CN212403979U - Device for producing methyl isocyanate by dimethyl sulfate - Google Patents
Device for producing methyl isocyanate by dimethyl sulfate Download PDFInfo
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- CN212403979U CN212403979U CN202020744417.XU CN202020744417U CN212403979U CN 212403979 U CN212403979 U CN 212403979U CN 202020744417 U CN202020744417 U CN 202020744417U CN 212403979 U CN212403979 U CN 212403979U
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Abstract
The utility model belongs to the technical field of fine chemical synthesis, in particular to a device for producing methyl isocyanate by dimethyl sulfate; the device comprises a methyl isocyanate reactor, wherein the methyl isocyanate reactor is connected with a raw material solvent oil feeding pipeline, a sodium cyanate feeding pipeline and a dimethyl sulfate feeding pipeline, the methyl isocyanate reactor is connected with a methyl isocyanate condenser through a product discharging pipeline after reaction, and a mixture conveying pipeline after condensation is connected with a gas-liquid separation tank; the gas-liquid separation tank is connected with a methyl isocyanate reactor through a circulating solvent oil conveying pipeline, a nitrogen conveying pipeline is connected with a nitrogen compressor after gas-liquid separation, and the nitrogen compressor is connected with the methyl isocyanate reactor through a compressed nitrogen conveying pipeline; the gas-liquid separation tank is connected with a methyl isocyanate discharging pump through a gas-liquid separated methyl isocyanate conveying pipeline; the utility model discloses can use dimethyl sulfate to realize methyl isocyanate's serialization production, reaction rate is fast, and the yield is high.
Description
Technical Field
The utility model belongs to the technical field of fine chemical synthesis, concretely relates to device and serialization technology of dimethyl sulfate production methyl isocyanate.
Background
Methyl isocyanate is one of the most important varieties in monoalkyl isocyanates, is widely applied in many fields such as polymer industry, plastic industry, medical industry, pesticide industry and the like, and is a monomer for synthesizing polyisocyanates, polyurethanes, polyureas and high polymer adhesives; it is a major intermediate in the pesticide industry for the manufacture of carbamate insecticides like carbaryl, aldicarb, carbofuran, herbicides like prosulfocarb, foenicide, etc.; isocyanates of methyl
One carbon atom in the molecule is connected with two double bonds, so that the compound has the characteristics similar to a ketene structure, has strong addition property, can perform addition reaction with various compounds containing active hydrogen, such as phenol, oxime, amine, acid, alcohol, nitrogen-containing heterocyclic ring and other organic compounds, and is the reason for extremely wide application of the methyl isocyanate.
Methyl isocyanate has many synthesis process routes, and a methylamino formyl chloride thermal decomposition method is a route which is used for many years in foreign industrial mass production, and has the advantages that the technology is mature, the product yield and quality reach better levels, and the production scale is large, and is economic and reasonable; the defects are that the solvent circulation amount is large, the period is long, the toxicity of raw materials (phosgene) is high, the engineering and the equipment are complex, and the equipment corrosion is serious in the whole process; the cyanate method has been applied in recent years, wherein the route for synthesizing methyl isocyanate from dimethyl sulfate is the most common, and the reaction equation is as follows:
methyl isocyanate is flammable and highly toxic liquid, at present, the synthesis of methyl isocyanate from dimethyl sulfate in China is an intermittent production process, a reaction kettle needs to be frequently opened manually for feeding, and gases such as highly toxic methyl isocyanate and the like are easily volatilized into the air in the process, so that the environment and the safety of workers are influenced; therefore, it is necessary to design a device and a continuous process for producing methyl isocyanate by dimethyl sulfate, which can realize continuous operation, simple flow, low equipment investment and high reaction rate.
SUMMERY OF THE UTILITY MODEL
The utility model aims at overcoming the defects of the prior art and providing a device which has reasonable design, can realize continuous operation, simple flow, less equipment investment, high reaction rate and high yield for producing methyl isocyanate by dimethyl sulfate.
