CN114534291A - Device and method for producing ethyl methyl carbonate by coupling reaction and rectification of solid catalyst - Google Patents
Device and method for producing ethyl methyl carbonate by coupling reaction and rectification of solid catalyst Download PDFInfo
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- CN114534291A CN114534291A CN202210414055.1A CN202210414055A CN114534291A CN 114534291 A CN114534291 A CN 114534291A CN 202210414055 A CN202210414055 A CN 202210414055A CN 114534291 A CN114534291 A CN 114534291A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
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- C07C68/00—Preparation of esters of carbonic or haloformic acids
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Abstract
The invention provides a device and a method for producing methyl ethyl carbonate by coupling reaction and rectification of a solid catalyst, and relates to the field of methyl ethyl carbonate. The device and the method for producing the methyl ethyl carbonate by the coupling reaction and rectification of the solid catalyst comprise a dimethyl carbonate storage tank, an absolute ethyl alcohol storage tank, a feeding mixer, a raw material mixing tank, a raw material delivery pump and a feeding preheater. The process can improve the ratio of ethyl methyl carbonate to diethyl carbonate to be more than 3:1, simultaneously reserves the flexible switching capacity of homogeneous catalyst sodium methoxide, uses a solid catalyst, improves the reaction conversion rate of dimethyl carbonate and ethanol as raw materials, reduces side reactions, improves the product quality, reduces the generation of solid wastes, reduces the safety and environmental protection problems caused by emission, the safety problems required to be treated when flammable and explosive materials are subjected to slag removal, the environmental protection problems of material odor caused by open slag removal and the occupational health problems of personnel, prolongs the service cycle of equipment, and ensures the safe and stable production of the device.
Description
Technical Field
The invention relates to the technical field of ethyl methyl carbonate production, in particular to a device and a method for producing ethyl methyl carbonate by coupling reaction and rectification of a solid catalyst.
Background
The methyl ethyl carbonate is an organic compound and has wide application value. The molecule has high-activity reactive groups, such as carbonyl, methyl, methoxyl and other functional groups. Can be used as an intermediate of organic synthesis raw materials in industrial production. Meanwhile, the methyl ethyl carbonate has small viscosity, large dielectric constant and strong solubility to lithium salt, so that the energy density and the charge-discharge capacity of the battery can be well improved, the safety performance of the battery is improved, and the service life of the battery is prolonged.
The current industrial production method of methyl ethyl carbonate is to produce methyl ethyl carbonate by the ester exchange reaction of dimethyl carbonate and ethanol, wherein the main reaction is to produce methyl ethyl carbonate and the reaction byproduct is diethyl carbonate. The reaction is usually carried out with a homogeneous catalyst such as alkali metal alkoxide such as sodium methoxide. Homogeneous catalysts have the advantage of being flexible in switching, but have the problems of: the homogeneous catalyst has poor selectivity relative to methyl ethyl carbonate, and the by-product diethyl carbonate is more; sodium methoxide meets water and hydrolyzes to generate sodium hydroxide, sodium hydroxide reacts with trace carbon dioxide in raw materials to generate sodium carbonate or sodium bicarbonate, and the tower tray and the reboiler of the reaction rectifying tower are easy to be blocked due to long-time operation, so that the pressure difference of the reaction rectifying tower fluctuates, and the normal and stable production of the device is influenced. The catalyst cannot be separated from the product in time to cause deep reaction, and side reactions are increased; after the homogeneous catalyst reaction is finished, the solid waste and dust are generated through separation, and the problems of safety and environmental protection exist in the separation process.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a device and a method for producing ethyl methyl carbonate by coupling reaction and rectification of a solid catalyst, which solve the existing problems.
