CN111909036A - DMC production system and method - Google Patents
DMC production system and method Download PDFInfo
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- CN111909036A CN111909036A CN202010852070.5A CN202010852070A CN111909036A CN 111909036 A CN111909036 A CN 111909036A CN 202010852070 A CN202010852070 A CN 202010852070A CN 111909036 A CN111909036 A CN 111909036A
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- C07C68/01—Preparation of esters of carbonic or haloformic acids from carbon monoxide and oxygen
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Abstract
A DMC production system includes a synthesis reaction main loop; the synthesis reaction main circulation ring comprises a DMC synthesis reactor, a circulation compressor, a first esterification tower and an ester removal tower; one end of the DMC synthesis reactor is connected with one end of the first esterification tower through the circulating compressor; the other end of the DMC synthesis reactor is connected with the other end of the first esterification tower through the ester removal tower; the DMC production method comprises the main circulation reaction of the synthetic reaction and the esterification parallel bypass reaction. The invention has the advantages that the DMC synthesis carbonylation coupling reaction system adopts the reaction rectification esterification parallel bypass, meets all process parameters of DMC synthesis, ensures higher nitric acid reduction efficiency, effectively reduces the consumption of nitric acid, and ensures lower content of waste liquid nitric acid. Effectively reduces the consumption of methanol, effectively reduces and improves the content of methanol which returns to the gasification component of the DMC synthesis loop, and reduces the content of methanol in discharged waste liquid. Meanwhile, the side reaction in the esterification tower is reduced, the generation amount of nitric acid and nitrous acid is reduced, and the esterification reaction efficiency is improved.
Description
Technical Field
The invention relates to a system and a method for producing DMC by a gas phase carbon-based method.
Background
Dimethyl carbonate (DMC), a chemical raw material with low toxicity, excellent environmental protection performance and wide application, is an important organic synthesis intermediate, contains functional groups such as carbonyl, methyl, methoxy and the like in a molecular structure, has various reaction performances, and has the characteristics of safe and convenient use, less pollution, easy transportation and the like in production. Because the toxicity of the dimethyl carbonate is low, the dimethyl carbonate is a green chemical product with development prospect.
The current well-established process for the direct synthesis of DMC is the methanol carbonylation coupling. Wherein the procedure of the vinylester supplementation is currently in progress. The adopted stirring reaction kettle has the defects of high power consumption, low nitric acid reduction efficiency, poor safety and stability of mechanical operation equipment and the like. The parallel reaction rectification esterification process is adopted at present, so that the reduction efficiency of nitric acid can be ensured to be higher while various process parameters of DMC synthesis are met, the consumption of nitric acid is effectively reduced, and the content of waste liquid nitric acid is ensured to be lower. Effectively reduces the consumption of methanol, effectively reduces and improves the content of the gasification component methanol returned to the DMC synthesis loop, and reduces the content of the methanol in the discharged waste liquid. The reaction control means for reducing the nitric acid is added, the device is more stable in operation and higher in safety. Meanwhile, the side reaction nitrogen oxides and the aquatic side reaction in the esterification tower are reduced, the generation amount of nitric acid and nitrous acid is reduced, and the esterification reaction efficiency is improved.
Disclosure of Invention
The invention relates to a production system and a production method for producing DMC by a gas phase carbon-based method. The DMC synthesis carbonylation coupling reaction system adopts a reaction rectification esterification parallel bypass, meets all process parameters of DMC synthesis, can ensure higher nitric acid reduction efficiency, effectively reduces the consumption of nitric acid, and ensures lower content of waste liquid nitric acid. Effectively reduces the consumption of methanol, effectively reduces and improves the content of the gasification component methanol returned to the DMC synthesis loop, and reduces the content of the methanol in the discharged waste liquid. The reaction control means for reducing the nitric acid is added, the device is more stable in operation and higher in safety. Meanwhile, the side reaction nitrogen oxides and the aquatic side reaction in the esterification tower are reduced, the generation amount of nitric acid and nitrous acid is reduced, and the esterification reaction efficiency is improved.
The technical scheme for realizing the purpose of the invention is that a DMC production system comprises a synthesis reaction main circulation ring;
the synthesis reaction main circulation ring comprises a DMC synthesis reactor, a circulation compressor, a first esterification tower and an ester removal tower;
one end of the DMC synthesis reactor is connected with one end of the first esterification tower through the circulating compressor;
the other end of the DMC synthesis reactor is connected with the other end of the first esterification tower through the ester removal tower.
