A method of producing dimethyl succinate
A technology of dimethyl succinate and its production method, which is applied in the preparation of carboxylic acid esters, chemical instruments and methods, and the preparation of organic compounds, and can solve the problems of highly toxic dimethyl sulfate, waste of materials, and difficulty in removing water in time and other problems, to achieve the effect of simplified process, short process, simple equipment, small quantity, and stable product quality
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Embodiment 1
[0031] Add 110Kg of potassium hydrogensulfate monohydrate, 366Kg of succinic acid, and 412Kg of methanol into an esterification kettle with an internal reflux condenser, and perform an esterification reaction under normal pressure internal reflux for 5 hours, and the internal temperature of the kettle is stabilized at 82°C to stop the reaction. Obtain crude ester, after cooling and standing still, suction filter to rectifying still;
[0032] Recover methanol under normal pressure, distill water under slight negative pressure; vacuum rectify to obtain the finished product dimethyl succinate;
[0033] Monomethyl succinate and a small amount of entrained potassium bisulfate stay in the rectifying still and send back to the esterification still; reclaim the methanol in the methanol aqueous solution and recycle;
[0034] When the obtained crude ester content≤80%, use denatured methanol to activate the catalyst; the activation method includes the following steps:
[0035] Add denat...
Embodiment 2
[0039] Add 110Kg of potassium hydrogensulfate monohydrate, 366Kg of succinic acid, and 412Kg of methanol into an esterification kettle with an internal reflux condenser, and react for 3.5 hours under a pressure of 0.20Mpa. The temperature in the kettle is stabilized at 99.7°C, and the reaction is stopped to obtain Crude ester, after cooling and standing still, suction filter to rectifying still;
[0040] Methanol is recovered under normal pressure, water is distilled out under slight negative pressure; the finished product dimethyl succinate is obtained through vacuum rectification.
[0041] Monomethyl succinate and a small amount of entrained potassium bisulfate remain in the rectifying still and are sent back to the esterification still;
[0042] Recover the methanol in the methanol aqueous solution and recycle it;
[0043] When the obtained crude ester content≤80%, use denatured methanol to activate the catalyst; the activation method includes the following steps:
[0044...
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