In order to achieve the purpose, the invention is realized by the following technical scheme: a device for producing methyl ethyl carbonate by coupling reaction and rectification of a solid catalyst comprises a dimethyl carbonate storage tank, an anhydrous ethanol storage tank, a feeding mixer, a raw material mixing tank, a raw material delivery pump, a feeding preheater, a fixed bed pre-reactor, a reaction rectifying tower, a circulating water cooler, a reflux tank, a tower kettle reboiler, a plate-and-frame filter press, a filtrate tank, a crude diethyl carbonate separating tower and a crude methyl ethyl carbonate separating tower, wherein the dimethyl carbonate storage tank and the anhydrous ethanol storage tank are both connected with the feeding mixer through pumps, the output end of the feeding mixer is connected with the raw material mixing tank through a pipeline, the output end of the raw material mixing tank is connected with the feeding preheater through the raw material delivery pump, the feeding preheater is connected with the fixed bed pre-reactor through a pipeline, the output end of the fixed bed pre-reactor is connected with the top of the reaction rectifying tower through a pipeline, the gas phase at the top of the reaction rectifying tower is connected with a circulating water cooler through a pipeline, the reaction rectification tower's tower cauldron passes through the pipeline and links to each other with the plate and frame filter press, the output of plate and frame filter press passes through the pipeline and links to each other with the filtrating jar, the reaction rectification tower passes through the pipeline and links to each other with the tower cauldron reboiler, the output of tower cauldron reboiler passes through the pipeline and links to each other with the bottom of reaction rectification tower, the filtrating jar passes through the pipeline and links to each other with thick diethyl carbonate knockout tower, the output of thick diethyl carbonate knockout tower passes through the pipeline and links to each other with thick ethyl methyl carbonate knockout tower, the top of the tower of thick ethyl methyl carbonate knockout tower passes through the pipeline and links to each other with the feed mixer.
Preferably, the feed mixer is provided with three inlets, and the three inlets are respectively connected with the dimethyl carbonate storage tank, the absolute ethyl alcohol storage tank and the crude ethyl methyl carbonate separation tower.
Preferably, the feed preheater is a shell-and-tube heat exchanger in countercurrent contact, and a jacket heat retainer is arranged in the fixed bed prereactor.
Preferably, the reactive distillation column consists of two sections of CY700 wire mesh corrugated packing and 25 layers of trays.
Preferably, the output end of the circulating water cooler is connected with a reflux tank, and the output end of the reflux tank is connected with the top of the reaction rectifying tower.
Preferably, the method for producing the methyl ethyl carbonate by the coupling reaction and rectification of the solid catalyst is characterized by comprising the following steps: the method comprises the following steps:
s1, firstly, conveying raw materials of ethanol and dimethyl carbonate into a feeding mixer through a raw material conveying pump and a pipeline, preheating the raw materials to a reaction temperature of 85 ℃ through a feeding preheater, conveying the raw materials into a fixed bed prereactor, carrying out a first-stage reaction balance through the prereaction, wherein 50% of dimethyl carbonate and ethanol are consumed in the reaction, feeding the reacted materials into a reaction rectifying tower, carrying out reaction rectification under the catalysis of homogeneous sodium methoxide, extracting a side reaction product of methanol from the top of the reaction rectifying tower, extracting ethyl methyl carbonate, diethyl carbonate and excessive dimethyl carbonate which is not reacted in the tower kettle, and if the tower kettle contains trace amount of ethanol which is not reacted completely, recycling the ethanol along with the top of a crude ethyl methyl carbonate separating tower for reuse;
s2, feeding tower bottom materials in the reaction rectifying tower into a crude diethyl carbonate separating tower, obtaining crude diethyl carbonate with the purity of 99.8% at the tower bottom, extracting ethyl methyl carbonate and unreacted dimethyl carbonate from the tower top, and feeding tower top products into the crude ethyl methyl carbonate separating tower;
and (3) further rectifying and refining the two crude products produced in the steps of S3, S1 and S2 to produce electronic grade ethyl methyl carbonate and diethyl carbonate, and repeating the steps until the dimethyl carbonate and the ethanol are sufficiently deeply reacted and discharged.
