The preparation method of methyl isocyanate

A technology of methyl isocyanate and monomethylamine, which is applied in the field of preparation of methyl isocyanate, can solve the problems of increasing three wastes, large equipment investment, and long preparation process, so as to reduce energy consumption and the generation of by-products, reduce production costs, The effect of improving one-way yield

Active Publication Date: 2017-01-25
HUNAN HAILI HIGH TECH IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, there are many reports about the preparation method of methyl isocyanate, such as German published patents 2422211, 2503270, U.S. patent 8969889, Japanese patents 42-8911, 46-24123, Chinese patents CN86100286, CN102976976A, etc.; The preparation method of base isocyanate all is to prepare methylcarbamoyl chloride first with phosgene and monomethylamine as raw material, then in the presence of inert solvent (such as carbon tetrachloride, trichloromethane, toluene etc.), methylcarbamoyl chloride Acyl chloride is decomposed and rectified to produce methyl isocyanate. Since the reaction of methyl carbamoyl chloride to generate methyl isocyanate and hydrogen chloride is a reversible reaction, the single-pass yield is low, and the molar percentage is about 60%. Therefore, the existing methyl In the preparation method of isocyanate, the whole preparation process requires repeated heating and condensation, and the preparation process is relatively long. On the one hand, there are more reaction by-products, trimeric methyl isocyanate, which in turn reduces the yield of methyl isocyanate and increases the three wastes; on the other hand, On the one hand, because the yield of methyl isocyanate prepared by the decomposition of methylcarbamoyl chloride is low, it is necessary to configure multiple decomposition reactors, which leads to large equipment investment

Method used

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  • The preparation method of methyl isocyanate

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preparation example Construction

[0025] The invention provides a kind of preparation method of methyl isocyanate, comprising:

[0026] 1) reacting phosgene and methylamine at 300-400°C, keeping the obtained reaction product at 200-300°C and mixing it with the first organic solvent to obtain a solution containing methyl isocyanate and a first gas phase substance;

[0027] 2) removing the organic solvent in the solution containing methyl isocyanate to obtain methyl isocyanate.

[0028] According to the present invention, the present invention first reacts phosgene and methylamine at 300-400° C., the molar ratio of said phosgene to said monomethylamine is (1.0-1.2): 1; the temperature of said reaction is preferably 350 ~380°C.

[0029] According to the present invention, the obtained reaction product is kept at 200-300°C and mixed with the first organic solvent to obtain a solution containing methyl isocyanate and the first gas-phase substance; the first organic solvent is benzene, toluene, chlorobenzene, di O...

Embodiment 1

[0049] Pass 5.94kg / hr of phosgene and 1.56kg / hr of monomethylamine into the tubular reactor, and carry out the reaction at 330°C. The obtained reaction product is controlled at 245°C and directly enters the tank containing chloroform from the bottom In the bubble tower with automatic chain control liquid level, the soluble methyl isocyanate is absorbed by chloroform, and the solution containing methyl isocyanate is sent to the de-lighting tower. The molar ratio of methyl isocyanate and chloroform in the bubble tower is 1 : 6, the operating temperature is 55°C. The gas at the top of the bubbling tower enters the absorption tower for absorption. The operating temperature of the absorption tower is 35°C. The solution containing methyl isocyanate is treated with phosgene removal in a stripping tower with automatic chain control of the liquid level in the tower kettle. The operating temperature of the tower kettle is 45°C. The gas at the top of the stripping tower is treated by the...

Embodiment 2

[0052] Pass 5.44kg / hr of phosgene and 1.56kg / hr of monomethylamine into the tubular reactor, and carry out the reaction at 350°C, and control the obtained reaction product at 260°C and directly enter the tank containing chloroform In the bubble tower with automatic chain control liquid level, the soluble methyl isocyanate is absorbed by chloroform, and the solution containing methyl isocyanate is sent to the de-lighting tower. The molar ratio of methyl isocyanate and chloroform in the bubble tower is 1 : 8, the operating temperature is 50°C. The gas at the top of the bubbling tower enters the absorption tower for absorption. The operating temperature of the absorption tower is 38°C. The solution containing methyl isocyanate is treated with phosgene removal in the delighting tower with automatic chain control of the liquid level in the tower kettle. The operating temperature of the tower kettle is 50°C. The gas at the top of the delightening tower is treated by the tower top co...

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Abstract

The invention provides a preparation method of methyl isocyanate. A reaction product synthesized at the high temperature is directly fed into a first organic solvent for treatment at the temperature of 200-300 DEG C, effective separation of the methyl isocyanate and hydrogen chloride is realized, the fact that the methyl isocyanate reacts with the hydrogen chloride to produce methyl carbamyl chloride is avoided, the once-through yield of the methyl isocyanate is increased, repeated heating and condensation are not required, energy consumption and production of by-products are reduced, meanwhile, multiple decomposition reactors are not required and the number of condensers is decreased in the aspect of devices, and the investment cost and the production cost are greatly reduced.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a method for preparing methyl isocyanate. Background technique [0002] Methyl isocyanate is an important pesticide intermediate, mainly used in the synthesis of carbamate pesticides, such as: carbofuran, methomyl, amethomyl, isoprocarb (Yechansan), secbucarb (Barba Sand), carbaryl, propoxur, haoanwei, thiodicarb, carbosulfan and butylthiuron, etc. [0003] At present, there are many reports about the preparation method of methyl isocyanate, such as German published patents 2422211, 2503270, U.S. patent 8969889, Japanese patents 42-8911, 46-24123, Chinese patents CN86100286, CN102976976A, etc.; The preparation method of base isocyanate all is to prepare methylcarbamoyl chloride first with phosgene and monomethylamine as raw material, then in the presence of inert solvent (such as carbon tetrachloride, trichloromethane, toluene etc.), methylcarbamoyl chloride Acyl chloride is de...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C265/04C07C263/10C07C263/20
Inventor 蒋卓良王晓光廖兰贵余晖陈蒙慈
Owner HUNAN HAILI HIGH TECH IND GRP
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