Method for preparing epoxidized fatty acid methyl ester with microreactor one-step method

A technology of epoxy fatty acid methyl ester and microreactor, applied in the direction of organic chemistry and the like, can solve the problems of inability to prepare epoxy fatty acid methyl ester, inability to accurately control temperature, incapable of continuous production, etc., and achieve short reaction residence time and production equipment. Simple, easy-to-operate controls

Active Publication Date: 2013-03-27
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is that the epoxidation of fatty acid methyl esters in the existing technology cannot accurately control the temperature, the selectivity is low, the safety is not high, the epoxidation speed is low, and continuous production is not possible, especially it needs to be prepared and purified first. Fatty acid methyl esters cannot be directly prepared by one-step method of epoxy fatty acid methyl ester from oil, but a method for preparing epoxy fatty acid methyl ester by one-step method with microreactor is proposed

Method used

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  • Method for preparing epoxidized fatty acid methyl ester with microreactor one-step method
  • Method for preparing epoxidized fatty acid methyl ester with microreactor one-step method
  • Method for preparing epoxidized fatty acid methyl ester with microreactor one-step method

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Experimental program
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Effect test

Embodiment 1

[0038] Soybean oil (first raw material storage tank 1) and methanol solution of sodium methoxide (wherein sodium methoxide accounts for 1wt% of soybean oil (second raw material storage tank 2) are passed through the second raw material sequentially according to the molar ratio of soybean oil and methanol as 1:13 A microstructure mixer 3, a first heat exchanger 4, a first tubular temperature control module 5, and a first microstructure reactor 6, and react in the first microstructure reactor 6 at normal pressure and 75° C. for 7 minutes At the same time, the mixture of 30wt% hydrogen peroxide, 98wt% formic acid, 98wt% concentrated sulfuric acid and EDTA (the third raw material storage tank 7) is injected into the first microstructure reactor 6 through another constant flow pump. Two microstructure mixers 8, wherein the molar ratio of hydrogen peroxide and formic acid is 1:1, the added quality of concentrated sulfuric acid is 3% of the soybean oil quality, the added quality of ED...

Embodiment 2

[0040] Soybean oil (first raw material storage tank 1) and methanol solution of sodium methoxide (wherein sodium methoxide accounts for 1wt% of soybean oil (second raw material storage tank 2) pass through the first The microstructure mixer 3 , the first heat exchanger 4 , the first tubular temperature control module 5 and the first microstructure reactor 6 are reacted in the first microstructure reactor 6 at normal pressure and 75° C. for 7 minutes. At the same time, the mixture of 30wt% hydrogen peroxide, 98wt% formic acid, 98wt% concentrated sulfuric acid and urea (the third raw material storage tank 7) is fed into the second Microstructure mixer 8, wherein the molar ratio of hydrogen peroxide and formic acid is 1:1, the added mass of concentrated sulfuric acid is 4% of the mass of soybean oil, the mass of urea added is 3% of the mass of soybean oil, and the formic acid and soybean oil are guaranteed The molar ratio of the number of double bonds is 14:1, and the material pa...

Embodiment 3-8

[0042] Adopt the reaction condition identical with embodiment 1, difference is, embodiment 3-4 replaces soybean oil with cottonseed oil; Embodiment 5-6 replaces soybean oil with peanut oil, replaces formic acid with acetic acid simultaneously; Embodiment 7-8 uses Rapeseed oil was substituted for soybean oil; the epoxy fatty acid methyl ester product was obtained, and its epoxy value is shown in Table 1.

[0043] Table 1

[0044] Example number

[0045] 8

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Abstract

The invention discloses a method for preparing epoxidized fatty acid methyl ester with microreactor one-step method, comprising the following steps: injecting oil and fat, low-carbon alcohol and basic catalyst in a first microstructure reactor of a microchannel modularized reaction device, wherein the mole ratio of oil and fat to low-carbon alcohol is 1:11-17, and remaining for 3-10 min at the temperature of 65-85 DEG C; mixing outlet material of the first microstructure reactor with hydrogen peroxide, organic acid, acidic catalyst and stabilizing agent in a second microstructure reactor of the microchannel modularized reaction device, wherein the mole ratio of number of double bonds in organic acid to number of double bonds in oil and fat is 11-17:1, and remaining 1-5 min at the temperature of 65-95 DEG C; guiding the outlet material of the first microstructure reactor in a separator, standing for demixing to remove aqueous solution at lower layer; washing an organic phase at the upper layer with water till the pH is 6.5-7.5; and drying to obtain epoxidized fatty acid methyl ester.

Description

technical field [0001] The present invention relates to a preparation method of epoxy fatty acid methyl ester, in particular to a method for preparing plasticizer epoxy fatty acid methyl ester in a microstructure reactor by using oil, formic acid (or acetic acid), sulfuric acid (or phosphoric acid) and hydrogen peroxide as raw materials. ester method. Background technique [0002] Engineering plastics such as polyvinyl chloride (PVC) have a high glass transition temperature and are difficult to be thermoplastically processed. Plasticizers must be added to increase the plasticity of the material, making it easy to process and giving softness to the product. Phthalic plasticizers are the most important additives used in plastic processing, accounting for about 90% of plasticizers. However, it was found that phthalic acid plasticizers have persistent reproductive toxicity during application. In October 2008, the European Chemicals Agency explicitly banned the use in industries...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D303/42C07D301/16
Inventor 郭凯方正何伟欧阳平凯
Owner NANJING UNIV OF TECH
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