The invention provides a device and a method for producing methyl ethyl carbonate by coupling reaction and rectification of a solid catalyst. The method has the following beneficial effects:
the invention fully researches the bed pre-reactor, the reaction rectifying tower and the fixed bed pre-reactor reaction and researches one by one on the basis of the reaction mechanism, couples the fixed bed reaction and the reaction rectification, realizes the step-by-step deep reaction of raw materials of dimethyl carbonate and ethanol, utilizes the high selectivity of a solid catalyst to methyl ethyl carbonate, can improve the proportion of the methyl ethyl carbonate and the diethyl carbonate to be more than 3:1, simultaneously reserves the flexible switching capacity of homogeneous catalyst sodium methoxide, improves the reaction conversion rate of the raw materials of the dimethyl carbonate and the ethanol by using the solid catalyst, reduces side reactions, improves the product quality, reduces the generation of solid wastes, reduces the safety and environmental protection problems caused by discharge, the safety problem needing to be treated when inflammable and explosive materials are cleared, the environmental protection problem of material peculiar smell caused by opening clearing and the occupational health problem of personnel, meanwhile, the service cycle of the equipment is prolonged, and the safe and stable production of the device is ensured.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Wherein, 1, a dimethyl carbonate storage tank; 2. an absolute ethyl alcohol storage tank; 3. a feed mixer; 4. a raw material mixing tank; 5. a raw material delivery pump; 6. a feed preheater; 7. a fixed bed pre-reactor; 8. a reactive distillation column; 9. a circulating water cooler; 10. a reflux tank; 11. a tower kettle reboiler; 12. a plate-and-frame filter press; 13. a filtrate tank; 14. a crude diethyl carbonate separation column; 15. crude methyl ethyl carbonate separating tower.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example (b):
as shown in fig. 1, an embodiment of the present invention provides an apparatus for producing ethyl methyl carbonate by solid catalyst coupling reaction rectification, including a dimethyl carbonate storage tank 1, an anhydrous ethanol storage tank 2, a feed mixer 3, a raw material mixing tank 4, a raw material transfer pump 5, a feed preheater 6, a fixed bed pre-reactor 7, a reaction rectification tower 8, a circulating water cooler 9, a reflux tank 10, a column bottom reboiler 11, a plate-and-frame filter press 12, a filtrate tank 13, a crude diethyl carbonate separation tower 14, and a crude ethyl methyl carbonate separation tower 15, where the dimethyl carbonate storage tank 1 and the anhydrous ethanol storage tank 2 are both connected to the feed mixer 3 through a pump, an output end of the feed mixer 3 is connected to the raw material mixing tank 4 through a pipeline, an output end of the raw material mixing tank 4 is connected to the feed preheater 6 through the raw material transfer pump 5, the feed preheater 6 is connected to the fixed bed pre-reactor 7 through a pipeline, an output end of the fixed bed pre-reactor 7 is connected to a top of the reaction rectification tower 8 through a pipeline, the gas phase at the top of the reaction rectifying tower 8 is connected with a circulating water cooler 9 through a pipeline, the tower kettle of the reaction rectifying tower 8 is connected with a plate-and-frame filter press 12 through a pipeline, carbonate can be filter-pressed and filtered through the plate-and-frame filter press 12, the output end of the plate-and-frame filter press 12 is connected with a filtrate tank 13 through a pipeline, the reaction rectifying tower 8 is connected with a tower kettle reboiler 11 through a pipeline, the output end of the tower kettle reboiler 11 is connected with the bottom of the reaction rectifying tower 8 through a pipeline, the filtrate tank 13 is connected with a crude diethyl carbonate separating tower 14 through a pipeline, the output end of the crude diethyl carbonate separating tower 14 is connected with a crude methyl ethyl carbonate separating tower 15 through a pipeline, and the top of the crude methyl ethyl carbonate separating tower 15 is connected with a feed mixer 3 through a pipeline.
The feed mixer 3 is provided with three inlets which are respectively connected with a dimethyl carbonate storage tank 1, an absolute ethyl alcohol storage tank 2 and a crude ethyl methyl carbonate separation tower 15.
The feed preheater 6 is a shell-and-tube heat exchanger in countercurrent contact, the hot material flow of the shell-and-tube heat exchanger is from the heat transfer oil of the public works, the inlet temperature of the heat transfer oil is 230 ℃, and the outlet temperature is 200 ℃. The cold material flow is from a raw material mixing tank 4, the raw material is preheated to the reaction temperature of 80-90 ℃, a jacket heat retainer is arranged inside a fixed bed pre-reactor 7, 0.4Mpa and 143 ℃ low-pressure saturated steam are introduced into the jacket heat retainer, the diameter of the fixed bed pre-reactor 7 is 1600mm, a section of catalyst bed layer is arranged and filled with a solid catalyst, a feeding distributor and a packing pressing ring are arranged on the upper part of the catalyst bed layer, ceramic balls of phi 3, phi 6 and phi 10 are sequentially filled for protection, after the fixed bed and the reactor 7 react to be balanced, the outlet material is conveyed to a feeding mixer of a reaction rectifying tower 8 through a pipeline to be mixed with a homogeneous sodium methoxide catalyst conveyed by the pipeline and then enters a first layer tower tray of the reaction rectifying tower 8, and the product is obtained after the reaction rectifying and the further reaction.
The reactive distillation column 8 consists of two sections of CY700 wire mesh corrugated packing and 25 layers of trays, and the reactive distillation process is completed in the 25 layers of trays.
The output end of the circulating water cooler 9 is connected with the reflux tank 10, and the output end of the reflux tank 10 is connected with the top of the reactive distillation tower 8.
The method for producing the methyl ethyl carbonate by the coupling reaction and rectification of the solid catalyst is characterized by comprising the following steps: the method comprises the following steps:
s1, firstly, conveying raw materials of ethanol and dimethyl carbonate into a feeding mixer 3 through a raw material conveying pump and a pipeline, preheating the raw materials to a reaction temperature of 85 ℃ through a feeding preheater 6, conveying the raw materials into a fixed bed prereactor 7, achieving first-stage reaction balance through prereaction, and consuming 50% of dimethyl carbonate and ethanol through reaction, conveying the materials after reaction into a reaction rectifying tower 8, carrying out reaction rectification under the catalysis of homogeneous sodium methoxide, extracting a side reaction product of methanol from the top of the reaction rectifying tower 8, extracting methyl ethyl carbonate, diethyl carbonate and excessive dimethyl carbonate which is not reacted in the tower kettle, and recycling the ethanol which is not reacted completely along with the top of a crude methyl ethyl carbonate separating tower 15 if the tower kettle contains trace ethanol;
s2, feeding tower bottom materials in the reaction rectifying tower 8 into a crude diethyl carbonate separating tower 14, obtaining crude diethyl carbonate with the purity of 99.8% at the tower bottom, extracting ethyl methyl carbonate and unreacted dimethyl carbonate from the tower top, and feeding tower top products into a crude ethyl methyl carbonate separating tower 15;
and (3) further rectifying and refining the two crude products produced in the steps S3, S1 and S2 to produce electronic grade ethyl methyl carbonate and diethyl carbonate, and repeating the steps until the dimethyl carbonate and the ethanol are fully and deeply reacted and discharged.
The fixed bed pre-reactor 7 and the reaction rectifying tower 8 are coupled by fully researching the reactions of the fixed bed pre-reactor 7, the reaction rectifying tower 8 and the fixed bed pre-reactor 7 and researching one by one on the basis of the reaction mechanism, so that the step-by-step deep reaction of the raw materials dimethyl carbonate and ethanol is realized. By utilizing the high selectivity of the solid catalyst to the methyl ethyl carbonate, the process can increase the ratio of the methyl ethyl carbonate to the diethyl carbonate to be more than 3:1, simultaneously reserve the flexible switching capacity of a homogeneous catalyst sodium methoxide, improve the reaction conversion rate of raw materials dimethyl carbonate and ethanol by using the solid catalyst, reduce side reactions, improve the product quality, simultaneously reduce the generation of solid wastes, prolong the service life of equipment, and ensure the safe and stable production of the device.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (6)
1. Device of solid catalyst coupling reaction rectification production ethyl methyl carbonate, including dimethyl carbonate storage tank (1), anhydrous alcohol storage tank (2), feed mixer (3), raw materials blending tank (4), raw materials delivery pump (5), feeding preheater (6), fixed bed prereactor (7), reactive distillation column (8), circulating water cooler (9), reflux drum (10), tower bottom reboiler (11), plate and frame filter press (12), filtrating jar (13), thick diethyl carbonate knockout tower (14) and thick ethyl methyl carbonate knockout tower (15), its characterized in that: the dimethyl carbonate storage tank (1) and the anhydrous ethanol storage tank (2) are connected with a feed mixer (3) through pumps, the output end of the feed mixer (3) is connected with a raw material mixing tank (4) through a pipeline, the output end of the raw material mixing tank (4) is connected with a feed preheater (6) through a raw material conveying pump (5), the feed preheater (6) is connected with a fixed bed pre-reactor (7) through a pipeline, the output end of the fixed bed pre-reactor (7) is connected with the top of a reaction rectifying tower (8) through a pipeline, the gas phase at the top of the reaction rectifying tower (8) is connected with a circulating water cooler (9) through a pipeline, the tower kettle of the reaction rectifying tower (8) is connected with a plate and frame filter press (12) through a pipeline, the output end of the plate and frame filter press (12) is connected with a filtrate tank (13) through a pipeline, the reaction rectifying tower (8) is connected with a reboiler kettle (11) through a pipeline, the output end of the tower kettle reboiler (11) is connected with the bottom of the reaction rectifying tower (8) through a pipeline, the filtrate tank (13) is connected with the crude diethyl carbonate separating tower (14) through a pipeline, the output end of the crude diethyl carbonate separating tower (14) is connected with the crude methylethyl carbonate separating tower (15) through a pipeline, and the top of the crude methylethyl carbonate separating tower (15) is connected with the feeding mixer (3) through a pipeline.
2. The device for producing ethyl methyl carbonate by coupling reaction and rectification of the solid catalyst according to claim 1, which is characterized in that: the feed mixer (3) is provided with three inlets which are respectively connected with a dimethyl carbonate storage tank (1), an absolute ethyl alcohol storage tank (2) and a crude methyl ethyl carbonate separation tower (15).
3. The device for producing ethyl methyl carbonate by coupling reaction and rectification of the solid catalyst according to claim 1, which is characterized in that: the feeding preheater (6) is a shell-and-tube heat exchanger in countercurrent contact, and a jacket heat retainer is arranged in the fixed bed prereactor (7).
4. The device for producing ethyl methyl carbonate by coupling reaction and rectification of the solid catalyst according to claim 1, which is characterized in that: the reactive distillation column (8) consists of two sections of CY700 wire mesh corrugated packing and 25 layers of trays.
5. The device for producing ethyl methyl carbonate by coupling reaction and rectification of the solid catalyst according to claim 1, which is characterized in that: the output end of the circulating water cooler (9) is connected with a reflux tank (10), and the output end of the reflux tank (10) is connected with the top of the reaction rectifying tower (8).
6. A method for producing methyl ethyl carbonate by coupling reaction and rectification of a solid catalyst is characterized by comprising the following steps: the method comprises the following steps:
s1, firstly, conveying raw materials of ethanol and dimethyl carbonate into a feeding mixer (3) through a raw material conveying pump and a pipeline, preheating the raw materials to a reaction temperature of 85 ℃ through a feeding preheater (6), conveying the raw materials into a fixed bed prereactor (7), achieving first-stage reaction balance through prereaction, consuming 50% of dimethyl carbonate and ethanol through reaction, feeding the reacted materials into a reaction rectifying tower (8), carrying out reaction rectification under the catalysis of homogeneous sodium methoxide, extracting a side reaction product of methanol from the top of the reaction rectifying tower (8), extracting methylethyl carbonate, diethyl carbonate and unreacted excessive dimethyl carbonate from the bottom of the tower, and if the bottom of the tower contains trace unreacted ethanol, recovering the unreacted ethanol along with the top of a crude methylethyl carbonate separating tower (15) for reuse;
s2, feeding tower bottom materials in the reaction rectifying tower (8) into a crude diethyl carbonate separating tower (14), obtaining crude diethyl carbonate with the purity of 99.8% at the tower bottom, extracting ethyl methyl carbonate and unreacted dimethyl carbonate from the tower top, and feeding tower top products into a crude ethyl methyl carbonate separating tower (15);
and (3) further rectifying and refining the two crude products produced in the steps S3, S1 and S2 to produce electronic grade ethyl methyl carbonate and diethyl carbonate, and repeating the steps until the dimethyl carbonate and the ethanol are fully and deeply reacted and discharged.
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| CN202210414055.1A CN114534291A (en) | 2022-04-20 | 2022-04-20 | Device and method for producing ethyl methyl carbonate by coupling reaction and rectification of solid catalyst |
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| CN202210414055.1A CN114534291A (en) | 2022-04-20 | 2022-04-20 | Device and method for producing ethyl methyl carbonate by coupling reaction and rectification of solid catalyst |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723834A (en) * | 2008-10-29 | 2010-06-09 | 深圳市飞扬实业有限公司 | Method for continuously producing carbonate mixed ester |
| WO2018233093A1 (en) * | 2017-06-20 | 2018-12-27 | 中国科学院过程工程研究所 | System and process for co-producing dimethyl carbonate and ethylene glycol |
| CN110845334A (en) * | 2019-11-15 | 2020-02-28 | 山东石大胜华化工集团股份有限公司 | Device and method for producing battery-grade ethyl methyl carbonate by using dimethyl carbonate and ethanol |
| CN215517222U (en) * | 2021-04-16 | 2022-01-14 | 汇智工程科技股份有限公司 | Safety interlocking system for process for co-producing methyl ethyl carbonate and diethyl carbonate by dimethyl carbonate and ethanol |
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- 2022-04-20 CN CN202210414055.1A patent/CN114534291A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101723834A (en) * | 2008-10-29 | 2010-06-09 | 深圳市飞扬实业有限公司 | Method for continuously producing carbonate mixed ester |
| WO2018233093A1 (en) * | 2017-06-20 | 2018-12-27 | 中国科学院过程工程研究所 | System and process for co-producing dimethyl carbonate and ethylene glycol |
| CN110845334A (en) * | 2019-11-15 | 2020-02-28 | 山东石大胜华化工集团股份有限公司 | Device and method for producing battery-grade ethyl methyl carbonate by using dimethyl carbonate and ethanol |
| CN215517222U (en) * | 2021-04-16 | 2022-01-14 | 汇智工程科技股份有限公司 | Safety interlocking system for process for co-producing methyl ethyl carbonate and diethyl carbonate by dimethyl carbonate and ethanol |
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Application publication date: 20220527 |