The purpose of the utility model is realized like this: a device for producing methyl isocyanate by dimethyl sulfate comprises a methyl isocyanate reactor, wherein the methyl isocyanate reactor is connected with a raw material solvent oil feeding pipeline, a sodium cyanate feeding pipeline and a dimethyl sulfate feeding pipeline, the methyl isocyanate reactor is connected with a methyl isocyanate condenser through a product discharging pipeline after reaction, and the methyl isocyanate condenser is connected with a gas-liquid separation tank through a mixture conveying pipeline after condensation; the gas-liquid separation tank is connected with the methyl isocyanate reactor through a circulating solvent oil conveying pipeline, the gas-liquid separation tank is connected with a nitrogen compressor through a nitrogen conveying pipeline after gas-liquid separation, the nitrogen compressor is connected with a nitrogen inlet pipeline, and the nitrogen compressor is connected with the methyl isocyanate reactor through a compressed nitrogen conveying pipeline; the gas-liquid separation tank is connected with an inlet of a methyl isocyanate discharging pump through a gas-liquid separated methyl isocyanate conveying pipeline, and an outlet of the methyl isocyanate discharging pump is connected with a methyl isocyanate product output pipeline.
The methyl isocyanate reactor is externally provided with a jacket capable of controlling the reaction temperature.
The lower part of methyl isocyanate reactor is provided with and is used for connecting respectively raw materials solvent oil inlet line sodium cyanate inlet line with dimethyl sulfate inlet line's raw materials import, the bottom of methyl isocyanate reactor is provided with and is used for connecting compressed nitrogen gas pipeline's nitrogen gas import, the top of methyl isocyanate reactor is provided with and is used for connecting the product export of product discharging line after the reaction, the upper portion of methyl isocyanate reactor is provided with and is used for connecting solvent oil backward flow import and the material export that is used for connecting other material discharging line after the reaction of circulation solvent oil pipeline.
And a gas distributor is arranged at the bottom of the methyl isocyanate reactor.
The methyl isocyanate reactor is a multistage loop reactor.
The gas distributor is an aeration head.
And the raw material solvent oil feeding pipeline, the sodium cyanate feeding pipeline and the dimethyl sulfate feeding pipeline are all provided with flow regulating valves.
The methyl isocyanate discharging pump is a positive displacement pump.
The continuous process for producing methyl isocyanate by using dimethyl sulfate uses the device for producing methyl isocyanate by using dimethyl sulfate, and comprises the following steps:
step one): the solvent oil and the sodium cyanate enter the methyl isocyanate reactor through the raw material solvent oil feeding pipeline and the sodium cyanate feeding pipeline respectively;
step two): dimethyl sulfate continuously enters the methyl isocyanate reactor through the dimethyl sulfate feed line;
step three): controlling the reaction temperature of the methyl isocyanate reactor to be between 150 ℃ and 190 ℃;
step four): nitrogen enters the methyl isocyanate reactor through the nitrogen inlet pipeline, the nitrogen compressor and the compressed nitrogen conveying pipeline;
step five): after the reaction, the product after the reaction enters the methyl isocyanate condenser through a product discharge pipeline, and the outlet temperature of the methyl isocyanate condenser is controlled to be less than 35 ℃;
step six): the condensed material enters the gas-liquid separation tank through the condensed mixture conveying pipeline, and the separated nitrogen returns to the methyl isocyanate reactor for recycling through the gas-liquid separated nitrogen conveying pipeline, the nitrogen compressor and the compressed nitrogen conveying pipeline; the separated solvent oil continuously flows back to the methyl isocyanate reactor through the circulating solvent oil conveying pipeline, and the methyl isocyanate after gas-liquid separation is taken as a product to be extracted through the methyl isocyanate conveying pipeline, the methyl isocyanate discharging pump and the methyl isocyanate product output pipeline after the gas-liquid separation;
step seven): and other reacted materials enter a recovery working section from the methyl isocyanate reactor through a discharge pipeline of the other reacted materials.
Preferably, the reaction temperature of the methyl isocyanate reactor D1 is controlled between 170 ℃ and 185 ℃.
