CN111454179B - Device and continuous process for producing methyl isocyanate from dimethyl sulfate - Google Patents
Device and continuous process for producing methyl isocyanate from dimethyl sulfate Download PDFInfo
- Publication number
- CN111454179B CN111454179B CN202010382901.7A CN202010382901A CN111454179B CN 111454179 B CN111454179 B CN 111454179B CN 202010382901 A CN202010382901 A CN 202010382901A CN 111454179 B CN111454179 B CN 111454179B
- Authority
- CN
- China
- Prior art keywords
- methyl isocyanate
- reactor
- pipeline
- dimethyl sulfate
- gas
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C263/00—Preparation of derivatives of isocyanic acid
- C07C263/18—Separation; Purification; Stabilisation; Use of additives
- C07C263/20—Separation; Purification
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of fine chemical synthesis, and particularly relates to a device and a continuous process for producing methyl isocyanate from 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 gas-liquid separation tank is connected with a mixture conveying pipeline after condensation; the gas-liquid separation tank is connected with a methyl isocyanate reactor through a circulating solvent oil conveying pipeline, a nitrogen compressor is connected with a nitrogen conveying pipeline 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 methyl isocyanate conveying pipeline after gas-liquid separation; the invention can realize continuous production of methyl isocyanate by using dimethyl sulfate, and has the advantages of 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 from dimethyl sulfate and a continuous process.
Background
Methyl isocyanate is one of the most important species in monoalkyl isocyanates, and is widely used in a variety of fields such as polymer industry, plastic industry, pharmaceutical industry, pesticide industry, etc., and is synthesized into polyisocyanates, polyurethanes, polyureas, and high levelsMonomers of the polymeric binder; in the pesticide industry it is a major intermediate for the manufacture of carbamate pesticides like carbaryl, aldicarb, furadan, herbicides like captan, avenanthramide and the like; methyl isocyanateThe molecular structure of (C) has one carbon atom connected with two double bonds, which makes it have the characteristics similar to ketene structure, has strong additivity, can perform addition reaction with various active hydrogen-containing compounds, such as phenols, oximes, amines, acids, alcohols, nitrogen-containing heterocycle and other organic compounds, and is also the reason for extremely wide application of methyl isocyanate.
The synthesizing process of methyl isocyanate has a plurality of routes, and the methylcarbamoyl chloride thermal decomposition method is a route which is used for years in the industrialized mass production abroad, and has the advantages that the technology is mature, the product yield and quality reach better levels, and the production scale is economical 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 used in recent years, wherein the route for synthesizing methyl isocyanate from dimethyl sulfate is most common, and the reaction equation is as follows:
methyl isocyanate is inflammable and dramatic toxic liquid, and at present, the intermittent production process for synthesizing methyl isocyanate from dimethyl sulfate in China is adopted, so that a reaction kettle is required to be frequently and manually opened for feeding, and extremely toxic gases such as 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 from dimethyl sulfate, which can realize continuous operation, simple flow, less equipment investment and high reaction rate.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, and provides a device and a continuous process for producing methyl isocyanate from dimethyl sulfate, which have reasonable design, can realize continuous operation, simple flow, less equipment investment, high reaction rate and high yield.
The purpose of the invention is realized in the following way: the device for producing methyl isocyanate by using 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 nitrogen conveying pipeline of the gas-liquid separation tank after gas-liquid separation is connected with a nitrogen compressor, 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 methyl isocyanate conveying pipeline after gas-liquid separation, and an outlet of the methyl isocyanate discharging pump is connected with a methyl isocyanate product output pipeline.
The outside of the methyl isocyanate reactor is provided with a jacket capable of controlling the reaction temperature.
The lower part of the methyl isocyanate reactor is provided with a raw material inlet which is respectively used for connecting the raw material solvent oil feeding pipeline, the sodium cyanate feeding pipeline and the dimethyl sulfate feeding pipeline, the bottom of the methyl isocyanate reactor is provided with a nitrogen inlet which is used for connecting the compressed nitrogen conveying pipeline, the top of the methyl isocyanate reactor is provided with a product outlet which is used for connecting the product discharging pipeline after the reaction, and the upper part of the methyl isocyanate reactor is provided with a solvent oil backflow inlet which is used for connecting the circulating solvent oil conveying pipeline and a material outlet which is used for connecting other material discharging pipelines after the reaction.
