CN111454179A - Device and continuous process for producing methyl isocyanate by using dimethyl sulfate - Google Patents
Device and continuous process for producing methyl isocyanate by using dimethyl sulfate Download PDFInfo
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- CN111454179A CN111454179A CN202010382901.7A CN202010382901A CN111454179A CN 111454179 A CN111454179 A CN 111454179A CN 202010382901 A CN202010382901 A CN 202010382901A CN 111454179 A CN111454179 A CN 111454179A
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Abstract
The invention belongs to the technical field of fine chemical synthesis, and particularly relates to a device for producing methyl isocyanate by dimethyl sulfate and a continuous process; 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 invention can realize the continuous production of methyl isocyanate by using dimethyl sulfate, and has high reaction rate and high yield.
Description
Technical Field
The invention belongs to the technical field of fine chemical synthesis, and particularly relates to a device for producing methyl isocyanate by dimethyl sulfate and a continuous process.
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.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a continuous process for producing methyl isocyanate by dimethyl sulfate, which have the advantages of reasonable design, continuous operation realization, simple flow, low equipment investment, high reaction rate and high yield.
The purpose of the invention is realized as follows: 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 invention has the beneficial effects that: the invention relates to a device for producing methyl isocyanate by dimethyl sulfate, which mainly comprises a methyl isocyanate reactor, a methyl isocyanate condenser, a gas-liquid separation tank, a nitrogen compressor and a methyl isocyanate discharge pump, wherein raw material solvent oil, sodium cyanate and dimethyl sulfate react in the methyl isocyanate reactor, reacted materials enter the methyl isocyanate condenser to be condensed and then enter the gas-liquid separation tank to be separated, the separated solvent oil enters the methyl isocyanate reactor for recycling through a circulating solvent oil conveying pipeline, the separated nitrogen is re-input into the methyl isocyanate reactor for recycling through the nitrogen compressor, and the separated methyl isocyanate can be taken as a product to be extracted after passing through the methyl isocyanate discharge 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 device for producing methyl isocyanate by dimethyl sulfate has reasonable integral design, and the continuous process for producing methyl isocyanate by dimethyl sulfate can realize continuous production of methyl isocyanate by dimethyl sulfate by using the device, and has the advantages of simple operation flow, less equipment investment, high reaction rate and high yield.
Drawings
FIG. 1 is a schematic structural diagram of a device for producing methyl isocyanate from dimethyl sulfate according to the 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 invention is further described below 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 invention relates to a device for producing methyl isocyanate by dimethyl sulfate, which mainly comprises a methyl isocyanate reactor D1, a methyl isocyanate condenser C1, a gas-liquid separation tank D2, a nitrogen compressor C2 and a methyl isocyanate discharge pump P1, wherein raw material solvent oil, sodium cyanate and dimethyl sulfate react in the methyl isocyanate reactor D1, reacted materials enter the methyl isocyanate condenser C1 for condensation and then enter the gas-liquid separation tank D2 for separation, the separated solvent oil enters the methyl isocyanate reactor D1 for recycling through a circulating solvent oil conveying pipeline 6, the separated nitrogen is input into the methyl isocyanate reactor D1 for recycling through the nitrogen compressor C2, and the separated methyl isocyanate can be extracted as a product after passing through the methyl isocyanate discharge pump P1; 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 device for producing methyl isocyanate by dimethyl sulfate has reasonable integral design, can realize continuous production of methyl isocyanate by dimethyl sulfate, and has simple operation flow, less equipment investment, high reaction rate and high yield.
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 invention relates to a device for producing methyl isocyanate by dimethyl sulfate, which mainly comprises a methyl isocyanate reactor D1, a methyl isocyanate condenser C1, a gas-liquid separation tank D2, a nitrogen compressor C2 and a methyl isocyanate discharge pump P1, wherein raw material solvent oil, sodium cyanate and dimethyl sulfate react in the methyl isocyanate reactor D1, reacted materials enter the methyl isocyanate condenser C1 for condensation and then enter the gas-liquid separation tank D2 for separation, the separated solvent oil enters the methyl isocyanate reactor D1 for recycling through a circulating solvent oil conveying pipeline 6, the separated nitrogen is input into the methyl isocyanate reactor D1 for recycling through the nitrogen compressor C2, and the separated methyl isocyanate can be extracted as a product after passing through the methyl isocyanate discharge pump P1; 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 device for producing methyl isocyanate by dimethyl sulfate has reasonable integral design, can realize continuous production of methyl isocyanate by dimethyl sulfate, and has simple operation flow, less equipment investment, high reaction rate and high yield.