The utility model has the advantages that: the utility model discloses a device of dimethyl sulfate production methyl isocyanate, it is main including the methyl isocyanate reactor, the methyl isocyanate condenser, the gas-liquid separation jar, nitrogen compressor and methyl isocyanate ejection of compact pump, raw materials solvent oil, sodium cyanate and dimethyl sulfate react at the methyl isocyanate reactor, the material after the reaction gets into the gas-liquid separation jar after the methyl isocyanate condenser condensation and separates, the solvent oil of separation gets into methyl isocyanate reactor circulation through circulation solvent oil pipeline and uses, the nitrogen gas of separation imports methyl isocyanate reactor circulation again through nitrogen compressor and uses, the methyl isocyanate after the separation can be adopted as the product behind the methyl isocyanate ejection of compact pump; in the reaction process, nitrogen is introduced into the methyl isocyanate reactor, so that a large density difference is generated between a high-gas-content area and a low-gas-content area in the reactor, the materials are pushed to form high-speed circulation inside, the materials are fully mixed and subjected to shearing and dissolving, the reaction is effectively promoted completely, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged in time at the upper part of the reactor, so that the side reaction caused by the retention of the methyl isocyanate generated in the original intermittent production process in the reaction kettle is avoided, and the yield is improved; the utility model discloses a device overall design of dimethyl sulfate production methyl isocyanate is reasonable, can use dimethyl sulfate to realize methyl isocyanate's serialization production, and operation flow is simple, and equipment investment is few, and reaction rate is fast, and the yield is high.
Drawings
Fig. 1 is a schematic structural diagram of a device for producing methyl isocyanate from dimethyl sulfate according to the present invention.
In the figure: d1, a methyl isocyanate reactor D2, a gas-liquid separation tank C1, a methyl isocyanate condenser C2, a nitrogen compressor P1, a methyl isocyanate discharge pump 1, a raw material solvent oil feed pipeline 2, a sodium cyanate feed pipeline 3, a dimethyl sulfate feed pipeline 4, a reacted product discharge pipeline 5, a condensed mixture conveying pipeline 6, a circulating solvent oil conveying pipeline 7, a gas-liquid separated nitrogen conveying pipeline 8, a nitrogen gas inlet pipeline 9, a compressed nitrogen conveying pipeline 10, a gas-liquid separated methyl isocyanate conveying pipeline 11, a methyl isocyanate product output pipeline 12 and reacted other material discharge pipelines.
Detailed Description
The present invention will be further described with reference to the accompanying drawings.
Example 1
As shown in fig. 1, an apparatus for producing methyl isocyanate from dimethyl sulfate comprises a methyl isocyanate reactor D1, wherein the methyl isocyanate reactor D1 is connected with a raw material solvent oil feed line 1, a sodium cyanate feed line 2 and a dimethyl sulfate feed line 3, the methyl isocyanate reactor D1 is connected with a methyl isocyanate condenser C1 through a product discharge line 4 after reaction, and the methyl isocyanate condenser C1 is connected with a gas-liquid separation tank D2 through a mixture conveying line 5 after condensation; the gas-liquid separation tank D2 is connected with the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6, the nitrogen conveying pipeline 7 of the gas-liquid separation tank D2 after gas-liquid separation is connected with a nitrogen compressor C2, the nitrogen compressor C2 is connected with a nitrogen inlet pipeline 8, and the nitrogen compressor C2 is connected with the methyl isocyanate reactor D1 through a compressed nitrogen conveying pipeline 9; the gas-liquid separation tank D2 is connected with the inlet of a methyl isocyanate discharge pump P1 through a gas-liquid separated methyl isocyanate conveying pipeline 10, and the outlet of the methyl isocyanate discharge pump P1 is connected with a methyl isocyanate product output pipeline 11.
