Method for preparing epoxidized methyl acetorieinoleate

A technology for epoxy acetyl ricinole and methyl ricinoleate, which is applied in the field of preparing epoxy acetyl ricinoleate methyl ester, can solve problems such as reducing acetic anhydride and catalyst separation measures, and achieves short reaction time, little equipment corrosion, Easy-to-operate effects

Inactive Publication Date: 2010-07-14
JIANGSU POLYTECHNIC UNIVERSITY
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Problems solved by technology

[0006] The object of the invention is to overcome above-mentioned deficiencies in the prior art, provide a kind of method for the preparation epoxyacetyl ricinoleic acid methyl ester that a kind of acetylation reaction temperature is low, epoxidation reaction activity is high, the acetic anhydride that acetylation reaction is excessive and catalyzer do not Remove, and be used fo...

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  • Method for preparing epoxidized methyl acetorieinoleate
  • Method for preparing epoxidized methyl acetorieinoleate

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Embodiment 1

[0024] Embodiment 1: In 0.25L reactor, add ricinoleic acid methyl ester and acetic anhydride (molar mass ratio 1: 2), catalyst solid acid NaHSO 4 The addition amount is 1.5%, react at 70°C for 1 hour, and the conversion rate reaches 93.37%; the addition amount of hydrogen peroxide is 30%, the reaction temperature is 60°C, add hydrogen peroxide dropwise for 0.5 hour, and then react for 2.5 hours, the epoxy value of the product is 4.8.

Embodiment 2

[0025] Embodiment 2: In 0.25L reactor, add ricinoleic acid methyl ester and acetic anhydride (molar mass ratio 1: 2), catalyst solid acid NaHSO 4 The addition amount is 0.5%, reacted at 80°C for 2 hours, and the conversion rate reached 96.21%; the addition amount of hydrogen peroxide was 40%, the reaction temperature was 60°C, the hydrogen peroxide was added dropwise for 0.5 hour, and then reacted for 3 hours, the epoxy value of the product was 4.9.

Embodiment 3

[0026] Embodiment 3: in 0.25L reactor, add ricinoleic acid methyl ester and acetic anhydride (molar mass ratio 1: 2), catalyst solid acid NaHSO 4 The addition amount is 1%, react at 60°C for 3 hours, and the conversion rate reaches 90.36%; the addition amount of hydrogen peroxide is 40%, the reaction temperature is 70°C, add hydrogen peroxide dropwise for 0.5 hour, and react for another 2 hours, the epoxy value of the product is 5.0.

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Abstract

The invention relates to a method for preparing epoxidized methyl acetorieinoleate, which is processed by the following steps: (1) under the condition that the reaction pressure is the normal pressure and the reaction temperature is between the room temperature and 140 DEG C, adding a solid acid NaHSO4 catalyst into a mixed liquor of methyl ricinoleate and acetic anhydride, stirring the mixture, wherein the usage amount of the solid acid NaHSO4 catalyst occupies more than or equal to 0.1 percent of methyl ricinoleate by mass, the mole ratio of the methyl ricinoleate to the acetic anhydride is 1:1.5-2.5 and the reaction time is between 0.1 and 10 hours; (2) directly making the reaction liquid in the step (1) carry out epoxidation with aqueous solution of H2O2, wherein the mole ratio of methyl acetylricinolate to H2O2 is 1:1-2, the reaction temperature is between the room temperature and 100 DEG C, the reaction time is between 1 and 10 hours and the reaction pressure is the normal pressure; and (3) after washing the crude epoxidized methyl acetorieinoleate until the epoxidized methyl acetorieinoleate is neutral, dehydrating to obtain the refined epoxidized methyl acetorieinoleate. The method reduces the acetylation reaction temperature from 140 DEG C to between 60 and 80 DEG C and catalyzes the epoxidation of the acetylated product so as to improve the epoxide number of the epoxidation product.

Description

technical field [0001] The invention relates to a method for preparing epoxyacetyl ricinoleic acid methyl ester, which adopts ricinoleic acid methyl ester as raw material, solid acid NaHSO 4 As a catalyst, epoxyacetyl ricinoleic acid methyl ester can be prepared through acetylation and epoxidation. Background technique [0002] Epoxyacetyl ricinoleic acid methyl ester is a highly efficient, non-toxic and degradable plant epoxy plasticizer. The epoxy group can capture the free radical Cl- separated from the degradation of PVC, which can significantly improve the light resistance and durability of PVC products. Heat resistance, with the advantages of heat resistance, cold resistance, non-toxic, etc., it can be applied to process various packaging materials, toys and medical devices that come into contact with food. It is also a commonly used auxiliary heat stabilizer for PVC. It can be used together with organic metal salt stabilizers to reduce the amount of organic metal sal...

Claims

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Application Information

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IPC IPC(8): C07D303/42C07D301/16
Inventor 李为民邱玉华王车礼姚超李成燕
Owner JIANGSU POLYTECHNIC UNIVERSITY
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