The bottom of the methyl isocyanate reactor is provided with a gas distributor.
The methyl isocyanate reactor is a multistage loop reactor.
The gas distributor is an aeration head.
And flow regulating valves are arranged on the raw material solvent oil feeding pipeline, the sodium cyanate feeding pipeline and the dimethyl sulfate feeding pipeline.
The methyl isocyanate discharging pump is a positive displacement pump.
The continuous process for producing methyl isocyanate from dimethyl sulfate uses the device for producing methyl isocyanate from dimethyl sulfate, and comprises the following steps:
step one): solvent oil and sodium cyanate respectively enter the methyl isocyanate reactor through the raw material solvent oil feeding pipeline and the sodium cyanate feeding pipeline;
step two): continuously feeding dimethyl sulfate into the methyl isocyanate reactor through the dimethyl sulfate feed line;
step three): controlling the reaction temperature of the methyl isocyanate reactor to be 150-190 ℃;
step four): nitrogen enters the methyl isocyanate reactor through the nitrogen inlet pipeline, the nitrogen compressor and the compressed nitrogen delivery pipeline;
step five): the product after the reaction enters the methyl isocyanate condenser through a product discharge pipeline after the reaction, 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 through the gas-liquid separated nitrogen conveying pipeline, the nitrogen compressor and the compressed nitrogen conveying pipeline for recycling; 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 produced as products through the methyl isocyanate conveying pipeline, the methyl isocyanate discharging pump and the methyl isocyanate product output pipeline after gas-liquid separation;
step seven): and (3) other materials after the reaction are reacted enter a recovery section from the methyl isocyanate reactor through other material discharging pipelines after the reaction.
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, the 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 through a circulating solvent oil conveying pipeline to be recycled, and the separated nitrogen is re-input into the methyl isocyanate reactor through the nitrogen compressor to be recycled, and the separated methyl isocyanate can be taken as a product after passing through the methyl isocyanate discharge pump; in the reaction process, nitrogen is introduced into the methyl isocyanate reactor, so that on one hand, a high-gas content area and a low-gas content area in the reactor generate larger density difference, the materials are pushed to form internal high-speed circulation, the materials are fully mixed and sheared and dissolved, the reaction is effectively promoted, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged at the upper part of the reactor in time, so that side reactions caused by the fact that the methyl isocyanate generated in the original intermittent production process stays in the reaction kettle are avoided, and the yield is improved; the device for producing methyl isocyanate from dimethyl sulfate has reasonable overall design, and the continuous process for producing methyl isocyanate from dimethyl sulfate can realize continuous production of methyl isocyanate by using the device.
Drawings
FIG. 1 is a schematic diagram of an apparatus for producing methyl isocyanate from dimethyl sulfate according to the present invention.
In the figure: d1, methyl isocyanate reactor D2, gas-liquid separation tank C1, methyl isocyanate condenser C2, nitrogen compressor P1, methyl isocyanate discharge pump 1, raw material solvent oil feed line 2, sodium cyanate feed line 3, dimethyl sulfate feed line 4, reaction product discharge line 5, condensed mixture transfer line 6, circulating solvent oil transfer line 7, nitrogen transfer line after gas-liquid separation 8, nitrogen intake line 9, compressed nitrogen transfer line 10, methyl isocyanate transfer line after gas-liquid separation 11, methyl isocyanate product output line 12, and other material discharge lines after reaction.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
Example 1
As shown in fig. 1, the device 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 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 reaction product discharging pipeline 4, and the methyl isocyanate condenser C1 is connected with a gas-liquid separation tank D2 through a condensed mixture conveying pipeline 5; the gas-liquid separation tank D2 is connected with the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6, a nitrogen compressor C2 is connected with a nitrogen inlet pipeline 8 through a nitrogen conveying pipeline 7 after gas-liquid separation of the gas-liquid separation tank D2, 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 an inlet of a methyl isocyanate discharging pump P1 through a methyl isocyanate conveying pipeline 10 after gas-liquid separation, and an outlet of the methyl isocyanate discharging 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, the reacted materials enter the methyl isocyanate condenser C1 to be condensed and then enter the gas-liquid separation tank D2 to be separated, the separated solvent oil enters the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6 to be recycled, and the separated nitrogen is re-input into the methyl isocyanate reactor D1 through the nitrogen compressor C2 to be recycled, and the separated methyl isocyanate can be taken as a product after passing through the methyl isocyanate discharge pump P1; in the reaction process, nitrogen is introduced into the methyl isocyanate reactor D1, so that on one hand, a large density difference is generated between a high-gas content area and a low-gas content area in the reactor, materials are pushed to form internal high-speed circulation, the materials are fully mixed and sheared and dissolved, the reaction is effectively promoted, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged at the upper part of the reactor in time, so that side reactions caused by the fact that the methyl isocyanate generated in the original intermittent production process stays in the reaction kettle are avoided, and the yield is improved; the device for producing methyl isocyanate from dimethyl sulfate has reasonable overall design, can realize continuous production of methyl isocyanate by using dimethyl sulfate, and has the advantages of simple operation flow, less equipment investment, high reaction rate and high yield.
