CN115193364A - Device and method for synthesizing dimethyl carbonate - Google Patents

Device and method for synthesizing dimethyl carbonate Download PDF

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Publication number
CN115193364A
CN115193364A CN202211129911.5A CN202211129911A CN115193364A CN 115193364 A CN115193364 A CN 115193364A CN 202211129911 A CN202211129911 A CN 202211129911A CN 115193364 A CN115193364 A CN 115193364A
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dimethyl carbonate
flash
degassing
synthesizer
tower
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曹德龙
滕文彬
张生安
刘文祥
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Shandong Haike Xinyuan Material Technology Co ltd
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Shandong Haike Xinyuan Material Technology Co ltd
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J8/00—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes
    • B01J8/02—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds
    • B01J8/06—Chemical or physical processes in general, conducted in the presence of fluids and solid particles; Apparatus for such processes with stationary particles, e.g. in fixed beds in tube reactors; the solid particles being arranged in tubes
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C68/00—Preparation of esters of carbonic or haloformic acids
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C68/00—Preparation of esters of carbonic or haloformic acids
    • C07C68/08—Purification; Separation; Stabilisation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002—Chemical plants
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Abstract

The invention provides a device and a method for synthesizing dimethyl carbonate, and relates to the technical field of dimethyl carbonate synthesis. The dimethyl carbonate synthesizer is provided with a material circulating system, so that the conversion rate of mixed raw material gas can be improved, the material loss can be reduced by the degassing tower, the cyclic utilization of reaction materials is realized, the filler is filled in the flash tank, the loss of dimethyl carbonate can be reduced, the yield is improved, the method is simple and efficient, the synthesis of dimethyl carbonate is realized, and the primary separation and cyclic utilization of materials are realized at the same time.

Description

Device and method for synthesizing dimethyl carbonate
Technical Field
The invention relates to the technical field of fine chemical engineering, in particular to a device and a method for synthesizing dimethyl carbonate.
Background
Dimethyl carbonate (dimethyl carbonate) is an important, nontoxic and environment-friendly green chemical product, and is known as 'new base stone' organically synthesized in the 21 st century. Dimethyl carbonate is an important raw material for green synthesis of organic carbonate and polyester, can be used as an additive for improving the octane number of gasoline, and is also widely used for preparation of electrolyte of lithium ion batteries.
The industrial synthesis method of dimethyl carbonate mainly comprises a phosgene method, an ester exchange method, a methanol oxidation carbonylation method and a urea alcoholysis method. As is well known, phosgene is extremely toxic, and the phosgene method has been gradually replaced by other methods for environmental protection reasons; the equipment investment of the ester exchange method is high, and the product yield is low; and with methanol, O 2 And CO and the like are taken as raw materials, and the methanol oxidation carbonylation method for preparing the dimethyl carbonate has great attention because the raw materials are cheap and easy to obtain, have good economic value and meet the requirements of clean production and green chemical industry.
Patent application No. CN201610878323.X discloses a method for synthesizing dimethyl carbonate, which mainly solves the problems of poor catalyst activity and easy loss of active components in the prior art and comprises the steps of contacting ethylene carbonate and methanol with a catalyst under the condition of ester exchange reaction; the catalyst comprises: the technical proposal of 5 to 40 weight percent of alkaline earth metal calculated by MO and 60 to 95 weight percent of phosphorus-aluminum-oxygen carrier APO better solves the problem and can be used in the industrial production of preparing dimethyl carbonate by the ester exchange of ethylene carbonate and methanol.
The current patents focus mainly on the synthesis of catalysts, but there are few methods related to industrialization.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method and a device for synthesizing dimethyl carbonate, which have simple structure and convenient operation.
In order to realize the purpose, the invention is realized by the following technical scheme:
the raw material gas provided by the invention is Methyl Nitrite (MN), carbon monoxide (CO) and nitrogen (N) 2 ) The reaction product is a mixture of dimethyl carbonate (DMC), dimethyl oxalate (DMO), methanol (ME), methylal (DMM) and Methyl Formate (MF).
