Method for synthesizing methyl 4-chloroacetoacetate or ethyl 4-chloroacetoacetate
A technology of ethyl chloroacetoacetate and methyl acetate, which is applied in the field of synthesizing methyl 4-chloroacetoacetate or ethyl 4-chloroacetoacetate, can solve the problems of large amount of waste water, achieve less chlorine-containing by-products, reduce Pollution, the effect of sufficient chlorine reaction
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Embodiment 1
[0037] Embodiment 1 synthetic 4-chloroacetoacetate methyl ester
[0038] (1) Chlorination: Add the first part of solvent 1500Kg dichloroethane into the chlorination kettle and cool down to -5°C, then mix the second part of solvent 750Kg dichloroethane and 320Kg diketene into the chlorination kettle to continue cooling to -20°C, then feed 272Kg of chlorine gas into the chlorination kettle, and control the temperature of the chlorination kettle at -18°C during the process of introducing chlorine gas; / h; when the quality of chlorine gas is 190.4-231.2Kg, the flow rate is 20kg / h; when the quality of chlorine gas is 321.2-258.4Kg, the flow rate is 12kg / h; When the mass is 258.4-272Kg, the flow rate is 10kg / h.
[0039] (2) Esterification: After the chlorine gas feeds in, add 123Kg of methanol dropwise to the chlorination kettle; stir evenly after the methanol dropwise addition, then the material is transported from the chlorination kettle to the warming still, and the temperature ...
Embodiment 2
[0043] Embodiment 2 synthetic 4-chloroacetoacetate methyl ester
[0044] (1) Chlorination: Add the first part of solvent 1500Kg dichloroethane into the chlorination kettle and cool down to -7°C, then mix the second part of solvent 750Kg dichloroethane and 321.7Kg diketene into the chlorination kettle to continue Cool down to -20°C, and then feed 270.56Kg of chlorine gas into the chlorination tank. During the process of introducing chlorine gas, the temperature of the chlorination tank is controlled at -20°C; when the mass of chlorine gas is 0-190.4Kg, the flow rate 25kg / h; when the quality of chlorine gas is 190.4-231.2Kg, the flow rate is 20kg / h; when the quality of chlorine gas is 321.2-258.4Kg, the flow rate is 12kg / h; When the incoming mass is 258.4-271Kg, the incoming flow rate is 10kg / h.
[0045] (2) Esterification: After the chlorine gas feeds in, add 123Kg of methanol dropwise to the chlorination kettle; stir evenly after the methanol dropwise addition, then the mater...
Embodiment 3
[0048] Embodiment 3 synthetic 4-chloroacetoacetate methyl esters
[0049] (1) Chlorination: Add the first part of solvent 1500Kg dichloroethane into the chlorination kettle and cool down to -10°C, then mix the second part of solvent 750Kg dichloroethane and 316.3Kg diketene into the chlorination kettle to continue Cool down to -20°C, and then feed 275.2Kg of chlorine gas into the chlorination kettle. During the process of introducing chlorine gas, the temperature of the chlorination kettle is controlled at -18°C; when the mass of chlorine gas is 0-190.4Kg, the flow rate 25kg / h; when the quality of chlorine gas is 190.4-231.2Kg, the flow rate is 20kg / h; when the quality of chlorine gas is 321.2-258.4Kg, the flow rate is 12kg / h; When the incoming mass is 258.4~276g, the incoming flow rate is 10kg / h;
[0050] (2) Esterification: After the chlorine gas feeds in, add 123Kg of methanol dropwise to the chlorination kettle; stir evenly after the methanol dropwise addition, then the m...
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