Example 2
As shown in fig. 1, the device 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 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 reaction product discharging pipeline 4, and the methyl isocyanate condenser C1 is connected with a gas-liquid separation tank D2 through a condensed mixture conveying pipeline 5; the gas-liquid separation tank D2 is connected with the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6, a nitrogen compressor C2 is connected with a nitrogen inlet pipeline 8 through a nitrogen conveying pipeline 7 after gas-liquid separation of the gas-liquid separation tank D2, 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 an inlet of a methyl isocyanate discharging pump P1 through a methyl isocyanate conveying pipeline 10 after gas-liquid separation, and an outlet of the methyl isocyanate discharging pump P1 is connected with a methyl isocyanate product output pipeline 11.
In order to achieve better effect, the jacket capable of controlling the reaction temperature is arranged outside the methyl isocyanate reactor D1, and the reaction temperature in the methyl isocyanate reactor D1 can be efficiently and rapidly controlled through the jacket, so that the stability of the reaction is improved.
For better effect, the lower part of methyl isocyanate reactor D1 is provided with the raw materials import that is used for connecting respectively raw materials solvent oil feed line 1 sodium cyanate feed line 2 with dimethyl sulfate feed line 3, the bottom of methyl isocyanate reactor D1 is provided with and is used for connecting compressed nitrogen transfer line 9's nitrogen gas import, the top of methyl isocyanate reactor D1 is provided with and is used for connecting the product export of reaction back product ejection of compact pipeline 4, the upper portion of methyl isocyanate reactor D1 is provided with and is used for connecting the solvent oil backward flow import of circulating solvent oil transfer line 6 and the material export that is used for connecting other material ejection of compact pipelines 12 after the reaction set up each connector on the different positions of methyl isocyanate reactor D1 in order to realize with the connection of outside pipeline, make the overall structure of this device more reasonable, the whole overall layout and the connection of the device of being convenient for.
In order to achieve a better effect, a gas distributor is arranged at the bottom of the methyl isocyanate reactor D1, and nitrogen entering the methyl isocyanate reactor D1 can be effectively controlled through the gas distributor so as to effectively promote the reaction to be carried out and promote the reaction rate.
In order to achieve better effect, the methyl isocyanate reactor D1 is a multi-stage loop reactor, so that the reaction efficiency in the methyl isocyanate reactor D1 is further improved, and the raw material treatment speed is improved, so that the yield is improved.
In order to achieve a better effect, the gas distributor is an aeration head, 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 the sodium cyanate feed line 2 and the dimethyl sulfate feed line 3, be convenient for fast to get into the material in the methyl isocyanate reactor D1 carries out flow control, improves the operability of this device.