Preferably, the DMC production system further comprises an esterification parallel bypass;
the esterification parallel bypass comprises a second esterification tower and a booster;
the lower end of the second esterification tower is connected with the ester removal tower through a booster;
the first esterification tower is connected with the second esterification tower.
Preferably, the DMC production system further comprises an esterification parallel bypass; the esterification parallel bypass comprises an overhead condenser, a second esterification tower and a supercharger, wherein the upper end of the second esterification tower is provided with a rectifying part, and gas in the second esterification tower is discharged out of the second esterification tower through the rectifying part;
the lower end of the second esterification tower is connected with the ester removal tower through a booster;
the rectifying component at the upper end of the second esterification tower is connected with the first esterification tower through a tower top condenser;
the first esterification tower is connected with the second esterification tower.
Further, the overhead condenser is connected to the second esterification column via a return line.
Furthermore, a return fluid tank is arranged on the return pipe.
Further, the second esterification tower is supplemented with one or more of water and/or methanol and/or nitric acid and/or nitrous acid through a pipeline.
A DMC production method comprises the main cycle reaction of the synthesis reaction, wherein gas in a first esterification tower 3 enters a DMC synthesis reactor through a cycle compressor, and a DMC product is obtained after ester removal tower pressurization, reaction and separation;
the esterification is carried out in parallel with the bypass reaction, and the gas discharged by the ester removal tower comprises nitrogen, CO, methanol, MN and NOX、CO2The gas is pressurized by a booster and then enters a second esterification tower, the liquid in the first esterification tower enters the second esterification tower, the gas reacts with the liquid mixture of nitric acid and/or methanol and/or water and/or nitrous acid in the second esterification tower to produce ester materials and generate heat, the gaseous ester materials, the methanol and the water enter a rectifying part of the second esterification tower, the water is separated after the gaseous ester materials, the methanol and the ester materials enter the first esterification tower together with the synthesis gas after the gaseous ester materials, the methanol and the water enter the rectifying part of the second esterification tower.
A DMC production method comprises a main cycle reaction of synthetic reaction and a parallel bypass reaction of esterification;
the synthesis reaction is mainly carried out in a circulating reaction mode, gas in a first esterification tower enters a DMC synthesis reactor through a circulating compressor, and a DMC product is obtained after ester removal tower pressurization, reaction and separation;
the esterification is carried out in parallel with the bypass reaction, and the gas discharged by the ester removal tower comprises nitrogen, CO, methanol, MN and NOX、CO2The gas enters a second esterification tower after being pressurized by a booster, the liquid in the first esterification tower enters the second esterification tower, the gas reacts with the liquid mixture of nitric acid and/or methanol and/or water and/or nitrous acid in the second esterification tower to produce ester materials and generate heat, and the gaseous ester materials, the methanol and the water enter the second esterification tower to react and then enter the first esterification tower together.
Further, the temperature of each reaction chamber of the second esterification tower 6 is controlled to be 50-100 ℃.
Further, the condensing reflux temperature of the overhead condenser 5 is controlled to be 40-80 ℃.
The invention has the following beneficial effects:
1. the invention adopts the working principle that: the esterification process is applied to the production of DMC by a gas phase carbon-based method, which can ensure that the DMC synthesis reaction does not make great process adjustment and meet the production requirement of DMC.
2. The process comprises the following steps: the method can ensure that the reduction efficiency of the nitric acid is higher, effectively reduce the consumption of the nitric acid and the consumption of the nitric acid, the concentration of the nitric acid discharged by the reaction kettle is 2% -5%, the concentration of the nitric acid discharged by the second esterification tower in the patent is 0.15% -0.5%, and ensure that the content of the waste liquid nitric acid is lower, and in addition, the reaction tower is adopted to replace the reaction kettle, the reaction tower does not need to be stirred, and the reaction process is not influenced by the stirring speed.
3. The process comprises the following steps: effectively reduces the consumption of methanol, effectively reduces and improves the content of the gasification component methanol returned to the DMC synthesis loop, and reduces the content of the methanol in the discharged waste liquid.
4. The process comprises the following steps: the reaction control means for reducing the nitric acid is added, the device is more stable in operation and higher in safety.
5. The rectification component is arranged at the upper end of the second esterification tower, the second esterification tower and the upper rectification component thereof are matched with the tower top condenser to form a rectification reaction system, and the reaction temperature in the second esterification tower is effectively controlled, so that the fluctuation of the reaction temperature in the second esterification tower is small.
