Method for synthesizing 2-chlorobutyric acid
A technology of chlorobutyric acid and n-butyric acid, which is applied in the preparation of carboxylic acid anhydride, chemical recovery and other directions, can solve the problems such as the inability to recycle the catalyst, the by-product 3-chlorobutyric acid is too much, and the reaction time is long, so as to reduce excessive chlorine The effect of improving the environmental protection effect and high utilization rate
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Embodiment 1
[0016] 1) Add n-butyric acid and butyric anhydride in the reaction vessel, stir evenly at room temperature, the mass ratio of n-butyric acid and butyric anhydride is 1:0.5;
[0017] 2) continuous chlorine gas, the reaction temperature is controlled at 95 ° C, normal pressure, the reaction time is 5 hours, the mol ratio of the amount of chlorine to n-butyric acid is 2: 1 (during the reaction, check the conversion rate of n-butyric acid and control it at 85 %~95% to prevent over-chlorination);
[0018] 3) Add water equimolar to butyric anhydride, and hydrolyze it into n-butyric acid at 50°C under normal pressure; the hydrolyzed crude material contains 2-chlorobutyric acid, 3-chlorobutyric acid, n-butyric acid and other by-products. Detected by gas chromatography: 65% of 2-chlorobutyric acid, 33% of n-butyric acid, 0.99% of 3-chlorobutyric acid, 0.46% of 4-chlorobutyric acid, and 0.55% of others.
[0019] 4) The crude material is rectified to obtain 2-chlorobutyric acid with a c...
Embodiment 2
[0022] 1) Add n-butyric acid and butyric anhydride in the reaction vessel, stir evenly at room temperature, the mass ratio of n-butyric acid and butyric anhydride is 1:1;
[0023] 2) continuous chlorine gas, the reaction temperature is controlled at 90°C, normal pressure, the reaction time is 7 hours, the molar ratio of the amount of chlorine to n-butyric acid is 2.5: 1 (during the reaction, check the conversion rate of n-butyric acid and control it at 85 %~95% to prevent over-chlorination);
[0024] 3) Add water equimolar to butyric anhydride, and hydrolyze it into n-butyric acid at 50°C under normal pressure; the hydrolyzed crude material contains 2-chlorobutyric acid, 3-chlorobutyric acid, n-butyric acid and other by-products;
[0025] 4) The crude material is rectified to obtain 2-chlorobutyric acid with a content of more than 99%, and the yield of 2-chlorobutyric acid is 98%.
[0026] The rectification can also obtain n-butyric acid with a content of more than 99%, and ...
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