According to one aspect of the application, the device for synthesizing dimethyl carbonate comprises a preheater, a dimethyl carbonate synthesizer, a degassing tower and a flash tank, wherein a feeding port of the dimethyl carbonate synthesizer is connected with the preheater, the dimethyl carbonate synthesizer is provided with a material circulating system, a material inlet at the bottom of the degassing tower is connected with a bottom outlet of the dimethyl carbonate synthesizer, a condenser and a reflux tank are arranged at the top of the degassing tower, a bottom outlet of the degassing tower is connected with a bottom inlet of the flash tank, a bottom outlet of the flash tank is connected with a crude dimethyl carbonate pump through a flash discharging pump and the crude dimethyl carbonate tank, the material circulating system comprises a circulating reaction pump and a dimethyl carbonate reaction intermediate tank, and a circulating material outlet of the dimethyl carbonate synthesizer is connected with a circulating material inlet through the dimethyl carbonate reaction intermediate tank and the circulating reaction pump.
Preferably, the dimethyl carbonate synthesizer is a fixed bed reactor, preferably a tubular reactor, and the synthesizer is filled with a catalyst loaded with palladium-based metal.
Preferably, the degassing tower is a packed tower, and the number of tower plates in the packed tower is 10-25.
Preferably, the upper part of the flash tank is filled with 1-4 sections of fillers.
Preferably, the inlet material of the preheater is CO/MN/N 2 The mixed gas of (1).
According to another aspect of the present application, the present invention provides a method for synthesizing dimethyl carbonate.
The method is suitable for synthesizing the dimethyl carbonate by taking the Methyl Nitrite (MN) and the carbon monoxide (CO) as raw materials.
The method specifically comprises the following steps:
step one, dimethyl carbonate synthesis method
Preheating a raw material mixed gas, and conveying the raw material mixed gas to a dimethyl carbonate synthesizer for synthesis reaction, wherein in order to improve the conversion rate of raw material gas, part of reaction materials are subjected to cyclic reaction in a material circulating system, and a final reaction product is conveyed to a degassing tower from an outlet at the bottom of the dimethyl carbonate synthesizer for degassing treatment;
step two, degassing treatment method
The reaction product from the bottom outlet of the dimethyl carbonate synthesizer is degassed in a degassing tower, and the gas phase products obtained at the top of the degassing tower are mainly CO and N 2 Mixture of (2), CO and N 2 The mixture is treated by a condenser and a reflux tank, then is conveyed to a methyl nitrite regeneration tower for MN regeneration, and then is recycled, and liquid-phase products obtained at the bottom of a degassing tower mainly comprise dimethyl carbonate, dimethyl oxalate, methanol, methylal and methyl formate and are conveyed to a flash tank for treatment;
step three, flash evaporation treatment method
And (3) carrying out degassing treatment on the liquid-phase product from the bottom outlet of the degassing tower in a flash tank, conveying the light-component material obtained from the top of the flash tank to an alkaline washing tower for treatment, recovering methanol, and conveying the crude dimethyl carbonate obtained from the bottom of the flash tank to a subsequent refining method for purification treatment.
According to one embodiment of the application, in the dimethyl carbonate synthesis method, the volume composition of the raw material mixed gas is CO: MN: N 2 =1:2.5～5:4～6.5；
The temperature of the mixed raw material gas after the raw material mixed gas is preheated is 75-95 ℃;
the reaction temperature of the dimethyl carbonate synthesizer is 100-140 ℃, and the reaction pressure is 0.1-1 MPa.
According to one embodiment of the application, in the degassing treatment method, in order to prevent heavy component materials from being carried out from the top of a degassing tower by gas phase materials in the degassing process, methanol is injected into the upper part of the top of the degassing tower, and the gas phase materials are subjected to condensation treatment and recovery;
the temperature of the condensed material in the condenser is 10-30 ℃, and the pressure of the condensed material is 0.1-1 MPa.
According to one embodiment of the application, in the flash evaporation treatment method, in order to prevent the heavy component material from being carried out of the flash evaporation tank by the gas phase material in the flash evaporation process, methanol is injected into the upper part of the flash evaporation tank, and the temperature and the pressure of the flash evaporation are strictly controlled;
the temperature of the flash evaporation is 43-55 ℃, and the pressure of the flash evaporation is 0.1-0.2 MPa;
the mass ratio of the flash-evaporated light components is as follows: methylal: methyl formate: methanol: 50-60% of dimethyl carbonate, 1-10% of dimethyl carbonate, 0.05-0.5% of dimethyl carbonate, 30-40% of dimethyl carbonate, and 0.05-0.5% of dimethyl carbonate;
the mass ratio of the flash evaporated crude dimethyl carbonate is as follows: methanol: dimethyl carbonate: 70-78% and 0.5-2% of dimethyl oxalate = 20-28%.