6. The tower top condenser effectively controls the water content of the gas entering the first esterification tower, and the water content of the gas is reduced, so that the side reaction of generating nitrous acid from the gas in the first esterification tower is inhibited, and the main reaction efficiency of generating MN is higher.
Drawings
The invention is further described with reference to the following figures and implementations.
FIG. 1 is a schematic view of the present invention.
FIG. 2 is a preferred schematic of the present invention.
As shown in the figure, the DMC synthesis reactor 1, a recycle compressor 2, a first esterification column 3, a reflux drum tank 4, an overhead condenser 5, a second esterification column 6, an ester stripping column 7, and a booster 8.
The specific implementation mode is as follows:
as shown in fig. 1, a DMC production system includes a synthesis reaction main loop; the synthesis reaction main circulation ring comprises a DMC synthesis reactor 1, a circulation compressor 2, a first esterification tower 3 and an ester removal tower 7;
one end of the DMC synthesis reactor 1 is connected with one end of the first esterification tower 3 through the circulating compressor 2; the other end of the DMC synthesis reactor 1 is connected with the other end of the first esterification tower 3 through the ester removing tower 7.
Preferably, the DMC production system further comprises an esterification parallel bypass; the esterification parallel bypass comprises a second esterification tower 6 and a booster 8; the lower end of the second esterification tower 6 is connected with the ester removal tower 7 through a booster 8; the supercharger 8 adopts a centrifugal compressor or a centrifugal high-speed fan; preferably, the second esterification column 6 is divided into 1 to N sections, and heating steam coils are arranged in each section. The gas after being pressurized by the booster 8 is divided into 1-N strands to enter the second esterification tower 6,
the first esterification tower 3 is connected with the second esterification tower 6.
The working principle is as follows: the gas pressurized by the booster 8 is divided into 1-N streams and enters the second esterification tower 6. The first esterification tower 3 is connected with the second esterification tower 6 by adopting a pipeline, and the liquid in the first esterification tower 3 enters the second esterification tower 6. The second esterification column 6 is supplemented with a reaction material such as water and/or methanol and/or nitric acid and/or nitrous acid through a pipe. The gas which is divided into 1-N sections to react by the second esterification tower 6 is converged and enters the bottom of the second esterification tower 6. The temperature of each reaction chamber of the second esterification tower 6 is controlled between 50 and 100 ℃, and the second esterification tower 6 generates nitric acid, nitrous acid and methanol to generate methyl nitrite (MN), the generated gas enters a first esterification tower 3 and is subjected to main reaction in the first esterification tower 3 to generate MN, and the obtained synthetic gas contains (nitrogen, CO, methanol, MN and NO)XAnd CO) is pressurized, reacted and separated by a circulating compressor 2, a DMC synthesis reactor 1 and an ester removing tower 7 to obtain a DMC product.
As shown in fig. 2, a DMC production system includes a synthesis reaction main circulation loop; the synthesis reaction main circulation ring comprises a DMC synthesis reactor 1, a circulation compressor 2, a first esterification tower 3 and an ester removal tower 7;
one end of the DMC synthesis reactor 1 is connected with one end of the first esterification tower 3 through the circulating compressor 2; the other end of the DMC synthesis reactor 1 is connected with the other end of the first esterification tower 3 through the ester removing tower 7.
Preferably, the DMC production system further comprises an esterification parallel bypass; the esterification parallel bypass comprises an overhead condenser 5, a second esterification tower 6 and a supercharger 8, wherein a rectifying part (the rectifying part is a section of packing filled at the upper end of the second esterification tower 6, and the packing can be regular packing or flash packing) is arranged at the upper end of the second esterification tower 6, and gas in the second esterification tower 6 is discharged out of the second esterification tower 6 through the rectifying part;
the lower end of the second esterification tower 6 is connected with the ester removal tower 7 through a booster 8;
the rectifying component at the upper end of the second esterification tower 6 is connected with the first esterification tower 3 through a tower top condenser 5;
the first esterification tower 3 is connected with the second esterification tower 6, and the second esterification tower 6 adopts a tower type to perform nitric acid reduction to generate MN reaction.
Preferably, the overhead condenser 5 is connected with the second esterification column 6 through a return pipe, and the overhead condenser 5, the rectification part at the upper end of the overhead condenser and the second esterification column 6 together form a rectification reaction system.
Preferably, the return pipe is provided with a return liquid tank 4, and the return liquid tank 4 is arranged to effectively control the liquid flow.