In order to achieve a better effect, the methyl isocyanate discharging pump P1 is a positive displacement pump, has a 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, the reacted materials enter the methyl isocyanate condenser C1 to be condensed and then enter the gas-liquid separation tank D2 to be separated, the separated solvent oil enters the methyl isocyanate reactor D1 through a circulating solvent oil conveying pipeline 6 to be recycled, and the separated nitrogen is re-input into the methyl isocyanate reactor D1 through the nitrogen compressor C2 to be recycled, and the separated methyl isocyanate can be taken as a product after passing through the methyl isocyanate discharge pump P1; in the reaction process, nitrogen is introduced into the methyl isocyanate reactor D1, so that on one hand, a large density difference is generated between a high-gas content area and a low-gas content area in the reactor, materials are pushed to form internal high-speed circulation, the materials are fully mixed and sheared and dissolved, the reaction is effectively promoted, and the reaction rate is improved; on the other hand, the produced methyl isocyanate gas phase is discharged at the upper part of the reactor in time, so that side reactions caused by the fact that the methyl isocyanate generated in the original intermittent production process stays in the reaction kettle are avoided, and the yield is improved; the device for producing methyl isocyanate from dimethyl sulfate has reasonable overall design, can realize continuous production of methyl isocyanate by using dimethyl sulfate, and has the advantages of simple operation flow, less equipment investment, high reaction rate and high yield.
Example 3
The continuous process for producing methyl isocyanate from dimethyl sulfate, which uses the device for producing methyl isocyanate from dimethyl sulfate shown in the 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 2000g/h and at 267g/h respectively, dimethyl sulfate enters the methyl isocyanate reactor D1 through a dimethyl sulfate feeding pipeline 3 at 323g/h, and the reaction temperature is controlled at 180 ℃ through a jacket; nitrogen enters the methyl isocyanate reactor D1 through the nitrogen compressor C2 at a speed of 6L/h; the reacted material enters 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 a gas-liquid separation tank D2, and separated nitrogen is returned to the methyl isocyanate reactor D1 through a nitrogen compressor C2 for recycling; the separated solvent oil continuously flows back to the methyl isocyanate reactor D1, and methyl isocyanate is extracted as a product by the methyl isocyanate discharging pump P1 at the speed of 189 g/h; the other materials after the reaction are extracted from the other material discharging pipeline 12 at 2400g/h and enter the recovery section; the content of methyl isocyanate was 99.2% by chromatography.
Example 4
The continuous process for producing methyl isocyanate from dimethyl sulfate, which uses the device for producing methyl isocyanate from dimethyl sulfate shown in the 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 speed of 1600g/h and sodium cyanate at the speed of 142g/h respectively, dimethyl sulfate enters the methyl isocyanate reactor D1 through a dimethyl sulfate feeding pipeline 3 at the speed of 172g/h, and the reaction temperature is controlled at 160 ℃ through a jacket; nitrogen enters the methyl isocyanate reactor D1 through the nitrogen compressor C2 at a speed of 4L/h; the reacted material enters 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 a gas-liquid separation tank D2, and separated nitrogen is returned to the methyl isocyanate reactor D1 through a nitrogen compressor C2 for recycling; the separated solvent oil continuously flows back to the methyl isocyanate reactor D1, and methyl isocyanate is extracted at the speed of 100g/h by the methyl isocyanate discharging pump P1 as a product; the other materials after the reaction are extracted from the other material discharging pipeline 12 at a speed of 1814g/h and enter a recovery section; the content of methyl isocyanate was 98.4% by chromatography.
