Method for efficiently and environmentally friendly preparing dibutyl itaconate on basis of heterogeneous catalysis
A technology of di-n-butyl itaconate and heterogeneous catalysis, which is applied in chemical instruments and methods, preparation of organic compounds, preparation of carboxylic acid esters, etc., can solve problems affecting product color and performance, many reaction by-products, and product color To achieve the effects of high product yield, less discharge of three wastes, and light product color
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Embodiment 1
[0032] The purchased sodium type D001 type macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution with a hydrochloric acid concentration of 4% for 6 hours of replacement.
[0033] Weigh 13.01g of itaconic acid and 29.648g of n-butanol, add it into a three-necked flask with a water separator and a thermometer, magnetically stir and heat up, and weigh 0.6505g of hydrogenated D001 type strongly acidic cation after itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, start timing after heating to 110°C, and react for 4 hours to obtain the crude product of di-n-butyl itaconate; stop heating, cool to room temperature and filter, and the filtrate is washed with anhydrous sodium sulfate and dried. Pressure distillation, the unreacted n-butanol obtained in the first stage is used for the next esterification reaction, and the finished product of di-n-butyl itaconate is obta...
Embodiment 2
[0035] The purchased sodium type D001 macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution of 5% hydrochloric acid for 8 hours of replacement.
[0036] Weigh 13.01g of itaconic acid and 25.942g of n-butanol, add it into a three-necked flask with a water separator and a thermometer, stir it magnetically and raise the temperature, and weigh 1.301g of hydrogenated D001 type strongly acidic cation after the itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, heat it to 115°C, start timing, and react for 4 hours to obtain the crude product of di-n-butyl itaconate; the subsequent purification process is the same as in Example 1 to obtain the finished product of di-n-butanol itaconate. The rate is 97.8%.
Embodiment 3
[0038] The purchased sodium type D001 macroporous strongly acidic cation exchange resin was washed with absolute ethanol and deionized water, and then placed in a solution with a hydrochloric acid concentration of 6% for 8 hours of replacement.
[0039] Weigh 26.02g of itaconic acid and 59.296g of n-butanol, add it to a three-necked flask with a water separator and a thermometer, magnetically stir and heat up, and weigh 3.2525g of hydrogenated D001 type strongly acidic cation after the itaconic acid is completely dissolved Put the exchange resin into the three-necked flask, heat it to 120°C, start timing, and react for 5 hours to obtain the crude product of di-n-butyl itaconate; the subsequent purification process is the same as in Example 1 to obtain the finished product of di-n-butanol itaconate, The rate is 96.4%.
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