The invention provides a device and a method for synthesizing dimethyl carbonate. The method has the following beneficial effects:
1. the dimethyl carbonate synthesizer is provided with a material circulating system, the material circulating system comprises a circulating reaction pump and a dimethyl carbonate reaction intermediate tank, a circulating material outlet of the dimethyl carbonate synthesizer is connected with a circulating material inlet through the dimethyl carbonate reaction intermediate tank and the circulating reaction pump, and the conversion rate of mixed raw material gas can be improved;
2. according to the degassing tower, the tower plate is arranged in the packed tower, so that the material loss can be reduced, and the cyclic utilization of reaction materials is realized;
3. the flash tank is filled with the filler, so that the loss of the dimethyl carbonate can be reduced, and the yield is improved;
4. the method is simple and efficient, and not only realizes the synthesis of the dimethyl carbonate, but also realizes the primary separation and the recycling of materials.
Drawings
FIG. 1 is a schematic view of an apparatus of the present invention;
wherein: 1. a preheater; 2. a dimethyl carbonate synthesizer; 3. a dimethyl carbonate reaction intermediate tank; 4. a circulating reaction pump; 5. a degassing tower; 6. a condenser; 7. a reflux tank; 8. a flash tank; 9. a flash evaporation discharge pump; 10. a crude dimethyl carbonate tank; 11. crude dimethyl carbonate pump.
12: raw material mixed gas; 13: methanol; 14: methanol; 15: introducing the mixture of nitric oxide and nitrogen into a methyl nitrite regeneration tower; 16: sending the light components to an alkaline washing tower, and recovering methanol; 17: crude dimethyl carbonate to a subsequent refining process.
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 obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
The application provides a device and a method for synthesizing dimethyl carbonate, and the method and the device are suitable for synthesizing the dimethyl carbonate by taking Methyl Nitrite (MN) and carbon monoxide (CO) as raw materials.
The raw material gas provided by the invention is Methyl Nitrite (MN), carbon monoxide (CO) and nitrogen (N) 2 ) The reaction product is a mixture of dimethyl carbonate (DMC), dimethyl oxalate (DMO), methanol (ME), methylal (DMM) and Methyl Formate (MF).
The first embodiment is as follows:
as shown in fig. 1, the embodiment of the invention provides an apparatus and a method for synthesizing dimethyl carbonate, the apparatus includes a preheater 1, a dimethyl carbonate synthesizer 2, a degassing tower 5, and a flash tank 8, a feed inlet of the dimethyl carbonate synthesizer 2 is connected with the preheater 1, the dimethyl carbonate synthesizer 2 is provided with a material circulation system, a material inlet at the bottom of the degassing tower 5 is connected with a bottom outlet of the dimethyl carbonate synthesizer 2, the top of the degassing tower 5 is provided with a condenser 6 and a reflux tank 7, a bottom outlet of the degassing tower 5 is connected with a bottom inlet of the flash tank 8, and a bottom outlet of the flash tank 8 is connected with a crude dimethyl carbonate pump 11 through a flash discharge pump 9 and a crude dimethyl carbonate tank 10.
The dimethyl carbonate synthesizer 2 is provided with the material circulating system, so that the conversion rate of the mixed raw material gas can be improved, the device is simple and efficient, the synthesis of dimethyl carbonate is realized, and the primary separation and the cyclic utilization of materials are realized.
According to one embodiment of the application, the material circulating system comprises a circulating reaction pump 4 and a dimethyl carbonate reaction intermediate tank 3, and a circulating material outlet of a dimethyl carbonate synthesizer 2 is connected with a circulating material inlet through the dimethyl carbonate reaction intermediate tank 3 and the circulating reaction pump 4, so that the conversion rate of mixed raw material gas can be improved.
According to one embodiment of the present application, the dimethyl carbonate synthesizer 2 is a fixed bed reactor, preferably a tubular reactor, packed with a catalyst loaded with palladium-based metals.
According to one embodiment of the application, the degassing tower 5 is a packed tower, the number of tower plates in the packed tower is 10, the material loss can be reduced through the degassing tower 5, and the recycling of reaction materials is realized.
According to one embodiment of the application, the upper part of the flash tank 8 is filled with 1 section of filling material, and the flash tank 8 is filled with the filling material, so that the loss of dimethyl carbonate can be reduced, and the yield is improved.
According to one embodiment of the application, the inlet material of the preheater 1 is CO/MN/N 2 The mixed gas of (1).