Claims (8)
1. A continuous process for producing methyl isocyanate from dimethyl sulfate uses a device for producing methyl isocyanate from dimethyl sulfate, and the device 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 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 post-reaction product discharging pipeline (4), and the methyl isocyanate condenser (C1) is connected with a gas-liquid separation tank (D2) through a condensed mixture conveying pipeline (5); 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 nitrogen conveying pipeline (7) after gas-liquid separation, 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 an inlet of a methyl isocyanate discharging pump (P1) through a methyl isocyanate conveying pipeline (10) after gas-liquid separation, and an outlet of the methyl isocyanate discharging pump (P1) is connected with a methyl isocyanate product output pipeline (11);
the lower part of the methyl isocyanate reactor (D1) is provided with a raw material inlet which is respectively used for connecting the raw material solvent oil feeding pipeline (1), the sodium cyanate feeding pipeline (2) and the dimethyl sulfate feeding pipeline (3), the bottom of the methyl isocyanate reactor (D1) is provided with a nitrogen inlet which is used for connecting the compressed nitrogen conveying pipeline (9), the top of the methyl isocyanate reactor (D1) is provided with a product outlet which is used for connecting the reacted product discharging pipeline (4), and the upper part of the methyl isocyanate reactor (D1) is provided with a solvent oil backflow inlet which is used for connecting the circulating solvent oil conveying pipeline (6) and a material outlet which is used for connecting other materials discharging pipelines (12) after the reaction;
the continuous process for producing methyl isocyanate from dimethyl sulfate comprises the following steps:
step one): solvent oil and sodium cyanate enter the methyl isocyanate reactor (D1) through the raw material solvent oil feeding pipeline (1) and the sodium cyanate feeding pipeline (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 150-190 ℃;
step four): nitrogen enters the methyl isocyanate reactor (D1) through the nitrogen inlet line (8), the nitrogen compressor (C2) and the compressed nitrogen delivery line (9);
step five): the product after the reaction enters the methyl isocyanate condenser (C1) through the product discharging pipeline (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) through the gas-liquid separated nitrogen conveying pipeline (7), the nitrogen compressor (C2) and the compressed nitrogen conveying pipeline (9) for recycling; 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 produced as products through the methyl isocyanate conveying pipeline (10), the methyl isocyanate discharging pump (P1) and the methyl isocyanate product output pipeline (11) after gas-liquid separation;
step seven): and the other materials after the reaction are fed into a recovery section from the methyl isocyanate reactor (D1) through a discharging pipeline (12) of the other materials after the reaction.
2. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: the outside of the methyl isocyanate reactor (D1) is provided with a jacket capable of controlling the reaction temperature.
3. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: the bottom of the methyl isocyanate reactor (D1) is provided with a gas distributor.
4. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: the methyl isocyanate reactor (D1) is a multistage loop reactor.
5. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 3, wherein: the gas distributor is an aeration head.
6. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: flow regulating valves are arranged on the raw material solvent oil feeding pipeline (1), the sodium cyanate feeding pipeline (2) and the dimethyl sulfate feeding pipeline (3).
7. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: the methyl isocyanate discharging pump (P1) is a positive displacement pump.
8. A continuous process for producing methyl isocyanate from dimethyl sulfate as claimed in claim 1, wherein: the reaction temperature of the methyl isocyanate reactor (D1) is controlled between 170 ℃ and 185 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010382901.7A CN111454179B (en) | 2020-05-08 | 2020-05-08 | Device and continuous process for producing methyl isocyanate from dimethyl sulfate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010382901.7A CN111454179B (en) | 2020-05-08 | 2020-05-08 | Device and continuous process for producing methyl isocyanate from dimethyl sulfate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN111454179A CN111454179A (en) | 2020-07-28 |
| CN111454179B true CN111454179B (en) | 2023-10-20 |
Family
ID=71675087
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010382901.7A Active CN111454179B (en) | 2020-05-08 | 2020-05-08 | Device and continuous process for producing methyl isocyanate from dimethyl sulfate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111454179B (en) |