Preferably, the second esterification column 6 is divided into 1 to N sections, and heating steam coils are arranged in each section. The gas pressurized by the booster 8 is divided into 1-N streams and enters the second esterification tower 6.
Preferably, said overhead condenser 5 is connected to said second esterification column 6 via a return line.
Preferably, a return liquid tank 4 is arranged on the return pipe,
preferably, the second esterification tower 6 is supplemented with one or more of water and/or methanol and/or nitric acid and/or nitrous acid through a pipeline.
The working principle is as follows: the gas pressurized by the booster 8 is divided into 1-N streams and enters the second esterification tower 6. The first esterification tower 3 is connected with the second esterification tower 6 by adopting a pipeline, and the liquid in the first esterification tower 3 enters the second esterification tower 6. The second esterification column 6 is supplemented with a reaction material such as water and/or methanol and/or nitric acid and/or nitrous acid through a pipe. The second esterification column 6 is provided with a rectification section. The reflux liquid tank 4, the tower top condenser 5, the second esterification tower 6 and the rectifying part at the upper end of the second esterification tower form a rectifying reaction system together. The gas which is divided into 1-N sections to react by the second esterification tower 6 is converged and enters the bottom of the second esterification tower 6. The temperature of each reaction chamber of the second esterification tower 6 is controlled to be 50-100 ℃, and the condensation reflux temperature of the overhead condenser 5 is controlled to be 40-80 ℃. Part of the gas passes through a booster 8, a second esterification tower 6, a rectification part at the upper end of the second esterification tower and a tower top condenser 5 and is connected through a pipeline to form circulating gas after esterification parallel bypass reaction and returns to the first esterification tower 3. The temperature of the second esterification tower 6 can be controlled by a steam coil in the second esterification tower 6 and an overhead condenser 5. And (3) returning the circulating gas after the esterification parallel bypass reaction to a main circulating ring, pressurizing, reacting and separating by a circulating compressor 2, a DMC synthesis reactor 1 and an ester removing tower 7 to obtain a DMC product.
A DMC production method comprises the main cycle reaction of the synthesis reaction, wherein gas in a first esterification tower 3 enters a DMC synthesis reactor 1 through a cycle compressor 2, and is pressurized, reacted and separated in an ester removal tower 7 to obtain a DMC product;
the esterification is carried out in parallel by-pass reaction, and the gas discharged from the ester removing tower 7 comprises nitrogen, CO, methanol, MN and NOX、CO2One or more groups of the gas passes through a booster8, pressurizing, then feeding the mixture into a second esterification tower 6, feeding tower liquid (tower liquid comprises any one or a combination of methanol, water, nitric acid and nitrous acid) of a first esterification tower 3 into the second esterification tower 6, reacting the mixture with a nitric acid and/or methanol and/or water and/or nitrous acid liquid mixture in the second esterification tower 6 to produce ester materials and generate heat, feeding the synthesized gaseous ester materials, methanol and water into a rectification part of the second esterification tower 6, separating water after the mixture passes through the rectification part, and feeding the methanol, the ester materials and the synthesis gas into the first esterification tower 3.
A DMC production process, characterized in that: the method comprises a main cycle reaction of synthesis reaction and an esterification parallel bypass reaction;
the synthesis reaction is mainly carried out in a circulating reaction, gas in a first esterification tower 3 enters a DMC synthesis reactor 1 and an ester removal tower 7 through a circulating compressor 2, and a DMC product is obtained after pressurization, reaction and separation;
the esterification is carried out in parallel by-pass reaction, and the gas discharged from the ester removing tower 7 comprises nitrogen, CO, methanol, MN and NOX、CO2The gas is pressurized by a booster 8 and then enters a second esterification tower 6, the liquid in the first esterification tower 3 enters the second esterification tower 6, the gas reacts with the nitric acid and/or methanol and/or water and/or nitrous acid liquid mixture in the second esterification tower 6 to produce ester materials and generate heat, and the gaseous ester materials, the methanol and the water enter the second esterification tower 6 to react and then enter the first esterification tower 3.
Compared with other esterification processes, the method can ensure the DMC synthesis process, and has the advantages of higher safety and stability and higher utilization efficiency of raw materials.
Claims (10)
1. A DMC production system, comprising: the DMC production system comprises a synthesis reaction main circulation ring;
the synthesis reaction main circulation ring comprises a DMC synthesis reactor (1), a circulation compressor (2), a first esterification tower (3) and an ester removal tower (7);
one end of the DMC synthesis reactor (1) is connected with one end of the first esterification tower (3) through the circulating compressor (2);
the other end of the DMC synthesis reactor (1) is connected with the other end of the first esterification tower (3) through the ester removal tower (7).