The method comprises the following specific steps:
step one, dimethyl carbonate synthesis method
The raw material gas mixture is preheated and then conveyed to a dimethyl carbonate synthesizer 2 for synthesis reaction, in order to improve the conversion rate of the raw material gas, part of reaction materials are subjected to circulation reaction in a material circulation system, and the final reaction product is conveyed to a degassing tower 5 from the bottom outlet of the dimethyl carbonate synthesizer 2 for degassing treatment.
According to one embodiment of the present application, the raw gas mixture has a volume composition of CO: MN: N 2 =1:2.5～5:4～6.5；
The temperature of the mixed raw material gas after the raw material mixed gas is preheated is 75 ℃;
the reaction temperature of the dimethyl carbonate synthesizer 2 is 100 ℃, and the reaction pressure is 0.1MPa.
Step two, degassing treatment method
A reaction product from a bottom outlet of a dimethyl carbonate synthesizer 2 is subjected to degassing treatment in a degassing tower 5, a gas-phase product obtained at the top of the degassing tower 5 is mainly a mixture of nitric oxide and nitrogen, the mixture of nitric oxide and nitrogen is treated by a condenser 6 and a reflux tank 7 and then is conveyed to a methyl nitrite regeneration tower for methyl nitrite regeneration and then is recycled, and a liquid-phase product obtained at the bottom of the degassing tower 5 is mainly dimethyl carbonate, dimethyl oxalate, methanol, methylal and methyl formate and is conveyed to a flash tank 8 for treatment.
According to one embodiment of the present application, in order to prevent the heavy component materials from being carried out of the top of the degassing tower 5 by the gas phase materials during the degassing process, it is necessary to inject methanol into the top upper portion of the degassing tower 5, and to perform condensation processing and recovery of the gas phase materials.
According to one embodiment of the present application, the temperature of the condensed material in the condenser 6 is 10 ℃ to 30 ℃, and the pressure of the condensed material is 0.1MPa to 1MPa.
Step three, flash evaporation treatment method
And (3) degassing the liquid-phase product from the outlet at the bottom of the degassing tower 5 in a flash tank 8, conveying the light-component material obtained from the top of the flash tank 8 to an alkaline washing tower for treatment, recovering methanol, and conveying the crude dimethyl carbonate obtained from the bottom of the flash tank 8 to a subsequent refining method for purification treatment.
According to one embodiment of the present application, in order to prevent the heavy component material from being carried out of the flash tank 8 by the gas phase material in the flash process, methanol is injected into the upper part of the flash tank 8, and the temperature and pressure of the flash are strictly controlled;
according to one embodiment of the present application, the temperature of the flash is 43 ℃ and the pressure of the flash is 0.1MPa;
the mass ratio of the flash evaporated light components is as follows: methylal: methyl formate: methanol: dimethyl carbonate = 50-60%, 30-40%, 1-10%, 0.05-0.5%;
the mass ratio of the flash evaporated crude dimethyl carbonate is as follows: methanol: dimethyl carbonate: 70-78% of dimethyl oxalate and 0.5-2% of dimethyl oxalate.
The second embodiment:
as shown in fig. 1, the embodiment of the invention provides an apparatus and a method for synthesizing dimethyl carbonate, the apparatus includes a preheater 1, a dimethyl carbonate synthesizer 2, a degassing tower 5, and a flash tank 8, a feed inlet of the dimethyl carbonate synthesizer 2 is connected with the preheater 1, the dimethyl carbonate synthesizer 2 is provided with a material circulation system, a material inlet at the bottom of the degassing tower 5 is connected with a bottom outlet of the dimethyl carbonate synthesizer 2, the top of the degassing tower 5 is provided with a condenser 6 and a reflux tank 7, a bottom outlet of the degassing tower 5 is connected with a bottom inlet of the flash tank 8, and a bottom outlet of the flash tank 8 is connected with a crude dimethyl carbonate pump 11 through a flash discharge pump 9 and a crude dimethyl carbonate tank 10.
The dimethyl carbonate synthesizer 2 is provided with the material circulating system, so that the conversion rate of the mixed raw material gas can be improved, the device is simple and efficient, the synthesis of dimethyl carbonate is realized, and the primary separation and the cyclic utilization of materials are realized.
According to one embodiment of the application, the material circulation system comprises a circulation reaction pump 4 and a dimethyl carbonate reaction intermediate tank 3, and a circulation material outlet of a dimethyl carbonate synthesizer 2 is connected with a circulation material inlet through the dimethyl carbonate reaction intermediate tank 3 and the circulation reaction pump 4, so that the conversion rate of the mixed raw material gas can be improved.