Families Citing this family (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 |
Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4206136A (en) * | 1978-06-28 | 1980-06-03 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of methylisocyanate |
| US4495107A (en) * | 1983-03-10 | 1985-01-22 | Fmc Corporation | Process for producing alkali metal cyanates |
| JPH09110862A (en) * | 1995-10-24 | 1997-04-28 | Shimadzu Corp | Upright production apparatus and production of ester cyclic dimer |
| CN101029129A (en) * | 2007-02-12 | 2007-09-05 | 江苏中科金龙化工股份有限公司 | Continuous production of fatty poly-ester carbonate polyhydric alcohol |
| CN101074216A (en) * | 2007-04-23 | 2007-11-21 | 锦化化工集团氯碱股份有限公司 | Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane |
| CN102863382A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工股份有限公司 | Solvent recovery method of caprolactam rearrangement reaction products and application thereof |
| CN104399522A (en) * | 2014-10-21 | 2015-03-11 | 贵州大学 | Catalyst for production of low carbon olefin from methanol through iodination method, and preparation method thereof |
| CN109748822A (en) * | 2017-11-08 | 2019-05-14 | 万华化学（宁波）有限公司 | A kind of method and system preparing isocyanate-monomer |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120108811A1 (en) * | 2010-10-28 | 2012-05-03 | Formosa Laboratories Inc. | Process for preparing temozolomide |
-
2020
- 2020-05-08 CN CN202010382901.7A patent/CN111454179B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4206136A (en) * | 1978-06-28 | 1980-06-03 | Deutsche Gold- Und Silber-Scheideanstalt Vormals Roessler | Process for the production of methylisocyanate |
| US4495107A (en) * | 1983-03-10 | 1985-01-22 | Fmc Corporation | Process for producing alkali metal cyanates |
| JPH09110862A (en) * | 1995-10-24 | 1997-04-28 | Shimadzu Corp | Upright production apparatus and production of ester cyclic dimer |
| CN101029129A (en) * | 2007-02-12 | 2007-09-05 | 江苏中科金龙化工股份有限公司 | Continuous production of fatty poly-ester carbonate polyhydric alcohol |
| CN101074216A (en) * | 2007-04-23 | 2007-11-21 | 锦化化工集团氯碱股份有限公司 | Close-circulating chlorohydrination reactor and reactive method during production of epoxy-propane |
| CN102863382A (en) * | 2011-07-07 | 2013-01-09 | 中国石油化工股份有限公司 | Solvent recovery method of caprolactam rearrangement reaction products and application thereof |
| CN104399522A (en) * | 2014-10-21 | 2015-03-11 | 贵州大学 | Catalyst for production of low carbon olefin from methanol through iodination method, and preparation method thereof |
| CN109748822A (en) * | 2017-11-08 | 2019-05-14 | 万华化学（宁波）有限公司 | A kind of method and system preparing isocyanate-monomer |
Non-Patent Citations (1)
| Title |
|---|
| 异氰酸甲酯的制造方法;颜灿光;《湖南化工》;51-59 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN111454179A (en) | 2020-07-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US3887167A (en) | Apparatus for manufacture of organic isocyanates | |
| EP1575904B1 (en) | Method for the continuous production of isocyanates | |
| EP0322647B1 (en) | Process for the continuous production of mono- or polyisocyanates | |
| US20070299279A1 (en) | Process for the continuous preparation of isocyanates | |
| US20110190534A1 (en) | Method for decomposing and recovering isocyanate compound | |
| CN111454179B (en) | Device and continuous process for producing methyl isocyanate from dimethyl sulfate | |
| US4581174A (en) | Process for the continuous preparation of organic mono-and/or polyisocyanates | |
| EP2480525B1 (en) | Method for producing isocyanates | |
| US20050222453A1 (en) | Method for producing isocyanates | |
| CN111170891A (en) | Method for producing isocyanates by partial adiabatically operated phosgenation of the corresponding amines | |
| CN212403979U (en) | Device for producing methyl isocyanate by dimethyl sulfate | |
| WO2008025659A1 (en) | Method for producing isocyanates | |
| EP3307708B1 (en) | Method for manufacturing diisocyanates in the gaseous phase | |
| US8546606B2 (en) | Method for producing polyisocyanates | |
| CN115093348B (en) | Method for preparing isocyanate by pipeline phosgene method | |
| CZ299615B6 (en) | Continuous adiabatic process for preparing nitrochlorobenzene | |
| CN115043758B (en) | Method for preparing isocyanate by combining supercritical phosgenation method and pipelining method | |
| CN113880730A (en) | Industrial method for continuously preparing hexamethylene diisocyanate | |
| EP3873886B1 (en) | Production of hydroxyethylpiperazine | |
| CN116078293A (en) | Tubular reactor suitable for preparing hexamethylene diisocyanate by gas phase method and application thereof | |
| CN118718891A (en) | Fixed bed continuous flow preparation method of 3-hydroxypyrrolidine | |
| CN118026901A (en) | Method and device for preparing methylthio acetaldehyde oxime by two-step reaction with water as solvent | |
| WO2002074734A1 (en) | Method for the production of urea | |
| CN116354909A (en) | Synthesis method of 3-iminomethyl tetrahydrofuran | |
| EA043124B1 (en) | OBTAINING HYDROXYETHYLPIPERAZINE |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |