiment 2

[0012] The present invention prepares the method for epoxy fatty acid ethyl ester plasticizer, and each following component is all by weight percentage, and 86% soybean oil acidified grease and 13% dehydrated alcohol and 1% sulfuric acid catalyst are added in the reactor, react The temperature is controlled at 115°C, the pressure is controlled at 0.6Mpa, and the esterification reaction is carried out by continuous stirring for 0.5h. After the esterification reaction is completed, excess ethanol is recovered, and when the mixed liquid material is cooled to 30°C, it is washed with water at room temperature. The mixed liquid material after washing is left standstill or centrifuged for stratification, emits the glycerin of the lower floor, adds alkali to the mixed liquid material of the upper layer and then neutralizes it, such as adding the sodium hydroxide aqueous solution of concentration 30% (weight), the upper layer The pH value of the mixed liquid material is controlled at 8,...

Embodiment 3

[0014] The present invention prepares the method for epoxy fatty acid ethyl ester plasticizer, and each following component is all by weight percentage, and 74.5% soybean oil acidification grease and 24% dehydrated alcohol and 1.5% sulfuric acid catalyst are added in the reactor, react The temperature is controlled at 108°C, the pressure is controlled at 0.5Mpa, and the esterification reaction is carried out with continuous stirring for 1.5 minutes. After the esterification reaction is completed, excess ethanol is recovered, and when the mixed liquid material is cooled to 15°C, it is washed with water at room temperature. The mixed liquid material after washing is left standstill or centrifuged for stratification, emits the glycerin of the lower floor, adds alkali to the mixed liquid material of the upper layer and then neutralizes it, such as adding the sodium hydroxide aqueous solution of concentration 30% (weight), the upper layer The pH value of the mixed liquid material is...

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PUM

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Abstract

The invention relates to a method for preparing an epoxy fatty acid acetidin plasticizer. The method comprises the following steps: according to weight percent, adding 70-86% of soybean oil acid fat, 13-29% of absolute alcohole and 0.5-1.5% of sulphuric acid catalyst into a reaction kettle; stirring for 0.5-1.5h for esterification reaction at 100-115 DEG C and under 0.4-0.6 MPa, cleaning with water, separating, neutralizing, depressurizing and distilling to obtain fatty acid acetidin; adding 96.8-98.6% of fatty acid acetidin, 0.87-2.4% formaldehyde, 0.3-0.6% of stabilizer and 0.15-0.25% of catalyst in the reaction kettle, continuously introducing ozone with a concentration more than or equal to 30mg / L, and stirring for 0.5-2h for epoxy reaction at 70-80 DEG C and under 0.1-0.3MPa,, cleaning with water and dehydrating to obtain the product. The invention has a short reaction time and improves the stability and the conversion rate of the epoxy reaction.

Description

technical field [0001] The invention relates to a method for preparing an epoxy fatty acid ethyl ester plasticizer, belonging to the technical field of epoxy vegetable oil-based plasticizers. Background technique [0002] Epoxy fatty acid ethyl ester uses various animal and vegetable oils as raw materials, and undergoes esterification reaction with low-carbon alcohols such as ethanol, so that it can finally become a plasticizer that can be used in the plastics industry. Epoxy fatty acid ethyl ester plasticizer not only reduces the melt viscosity and melting temperature of the polymer, increases the plasticity and fluidity of the polymer, and makes plastic products flexible, but also has excellent environmental performance and can replace phthalic acid Esters such as DBP, DOP plasticizers. However, the traditional preparation of epoxy fatty acid ethyl ester plasticizers is made by using vegetable oil raw materials, formic acid, hydrogen peroxide and catalysts for epoxy react...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D303/42C07D301/02C08K5/1515
Inventor 张伟明景国林吴杰许梅芳张秋华蔡生祥
Owner 江苏悦达卡特新能源有限公司
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