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A technology of methyl chloroformate and a synthesis method, applied in the field of synthesis of methyl chloroformate, can solve problems such as many by-products, and achieve the effects of improving conversion rate, sufficient methanol reaction, and avoiding side reactions
Pending Publication Date: 2021-10-22
ANHUI DONGZHI GUANGXIN AGROCHEMICAL CO LTD
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[0004] The object of the present invention is to provide a kind of synthetic method of methyl chloroformate, replace the gas-liquid reaction of methanol and phosgene with...
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Embodiment 1
[0040] A synthetic method for methyl chloroformate, comprising the following steps:
[0041] Step 1. Purification of methanol: put methanol into a rectification tower, and carry out rectification and purification of methanol to reduce the occurrence of side reactions in the subsequent esterification reaction, wherein the rectification temperature is controlled at 65°C;
[0042] Step 2. Gasification of methanol: Put the purified methanol into the gasification tower to gasify the methanol to obtain methanol gas, wherein the gasification temperature is set to 70°C;
[0043] Step 3, the synthesis of phosgene: pass carbon monoxide and chlorine gas into the phosgene generating tower according to the molar ratio of 1:1.05, and synthesize and react to generate phosgene under the catalytic action of activated carbon;
[0044] Step 4, gas phase esterification reaction: Introduce nitrogen into the esterification tower for 15 minutes, drive away the air in the esterification tower, contro...
Embodiment 2
[0047] A synthetic method for methyl chloroformate, comprising the following steps:
[0048] Step 1. Purification of methanol: put methanol into a rectification tower, and carry out rectification and purification of methanol to reduce the occurrence of side reactions in the subsequent esterification reaction, and the rectification temperature is controlled at 68°C;
[0049] Step 2. Gasification of methanol: Put the purified methanol into the gasification tower to gasify the methanol to obtain methanol gas, wherein the gasification temperature is set to 75°C;
[0050] Step 3, the synthesis of phosgene: pass carbon monoxide and chlorine into the phosgene generating tower according to the molar ratio of 1:1.05, and synthesize and react to generate phosgene under the catalytic action of activated carbon;
[0051] Step 4, gas-phase esterification reaction: feed nitrogen into the esterification tower for 15 minutes, drive away the air in the esterification tower, control the flow of...
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Abstract
The invention discloses a synthesis method of methyl chloroformate, and belongs to the technical field of production of methyl chloroformate. The synthesis method of the methyl chloroformate comprises the following steps: step 1, purifying methanol; step 2, gasifying methanol; step 3, synthesizing phosgene; and 4, carrying out gas-phase esterification reaction. Gas-phase reaction of methanol gas and phosgene is utilized, and contact among gas-phase reaction molecules is more sufficient than contact among gas-liquid reaction molecules, so that the conversion rate of methanol is increased; through the arrangement of a circular baffle, a rotating shaft, a circulating gas pipe and a circulating pump, the mixing degree and the contact time between methanol gas and phosgene are increased, so that methanol reaction is more sufficient, side reaction of excessive methanol and methyl chloroformate is avoided, and the purity of methyl chloroformate and the conversion rate of methanol are improved; and methanol gas and phosgene are introduced by means of batch circulation, so that the phosgene is always excessive, and meanwhile, the phosgene is not excessive, and the tail gas treatment pressure is reduced.
Description
technical field [0001] The invention belongs to the technical field of methyl chloroformate production, in particular to a synthetic method of methyl chloroformate. Background technique [0002] Methyl chloroformate is an important intermediate in the synthesis of carbendazim, which is generally obtained by the reaction of phosgene and methanol. Mass production generally adopts a glass-lined reaction tower. First add methanol to the tower, control the reaction temperature at 20-30°C, and then ventilate methanol and phosgene from the bottom of the tower in the same direction to obtain methyl chloroformate. The reaction formula of this process is as follows : COCl 2 +CH 3 OH=C 2 h 3 ClO 2 +HCl. This process mainly uses the gas-liquid reaction of methanol and phosgene, and the generated methyl chloroformate has more by-products, and the conversion rate of methanol is lower. [0003] Therefore, the present invention proposes a kind of synthetic method of methyl chloroform...
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