The utility model discloses a device of dimethyl sulfate production methyl isocyanate, it is main including methyl isocyanate reactor D1, methyl isocyanate condenser C1, gas-liquid separation jar D2, nitrogen compressor C2 and methyl isocyanate ejection of compact pump P1, raw materials solvent oil, sodium cyanate and dimethyl sulfate react at methyl isocyanate reactor D1, the material after the reaction gets into methyl isocyanate condenser C1 and condenses the back and gets into gas-liquid separation jar D2 and separate, the solvent oil of separation gets into methyl isocyanate reactor D1 circulation use through circulation solvent oil pipeline 6, the nitrogen gas of separation reinjects into methyl isocyanate reactor D1 circulation use through nitrogen compressor C2, methyl isocyanate after the separation can be as the product behind methyl isocyanate ejection of compact pump P1 and adopt; in the reaction process, nitrogen is introduced into a methyl isocyanate reactor D1, so that on one hand, a high-gas-content area and a low-gas-content area in the reactor generate a large density difference, the materials are pushed to form high-speed circulation inside, the materials are fully mixed and subjected to shearing and dissolving, the reaction is effectively promoted completely, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged in time at the upper part of the reactor, so that the side reaction caused by the retention of the methyl isocyanate generated in the original intermittent production process in the reaction kettle is avoided, and the yield is improved; the utility model discloses a device overall design of dimethyl sulfate production methyl isocyanate is reasonable, can use dimethyl sulfate to realize methyl isocyanate's serialization production, and operation flow is simple, and equipment investment is few, and reaction rate is fast, and the yield is high.
Example 2
As shown in fig. 1, an apparatus for producing methyl isocyanate from dimethyl sulfate comprises a methyl isocyanate reactor D1, wherein the methyl isocyanate reactor D1 is connected with a raw material solvent oil feed line 1, a sodium cyanate feed line 2 and a dimethyl sulfate feed line 3, the methyl isocyanate reactor D1 is connected with a methyl isocyanate condenser C1 through a product discharge line 4 after reaction, and the methyl isocyanate condenser C1 is connected with a gas-liquid separation tank D2 through a mixture conveying line 5 after condensation; the gas-liquid separation tank D2 is connected with the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6, the nitrogen conveying pipeline 7 of the gas-liquid separation tank D2 after gas-liquid separation is connected with a nitrogen compressor C2, the nitrogen compressor C2 is connected with a nitrogen inlet pipeline 8, and the nitrogen compressor C2 is connected with the methyl isocyanate reactor D1 through a compressed nitrogen conveying pipeline 9; the gas-liquid separation tank D2 is connected with the inlet of a methyl isocyanate discharge pump P1 through a gas-liquid separated methyl isocyanate conveying pipeline 10, and the outlet of the methyl isocyanate discharge pump P1 is connected with a methyl isocyanate product output pipeline 11.
For better effect, the outer part of the methyl isocyanate reactor D1 is provided with a jacket capable of controlling the reaction temperature, and the reaction temperature in the methyl isocyanate reactor D1 can be controlled efficiently and rapidly through the jacket, so that the reaction stability is improved.
For better effect, the lower part of the methyl isocyanate reactor D1 is provided with raw material inlets respectively used for connecting the raw material solvent oil feed pipeline 1, the sodium cyanate feed pipeline 2 and the dimethyl sulfate feed pipeline 3, the bottom of the methyl isocyanate reactor D1 is provided with a nitrogen inlet used for connecting the compressed nitrogen conveying pipeline 9, the top of the methyl isocyanate reactor D1 is provided with a product outlet used for connecting the product discharge pipeline 4 after reaction, the upper part of the methyl isocyanate reactor D1 is provided with a solvent oil backflow inlet used for connecting the circulating solvent oil conveying pipeline 6 and a material outlet used for connecting the other material discharge pipelines 12 after reaction, and different positions of the methyl isocyanate reactor D1 are provided with connecting ports to realize the connection with external pipelines, so that the whole structure of the device is more reasonable, the overall layout and connection of the device are facilitated.
For better effect, the bottom of the methyl isocyanate reactor D1 is provided with a gas distributor, and nitrogen entering the methyl isocyanate reactor D1 can be effectively controlled by the gas distributor, so that the reaction is effectively promoted to be completely carried out, and the reaction rate is improved.
For better effect, the methyl isocyanate reactor D1 is a multistage loop reactor, further improving the reaction efficiency in the methyl isocyanate reactor D1, and improving the raw material processing speed to improve the yield.
For better effect, the gas distributor is an aerator, so that the mixing efficiency of nitrogen and reaction materials is improved, and the reaction rate is improved.