2. A DMC production system as recited in claim 1 wherein: the DMC production system further comprises an esterification parallel bypass;
the esterification parallel bypass comprises a second esterification tower (6) and a booster (8);
the lower end of the second esterification tower (6) is connected with the ester removal tower (7) through a booster (8);
the first esterification tower (3) is connected with the second esterification tower (6).
3. A DMC production system as recited in claim 1 wherein: the DMC production system further comprises an esterification parallel bypass;
the esterification parallel bypass comprises an overhead condenser (5), a second esterification tower (6) and a supercharger (8), a rectification part is arranged at the upper end of the second esterification tower (6), and gas in the second esterification tower (6) is discharged out of the second esterification tower (6) through the rectification part;
the lower end of the second esterification tower (6) is connected with the ester removal tower (7) through a booster (8);
the upper end rectifying part of the second esterification tower (6) is connected with the first esterification tower (3) through a tower top condenser (5);
the first esterification tower 3 is connected with the second esterification tower 6.
4. A DMC production system according to claim 3, wherein: the overhead condenser (5) is connected with the second esterification tower (6) through a return pipe.
5. DMC production system according to claim 4, wherein: and a return fluid tank (4) is arranged on the return pipe.
6. A DMC production system according to claim 2 or 3, wherein: and the second esterification tower (6) is supplemented with one or more of water and/or methanol and/or nitric acid and/or nitrous acid through a pipeline.
7. A DMC production process, characterized in that: the method comprises a main cycle reaction of synthesis reaction and an esterification parallel bypass reaction;
the synthesis reaction is mainly carried out in a circulating reaction, gas in a first esterification tower (3) enters a DMC synthesis reactor (1) and an ester removal tower (7) through a circulating compressor (2) to be pressurized, reacted and separated to obtain a DMC product;
the esterification is carried out in parallel by-pass reaction, and the gas discharged by the ester removal tower (7) comprises nitrogen, CO, methanol, MN and NOX、CO2The gas is pressurized by a booster (8) and then enters a second esterification tower (6), the liquid in the first esterification tower (3) enters the second esterification tower (6), the gas is mixed with externally supplemented nitric acid and/or methanol and/or water and/or nitrous acid liquid in the second esterification tower (6), and the mixed liquid and the gas discharged by an ester removal tower (7) comprise nitrogen, CO, methanol, MN and NOX、CO2One or more of the components are combined to react to produce ester substances and generate heat, the mixed gas of gaseous ester substances, methanol, water and CO enters a rectifying part of a second esterification tower (6), water is separated after the mixed gas passes through the rectifying part, and the methanol and the ester substances enter a first esterification tower (3) together.
8. A DMC production process, characterized in that: the method comprises a main cycle reaction of synthesis reaction and an esterification parallel bypass reaction;
the synthesis reaction is mainly carried out in a circulating reaction, gas in a first esterification tower (3) enters a DMC synthesis reactor (1) and an ester removal tower (7) through a circulating compressor (2) to be pressurized, reacted and separated to obtain a DMC product;
the esterification is carried out in parallel by-pass reaction, and the gas discharged by the ester removal tower (7) comprises nitrogen, CO, methanol, MN and NOX、CO2One or more combinations of gas throughThe booster (8) is pressurized and then enters the second esterification tower (6), the tower liquid of the first esterification tower (3) enters the second esterification tower (6), the mixture reacts with externally supplemented nitric acid and/or methanol and/or water and/or nitrous acid liquid mixture in the second esterification tower (6) to produce ester materials and generate heat, and the methanol, the water and the ester materials generated by the reaction enter the second esterification tower (6) and enter the first esterification tower (3).
9. A DMC production process according to claim 7 or 8, characterized in that: the temperature of each reaction chamber of the second esterification tower (6) is controlled to be 50-100 ℃.
10. A DMC production process according to claim 7, characterized in that: the condensing reflux temperature of the tower top condenser (5) is controlled to be 40-80 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114507136A (en) * | 2022-04-13 | 2022-05-17 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507136A (en) * | 2022-04-13 | 2022-05-17 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
| CN114507136B (en) * | 2022-04-13 | 2022-06-21 | 太原理工大学 | Efficient synthesis method of lithium ion battery electrolyte mixed solvent |
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