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 enters the methyl isocyanate reactor D1 through a raw material solvent oil feeding pipeline 1 and a sodium cyanate feeding pipeline 2 at the speeds of 2000g/h and 267g/h, dimethyl sulfate enters the methyl isocyanate reactor D1 through a dimethyl sulfate feeding pipeline 3 at the speed of 323g/h, the reaction temperature is controlled to be 180 ℃ through a jacket, nitrogen enters the methyl isocyanate reactor D1 through a nitrogen compressor C2 at the speed of 6L/h, the reacted materials enter a methyl isocyanate condenser C1 through a product discharging pipeline 4 after the reaction, the outlet temperature of the methyl isocyanate condenser C1 is controlled to be lower than 35 ℃, the condensed materials enter a gas-liquid separation tank D2, the separated nitrogen returns to the methyl isocyanate reactor D1 through the nitrogen compressor C2 for recycling, the separated solvent oil continuously returns to the methyl isocyanate reactor D1, the methyl isocyanate serving as a product through a methyl isocyanate discharging pump P1 and is collected at the speed of 189g/h, the other reacted materials enter a chromatographic material collection section at the speed of 2400.2 after the reaction, and the content of other materials is collected as a chromatographic recovery section.
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 enters the methyl isocyanate reactor D1 through a raw material solvent oil feeding pipeline 1 and a sodium cyanate feeding pipeline 2 at 1600g/h and sodium cyanate at 142g/h respectively, dimethyl sulfate enters the methyl isocyanate reactor D1 through a dimethyl sulfate feeding pipeline 3 at 172g/h, the reaction temperature is controlled at 160 ℃ through a jacket, nitrogen enters the methyl isocyanate reactor D1 through a nitrogen compressor C2 at 4L/h, the reacted material enters the methyl isocyanate condenser C1 through a product discharging pipeline 4 after the reaction, the outlet temperature of the methyl isocyanate condenser C1 is controlled to be lower than 35 ℃, the condensed material enters the gas-liquid separation tank D2, the separated nitrogen returns to the methyl isocyanate reactor D1 through the nitrogen compressor C2 for recycling, the separated solvent oil continuously returns to the methyl isocyanate reactor D1, the methyl isocyanate is taken as a product through a methyl isocyanate discharging pump P1 at 100g/h, the other reacted materials enter the chromatographic recovery section at 18112.1814 h after the reaction, and the content of other materials is analyzed as 98.1814 h.
Claims (10)
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) with be used for connecting the material export of 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 using dimethyl sulfate as set forth in 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.
9. A continuous process for producing methyl isocyanate from dimethyl sulfate, which comprises using the apparatus for producing methyl isocyanate from dimethyl sulfate according to claim 1, wherein: it comprises the following steps:
step one): the solvent oil and the sodium cyanate enter the methyl isocyanate reactor (D1) through the raw material solvent oil feeding line (1) and the sodium cyanate feeding line (2), respectively;
step two): dimethyl sulfate continuously enters the methyl isocyanate reactor (D1) through the dimethyl sulfate feed line (3);
step three): controlling the reaction temperature of the methyl isocyanate reactor (D1) to be between 150 ℃ and 190 ℃;
step four): nitrogen enters the methyl isocyanate reactor (D1) through the nitrogen inlet line (8), the nitrogen compressor (C2), the compressed nitrogen delivery line (9);
step five): the product after the reaction enters the methyl isocyanate condenser (C1) through the product discharging line (4) after the reaction, and the outlet temperature of the methyl isocyanate condenser (C1) is controlled to be less than 35 ℃;
step six): the condensed material enters the gas-liquid separation tank (D2) through the condensed mixture conveying pipeline (5), and the separated nitrogen returns to the methyl isocyanate reactor (D1) for recycling through the gas-liquid separated nitrogen conveying pipeline (7), the nitrogen compressor (C2) and the compressed nitrogen conveying pipeline (9); the separated solvent oil continuously flows back to the methyl isocyanate reactor (D1) through the circulating solvent oil conveying pipeline (6), and the methyl isocyanate after gas-liquid separation is taken as a product through the gas-liquid separated methyl isocyanate conveying pipeline (10), the methyl isocyanate discharging pump (P1) and the methyl isocyanate product output pipeline (11);
step seven): other materials after the reaction are discharged from the discharging pipeline (12) of other reacted materials after the reaction of the methyl isocyanate reactor (D1) to enter a recovery section.
10. The continuous process for producing methyl isocyanate from dimethyl sulfate according to claim 9, wherein: the reaction temperature of the methyl isocyanate reactor (D1) was controlled to be between 170 ℃ and 185 ℃.
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Cited By (1)
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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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