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Continuous preparation method of chloroformate

A technology of chloroformate and hydrogen chloride, which is applied in the preparation of phosgene or haloformate, organic chemistry, etc., can solve the problems of low single-pot production efficiency, high cost of waste gas treatment, high investment in fixed assets, and improve equipment utilization Efficiency, reducing the process of solvent removal and solvent recovery, and reducing the effect of auxiliary production time

Pending Publication Date: 2021-06-15
TIANJIN TIANDI CHUANGZHI TECH DEV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 1. The single-pot reaction time is about 24 hours, the reaction speed is slow, and the reaction selectivity is low
[0008] 2. The deacidification time is about 24 hours, and the single-pot production efficiency is low
[0009] 3. In order to increase production capacity, a large number of deacidification kettles need to be arranged, and the investment in fixed assets is high
[0010] 4. A large amount of nitrogen gas is required for deacidification, which leads to high energy consumption and high cost of waste gas treatment
[0011] 5. Most operations require manual on-site switching operations, which is low in automation, labor-intensive and not conducive to occupational health
[0012] 6. The raw material of phosgene needs a large excess, the consumption of phosgene is high, and the cost of waste gas treatment is high

Method used

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  • Continuous preparation method of chloroformate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] The process flow chart of the present invention's preparation methyl chloroformate is as figure 1 As shown, it specifically includes the following steps:

[0044] 1) The reactants methanol and phosgene are placed in the synthesis tower at a molar ratio of 1:1.1 for reaction, wherein methanol enters through the absorption tower at the top of the synthesis tower, and phosgene enters from the bottom of the synthesis tower, and the reaction temperature is 25 ℃, the two form a countercurrent in the synthesis tower and fully contact with each other to form the crude product methyl chloroformate and by-product hydrogen chloride;

[0045] 2) The crude product methyl chloroformate formed in the synthetic tower flows out from the bottom of the tower into the degassing tower. Carry out the removal of phosgene, and the released phosgene is combined with the raw material phosgene into the synthesis tower through pipelines to complete the recovery of phosgene; a small amount of hydr...

Embodiment 2

[0049]The method for preparing ethyl chloroformate of the present invention specifically comprises the following steps:

[0050] 1) The reactants ethanol and phosgene are placed in the synthesis tower at a molar ratio of 1:1.15 for reaction, wherein ethanol enters through the absorption tower at the top of the synthesis tower, phosgene enters from the bottom of the synthesis tower, and the reaction temperature is: At 20°C, the two form a countercurrent in the synthesis tower and fully contact with each other to form the crude product ethyl chloroformate and the by-product hydrogen chloride;

[0051] 2) The crude product ethyl chloroformate formed in the synthesis tower flows out from the bottom of the tower into the degassing tower. The top of the degassing tower is 40°C / the temperature of the bottom of the tower is 60°C, and the pressure at the top of the tower is -0.08MPa. Carry out the removal of phosgene, and the released phosgene is combined with the raw material phosgene...

Embodiment 3

[0053] The method for preparing benzyl chloroformate of the present invention specifically comprises the following steps:

[0054] 1) Put the reactants benzyl alcohol and phosgene in the synthesis tower at a molar ratio of 1:1.05, where the benzyl alcohol enters the top of the synthesis tower through the absorption tower, and the phosgene enters from the bottom of the synthesis tower. The temperature is: 15°C, the two form a countercurrent in the synthesis tower and fully contact with each other to form the crude product benzyl chloroformate and the by-product hydrogen chloride;

[0055] 2) The crude product benzyl chloroformate formed in the synthesis tower flows out from the bottom of the tower into the degassing tower. The removal of phosgene is carried out in the degassing tower, and the released phosgene is combined with the raw material phosgene into the synthesis tower to complete the recovery of phosgene; a small amount of hydrogen chloride gas in the degassing tower e...

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Abstract

The invention belongs to the technical field of chloroformate synthesis, and particularly relates to a continuous preparation method of chloroformate. The preparation method comprises the following steps: 1) feeding reactant raw material alcohol and phosgene into a synthesis tower through an absorption tower, and reacting to generate a crude product chloroformate and a byproduct hydrogen chloride; (2) feeding the crude product chloroformate formed in step (1) into a degassing tower, returning phosgene removed from the degassing tower into the synthesis tower, performing continuous reaction, and rectifying the chloroformate subjected to phosgene removal in a refining system to obtain the target product chloroformate; and 3) feeding a byproduct hydrogen chloride formed in step 1) into an absorption tower, washing with raw material alcohol, and feeding into a tail gas system. The method has the beneficial effects that synthesis and deacidification continuous production of the chloroformate product are realized, the synthesis reaction speed is increased, and the deacidification time is shortened; and meanwhile, phosgene is recycled, so that the consumption of the raw material is reduced, and clean and intrinsically safe automatic production is formed.

Description

technical field [0001] The invention belongs to the technical field of chloroformate synthesis, in particular to a continuous preparation method of chloroformate. Background technique [0002] At present, the most extensive chloroformate process technologies include: batch method, semi-continuous method, the synthesis and deacidification of chloroformate products take a long time, the production of continuous synthesis and continuous deacidification has not been realized, and the degree of automation is not high, and the consumption of raw materials high cost. [0003] The batch method is mainly to add a certain amount of alcohol and phosgene to the synthesis tank for reaction. After the reaction, the material is sent to the deacidification tank for nitrogen deacidification until the product reaches the target; the single tank reaction time is 24 hours, and the deacidification time is also At about 24 hours, the single-pot production efficiency is low and the reaction selec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C68/02C07C69/96
CPCC07C68/02C07C69/96
Inventor 胡辉张敏卿王群孝徐志宏李俊刘秉言佐毅温洪鹏李文鹏
Owner TIANJIN TIANDI CHUANGZHI TECH DEV
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