For better effect, all be provided with flow control valve on raw materials solvent oil feed line 1, sodium cyanate feed line 2 and the dimethyl sulfate feed line 3, be convenient for carry out flow control to the material that gets into in the methyl isocyanate reactor D1 fast, improve this device's operability.
For better effect, the methyl isocyanate discharging pump P1 is a positive displacement pump, has simple structure, is light and compact, and can further improve the safety and stability in the production process.
The utility model discloses a device of dimethyl sulfate production methyl isocyanate, it is main including methyl isocyanate reactor D1, methyl isocyanate condenser C1, gas-liquid separation jar D2, nitrogen compressor C2 and methyl isocyanate ejection of compact pump P1, raw materials solvent oil, sodium cyanate and dimethyl sulfate react at methyl isocyanate reactor D1, the material after the reaction gets into methyl isocyanate condenser C1 and condenses the back and gets into gas-liquid separation jar D2 and separate, the solvent oil of separation gets into methyl isocyanate reactor D1 circulation use through circulation solvent oil pipeline 6, the nitrogen gas of separation reinjects into methyl isocyanate reactor D1 circulation use through nitrogen compressor C2, methyl isocyanate after the separation can be as the product behind methyl isocyanate ejection of compact pump P1 and adopt; in the reaction process, nitrogen is introduced into a methyl isocyanate reactor D1, so that on one hand, a high-gas-content area and a low-gas-content area in the reactor generate a large density difference, the materials are pushed to form high-speed circulation inside, the materials are fully mixed and subjected to shearing and dissolving, the reaction is effectively promoted completely, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged in time at the upper part of the reactor, so that the side reaction caused by the retention of the methyl isocyanate generated in the original intermittent production process in the reaction kettle is avoided, and the yield is improved; the utility model discloses a device overall design of dimethyl sulfate production methyl isocyanate is reasonable, can use dimethyl sulfate to realize methyl isocyanate's serialization production, and operation flow is simple, and equipment investment is few, and reaction rate is fast, and the yield is high.
Example 3
A continuous process for producing methyl isocyanate from dimethyl sulfate, which uses the device for producing methyl isocyanate from dimethyl sulfate as shown in figure 1, can adopt the following steps:
180# solvent oil is fed into the methyl isocyanate reactor D1 through a raw material solvent oil feed line 1 and a sodium cyanate feed line 2 at the speed of 2000g/h and the speed of 267g/h, respectively, dimethyl sulfate is fed into the methyl isocyanate reactor D1 through a dimethyl sulfate feed line 3 at the speed of 323g/h, and the reaction temperature is controlled at 180 ℃ through a jacket; nitrogen was fed into the methyl isocyanate reactor D1 via the nitrogen compressor C2 at a rate of 6L/h; the reacted materials enter the methyl isocyanate condenser C1 through the reacted product discharge pipeline 4, and the outlet temperature of the methyl isocyanate condenser C1 is controlled to be less than 35 ℃; the condensed material enters the gas-liquid separation tank D2, and the separated nitrogen returns to the methyl isocyanate reactor D1 through the nitrogen compressor C2 for recycling; the separated solvent oil continuously flows back to the methyl isocyanate reactor D1, and the methyl isocyanate is taken out as a product through the methyl isocyanate discharging pump P1 at the speed of 189 g/h; other reacted materials are extracted by the discharging pipeline 12 of other reacted materials at 2400g/h and enter a recovery working section; the content of methyl isocyanate was 99.2% by chromatography.
