Method for preparing epoxy fatty acid methyl ester

A technology for epoxy fatty acid methyl ester and fatty acid methyl ester, which is applied in the field of preparing epoxy fatty acid methyl ester by using composite sulfate as a catalyst, can solve the problems of high cost, serious equipment corrosion, strong corrosiveness and the like, and achieves simple use and recovery. , The effect of reducing equipment corrosion and mild reaction conditions

Active Publication Date: 2011-05-18
JIANGSU ZHONGSHENG GAOKE ENVIRONMENTAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of using concentrated sulfuric acid as a catalyst to prepare epoxy fatty acid methyl ester is that liquid concentrated sulfuric acid is highly corrosive, inconvenient to store and use, and severely corrodes equipment. Therefore, it is necessary to use expensive corrosion-resistant alloys for preparation, and the investment cost of equipment is relatively high; Secondly, fatty acid esters are easily carbonized during the reaction process, resulting in a darker color of the product; moreover, the phenomenon of "overfilling the pot" is easy to occur due to the fast reaction speed, and the production safety is poor.
[0003] Chinese patent CN101235021 discloses the use of heteropolyacid liquid-phase catalyst, although the corrosion of the catalyst to equipment is reduced, but the heteropolyacid liquid-phase catalyst contains heavy metals, which will cause heavy metal pollution of products, and cannot be used as packaging materials for food and medicine, and Additives for toys and home decoration materials; secondly, the preparation of heteropolyacid catalysts is complicated, the process is long, and the cost is expensive
This method is complex and costly

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: 100g of fatty acid methyl ester, 4g of formic acid and 2g of compound sulfate (sodium bisulfate: iron sulfate: calcium sulfate = 60:30:10) were fully mixed. Stir and heat up to 60°C, add 50g of 30wt% hydrogen peroxide dropwise, one drop every 10 seconds. Insulated for 2 hours, stop the reaction, static layering, separate the catalyst of the lower floor, add sodium carbonate in the upper organic phase to wash to pH 6.5-7.5, dry to obtain epoxy fatty acid methyl ester, the yield is 99%, and the product ring Oxygen value 4.0.

Embodiment 2

[0018] Example 2: 100g of fatty acid methyl ester, 10g of formic acid and 2g of compound sulfate (sodium bisulfate: iron sulfate: calcium sulfate=70:25:5) were thoroughly mixed. Stir and heat up to 65°C, add 50g of 30wt% hydrogen peroxide dropwise, one drop every 10 seconds. After 3 hours of heat preservation, the epoxy value of the product was measured to be 4.4. Stop the reaction, remove the catalyst, wash with alkali, wash with water, and vacuum dry to obtain epoxy fatty acid methyl ester with a yield of 101%.

Embodiment 3

[0019] Example 3: 100g of fatty acid methyl ester, 8g of formic acid and 2g of compound sulfate (sodium bisulfate: iron sulfate: calcium sulfate=60:25:15) were fully mixed. Stir and heat up to 60°C, add 40g of 30wt% hydrogen peroxide dropwise, one drop every 10 seconds. After 4 hours of heat preservation, the epoxy value of the product was measured to be 3.9. Stop the reaction, remove the catalyst, wash with alkali, wash with water, and vacuum dry to obtain epoxy fatty acid methyl ester with a yield of 98%.

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Abstract

The invention relates to an improved method for preparing epoxy fatty acid methyl ester, which is characterized in that a solid catalyst or a sodium bisulfate solid catalyst obtained by mixing 30-90 parts of sodium bisulfate, 10-50 parts of ferric sulfate and 0-20 parts of calcium sulfate is adopted in an epoxidation reaction. By using the solid catalyst, when catalytic activity of the solid catalyst corresponds to that of sulfuric acid, the reaction condition is temperate; the production safety is good; the obtained product has high epoxy value which can reach more than 3.5; the epoxidation temperature is reduced to a certain degree, for example, the reaction temperature can be reduced by about 10 DEG C; and because too high temperature is needless, the fatty acid eater is not easy to be carbonized; the obtained product has light and bright color and luster and can be directly used for a light-color product without a decolorization process; the yield is also enhanced; and particularly the corrosivity to equipment is greatly reduced, thereby reducing equipment investment, maintainance and replacement. Meanwhile, the solid catalyst is simpler than a liquid catalyst in use and recovery aspects and is friendly to environment.

Description

technical field [0001] The invention is an improvement to the method for preparing epoxy fatty acid methyl ester, and in particular relates to a method for preparing epoxy fatty acid methyl ester by using composite sulfate as a catalyst. Background technique [0002] Epoxy fatty acid methyl ester can effectively replace dioctyl phthalate (DOP) as a non-toxic plasticizer. It is widely used in agricultural, film, cable, artificial leather, box, stationery and other processing industries. It can also be used as a softener for rubber products, a surfactant and a dispersant for epoxy coatings and epoxy resins. Its synthesis mainly adopts solvent method and solvent-free method. The solvent method brings pollution to the environment, the production process is long, the disposal of three wastes is large, and the product quality is poor. It has been basically replaced by the solvent-free method. The solvent-free method is mainly to react fatty acid ester, formic acid and hydrogen p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D301/12C07D303/40C07D303/42
Inventor 李为民许汉祥高琦
Owner JIANGSU ZHONGSHENG GAOKE ENVIRONMENTAL CO LTD
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