Method for rectifying dimethyl phosphite
A dimethyl phosphite and rectification technology, which is applied in the field of synthesis and preparation of pharmaceutical intermediates, can solve problems such as difficult industrial production, complex reactant components, and low equipment utilization, and achieve good product quality and low cost , the effect of short production time
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Embodiment 1
[0018] A kind of rectification method of dimethyl phosphite,
[0019] Specific steps are as follows:
[0020] Add methanol 1800L and phosphorus trichloride 1620 into the esterification reaction kettle at a volume ratio of 1:0.9 at a flow rate of 71L / min and 50L / min respectively, start stirring, and slowly heat up. After a period of reaction, pass a sampling port and take a sample for TLC Detect until the raw materials are completely reacted, and the crude product of dimethyl phosphite is obtained after the reaction is completed.
[0021] Put the reacted crude ester into the rectification kettle for rectification. (The height of the first rectification tower is 4m, and the height of the second rectification tower is 8m). Turn on the stirring and slowly raise the temperature. When the first rectification tower and the second rectification tower reach the set temperature, turn on the condensate gas At the same time, open the circulating hot water for cooling of the top condense...
Embodiment 2
[0023] A kind of rectification method of dimethyl phosphite,
[0024] Specific steps are as follows:
[0025] Add methanol 1800L and phosphorus trichloride 1620L phosphorus trichloride to the esterification reactor at a flow rate of 71L / min and 50L / min respectively according to the volume ratio of 1:0.9, start stirring, slowly raise the temperature, and after a period of reaction, pass a sample Take a sample for TLC detection until the reaction of the raw materials is complete, and the crude product of dimethyl phosphite is obtained after the reaction ends.
[0026] Put the reacted crude ester into the rectification kettle for rectification. (The height of the first rectification tower is 5m, and the height of the second rectification tower is 9m). Turn on the stirring and slowly raise the temperature. At the same time, open the circulating hot water for cooling of the top condenser of the second rectification tower, start the vacuum system, open the reflux ratio regulator o...
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