A kind of acetylated citric acid fatty acid ester plasticizer and its preparation method and application
A technology for acetylating citric acid and fatty acid ester, applied in the preparation of carboxylic acid ester, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as poor compatibility, precipitation, etc. Inexpensive and accessible effects
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Embodiment 1
[0028] The first step, the preparation of epoxidized methyl oleate: get the hydrogen peroxide 45mL of 30wt.% concentration and add dropwise in the there-necked flask that has added 30g methyl oleate, 30mL acetic acid and 1.5g ion exchange resin catalyst, control hydrogen peroxide in After 1.5 hours of dropwise addition, the temperature should not be higher than 65°C, and then keep the temperature at 65°C for 3 hours. After the reaction, neutralize with 4wt.% sodium carbonate solution, wash with water until neutral, and then dry to obtain an epoxy value of 3.6%. Pale yellow epoxidized methyl oleate.
[0029] In the second step, citric acid and epoxidized fatty acid methyl ester ring-opening reaction prepare citric acid fatty acid ester, the epoxidized methyl oleate 100g obtained in the first step, citric acid 13g, antioxidant 1010 0.1g and catalyst Dimethylimidazole 0.4g, reacted at 140°C for 3 hours to obtain a crude product with an acid value of 0.82mg / g, then distilled out t...
Embodiment 2
[0032] The first step, the preparation of epoxidized fatty acid methyl ester: the hydrogen peroxide 50mL that gets 30wt.% concentration is added dropwise to the ethyl acetate that has added 30g methyl oleate, 20mL and 1.2g phosphotungstic heteropolyacid quaternary ammonium salt catalyst In the three-necked flask, the hydrogen peroxide is controlled to be added dropwise in 2.0 hours, and the temperature is not higher than 65°C. After that, the temperature is kept at 65°C for 3 hours. After the reaction is completed, it is neutralized with 4wt.% sodium carbonate solution, washed with water until neutral, and then dried to obtain epoxy Value 4.1% yellowish epoxidized methyl oleate.
[0033] In the second step, citric acid and epoxidized fatty acid methyl ester ring-opening reaction prepare citric acid fatty acid ester, the epoxidized methyl oleate 100g obtained in the first step, citric acid 14g, antioxidant 168 0.1g and catalyst 0.3g of diethylenetriamine was reacted at 140°C fo...
Embodiment 3
[0036] The first step, the preparation of epoxidized methyl ricinoleate: get the hydrogen peroxide 55mL of 30wt.% concentration and add dropwise to the ethyl acetate that has added 30g methyl ricinoleate, 20mL and 1.2g phosphotungstic heteropolyacid quaternary ammonium In the three-necked flask of the salt catalyst, control the dropwise addition of hydrogen peroxide in 2 hours, the reaction temperature is not higher than 65 ° C, and then maintain the temperature of 65 ° C for 3 hours, after the reaction is completed, neutralize with 4% sodium carbonate solution, wash with water until neutral, and then dry. The epoxidized ricinoleic acid methyl ester with an epoxy value of 3.8% was obtained as light yellow.
[0037] In the second step, citric acid and epoxidized ricinoleic acid methyl ester ring-opening reaction prepare citric acid fatty acid ester, and the epoxidized ricinoleic acid methyl ester 100g that the first step obtains, citric acid 14g, 50% of the second Phosphoric ac...
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