Example 4
A continuous process for producing methyl isocyanate from dimethyl sulfate, which uses the device for producing methyl isocyanate from dimethyl sulfate as shown in figure 1, can adopt the following steps:
180# solvent oil is fed into the methyl isocyanate reactor D1 through a raw material solvent oil feed line 1 and a sodium cyanate feed line 2 at 1600g/h and sodium cyanate at 142g/h respectively, dimethyl sulfate is fed into the methyl isocyanate reactor D1 through a dimethyl sulfate feed line 3 at 172g/h, and the reaction temperature is controlled at 160 ℃ through a jacket; nitrogen was fed into the methyl isocyanate reactor D1 via the nitrogen compressor C2 at a rate of 4L/h; the reacted materials enter the methyl isocyanate condenser C1 through the reacted product discharge pipeline 4, and the outlet temperature of the methyl isocyanate condenser C1 is controlled to be less than 35 ℃; the condensed material enters the gas-liquid separation tank D2, and the separated nitrogen returns to the methyl isocyanate reactor D1 through the nitrogen compressor C2 for recycling; the separated solvent oil continuously flows back to the methyl isocyanate reactor D1, and the methyl isocyanate is taken out as a product at the speed of 100g/h through the methyl isocyanate discharging pump P1; other reacted materials are extracted by the discharging pipeline 12 of other reacted materials at the speed of 1814g/h and enter a recovery working section; the content of methyl isocyanate was 98.4% by chromatography.
Claims (8)
1. An apparatus for producing methyl isocyanate from dimethyl sulfate, which comprises a methyl isocyanate reactor (D1), and is characterized in that: the device is characterized in that the methyl isocyanate reactor (D1) is connected with a raw material solvent oil feeding pipeline (1), a sodium cyanate feeding pipeline (2) and a dimethyl sulfate feeding pipeline (3), the methyl isocyanate reactor (D1) is connected with a methyl isocyanate condenser (C1) through a product discharging pipeline (4) after reaction, and the methyl isocyanate condenser (C1) is connected with a gas-liquid separation tank (D2) through a mixture conveying pipeline (5) after condensation; the gas-liquid separation tank (D2) is connected with the methyl isocyanate reactor (D1) through a circulating solvent oil conveying pipeline (6), the gas-liquid separation tank (D2) is connected with a nitrogen compressor (C2) through a gas-liquid separated nitrogen conveying pipeline (7), the nitrogen compressor (C2) is connected with a nitrogen inlet pipeline (8), and the nitrogen compressor (C2) is connected with the methyl isocyanate reactor (D1) through a compressed nitrogen conveying pipeline (9); the gas-liquid separation tank (D2) is connected with the inlet of a methyl isocyanate discharge pump (P1) through a gas-liquid separated methyl isocyanate conveying pipeline (10), and the outlet of the methyl isocyanate discharge pump (P1) is connected with a methyl isocyanate product output pipeline (11).
2. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: the exterior of the methyl isocyanate reactor (D1) was provided with a jacket capable of controlling the reaction temperature thereof.
3. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: the lower part of methyl isocyanate reactor (D1) is provided with and is used for connecting respectively raw materials solvent oil inlet line (1), sodium cyanate inlet line (2) and the raw materials import of dimethyl sulfate inlet line (3), the bottom of methyl isocyanate reactor (D1) is provided with and is used for connecting the nitrogen gas import of compression nitrogen gas conveying pipeline (9), the top of methyl isocyanate reactor (D1) is provided with and is used for connecting the product export of reaction back product discharging line (4), the upper portion of methyl isocyanate reactor (D1) is provided with and is used for connecting the solvent oil backward flow import of circulation solvent oil conveying pipeline (6) and the material export that is used for connecting other material discharging pipeline (12) after the reaction.
4. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: the bottom of the methyl isocyanate reactor (D1) was provided with a gas distributor.
5. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: the methyl isocyanate reactor (D1) was a multistage loop reactor.
6. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 4, wherein: the gas distributor is an aeration head.
7. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: and the raw material solvent oil feeding pipeline (1), the sodium cyanate feeding pipeline (2) and the dimethyl sulfate feeding pipeline (3) are all provided with flow regulating valves.
8. The apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: the methyl isocyanate discharging pump (P1) is a positive displacement pump.
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| CN202020744417.XU CN212403979U (en) | 2020-05-08 | 2020-05-08 | Device for producing methyl isocyanate by dimethyl sulfate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114276277A (en) * | 2021-12-21 | 2022-04-05 | 福建南方济民医药研发中心有限公司 | Preparation method of methyl isocyanate |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114276277A (en) * | 2021-12-21 | 2022-04-05 | 福建南方济民医药研发中心有限公司 | Preparation method of methyl isocyanate |
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