Novel process for preparing chloropropionyl chloride
A chloropropionyl chloride, a new technology, applied in the preparation of carboxylate, the preparation of organic compounds, organic chemistry, etc., can solve the problems of high cost, non-reusable, non-conforming phosphorous acid, etc., and achieve quantity and quality improvement , ideal catalytic effect, high temperature is not easy to carbonize the effect of less residue
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Embodiment 1
[0019] Embodiment 1: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:
[0020] 1: Acylation process
[0021] 1.1: Put the quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 50°C, react for 4 hours, let stand, cool down for 1 hour, and then separate the phosphorous acid in the lower layer;
[0022] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;
[0023] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the soli...
Embodiment 2
[0033] Embodiment 2: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:
[0034] 1: Acylation process
[0035] 1.1: Put the quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 60°C, react for 4 hours, let stand, cool down for 1.5 hours, and then separate the phosphorous acid in the lower layer ;
[0036] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;
[0037] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the...
Embodiment 3
[0047] Embodiment 3: a kind of new process of preparing chloropropionyl chloride, its specific operation steps are as follows:
[0048] 1: Acylation process
[0049] 1.1: Put quantitative propionic acid in the acylation tank, add phosphorus trichloride dropwise, raise the temperature after the dropwise addition, control the temperature in the acylation tank to 65°C, react for 4 hours, let stand, cool down for 2 hours, and then separate the phosphorous acid in the lower layer;
[0050] 1.2: Place the phosphorous acid obtained in step 1.1 in a barrel, and transfer the crude propionyl chloride in the upper layer to an acylation distillation tank;
[0051] 1.3: Transfer the phosphorous acid in step 1.2 to the hydrolysis tank, add an appropriate amount of activated carbon according to the color of the phosphorous acid to ensure that the phosphorous acid is colorless, and transfer the phosphorous acid in the hydrolysis tank to the storage tank before distillation through the solid-l...
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