According to one embodiment of the present application, the dimethyl carbonate synthesizer 2 is a fixed bed reactor, preferably a tubular reactor, packed with a catalyst loaded with palladium-based metal.
According to one embodiment of the application, the degassing tower 5 is a packed tower, the number of tower plates in the packed tower is 18, the material loss can be reduced through the degassing tower 5, and the recycling of reaction materials is realized.
The upper part of the flash tank 8 is filled with 2 sections of filling materials, and the flash tank 8 is filled with the filling materials, so that the loss of the dimethyl carbonate can be reduced, and the yield is improved.
According to one embodiment of the application, the inlet material of the preheater 1 is CO/MN/N 2 The mixed gas of (1).
The method comprises the following specific steps:
step one, dimethyl carbonate synthesis method
The raw material mixed gas is preheated and then is conveyed to a dimethyl carbonate synthesizer 2 for synthesis reaction, in order to improve the conversion rate of the raw material gas, part of reaction materials are subjected to circulation reaction among material circulation systems, and the final reaction product is conveyed to a degassing tower 5 from the bottom outlet of the dimethyl carbonate synthesizer 2 for degassing treatment.
According to one embodiment of the present application, the raw gas mixture has a volume composition of CO: MN: N 2 =1:2.5～5:4～6.5；
The temperature of the mixed raw material gas after the raw material mixed gas is preheated is 85 ℃;
the reaction temperature of the dimethyl carbonate synthesizer 2 is 120 ℃, and the reaction pressure is 0.5MPa.
Step two, degassing treatment method
The reaction product from the bottom outlet of the dimethyl carbonate synthesizer 2 is degassed in a degassing tower 5, and the gas phase products obtained from the top of the degassing tower 5 are mainly nitric oxide and N 2 Mixture of (A), nitric oxide and N 2 The mixture is treated by a condenser 6 and a reflux tank 7, then is conveyed to a methyl nitrite regeneration tower for MN regeneration, and then is recycled, and liquid-phase products obtained from the bottom of a degassing tower 5, mainly dimethyl carbonate, dimethyl oxalate, methanol, methylal and methyl formate, are conveyed to a flash tank 8 for treatment.
According to one embodiment of the present application, in order to prevent the heavy component material from being carried out of the top of the degassing tower 5 by the gas phase material during the degassing process, it is necessary to inject methanol into the top upper portion of the degassing tower 5, and to perform condensation treatment and recovery of the gas phase material.
According to one embodiment of the present application, the temperature of the condensed material in the condenser 6 is 20 ℃ and the pressure of the condensed material is 0.5MPa.
Step three, flash evaporation treatment method
And (3) degassing the liquid-phase product from the outlet at the bottom of the degassing tower 5 in a flash tank 8, conveying the light-component material obtained from the top of the flash tank 8 to an alkaline washing tower for treatment, recovering methanol, and conveying the crude dimethyl carbonate obtained from the bottom of the flash tank 8 to a subsequent refining method for purification treatment.
According to one embodiment of the present application, in order to prevent the heavy component material from being carried out of the flash tank 8 by the gas phase material in the flash process, methanol is injected into the upper part of the flash tank 8, and the temperature and pressure of the flash are strictly controlled;
according to one embodiment of the present application, the temperature of the flash is 50 ℃ and the pressure of the flash is 0.15MPa;
the mass ratio of the flash evaporated light components is as follows: methylal: methyl formate: methanol: 50-60% of dimethyl carbonate, 1-10% of dimethyl carbonate, 0.05-0.5% of dimethyl carbonate, 30-40% of dimethyl carbonate, and 0.05-0.5% of dimethyl carbonate;
the mass ratio of the flash evaporated crude dimethyl carbonate is as follows: methanol: dimethyl carbonate: 70-78% of dimethyl oxalate and 0.5-2% of dimethyl oxalate.
According to one embodiment of the present application, the degassing column 5 is a packed column having 25 trays. The upper part of the flash tank 8 is filled with 4 sections of filling materials.
According to one embodiment of the application, the temperature of the mixed raw material gas after the raw material mixed gas is preheated is 95 ℃; the reaction temperature of the dimethyl carbonate synthesizer 2 is 140 ℃, and the reaction pressure is 1MPa.
According to one embodiment of the present application, the temperature of the condensed material in the condenser 6 is 30 ℃ and the pressure of the condensed material is 1MPa.
According to one embodiment of the present application, the temperature of the flash is 55 ℃ and the pressure of the flash is 0.2MPa;
although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various 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 (9)

1. The utility model provides a device of synthetic dimethyl carbonate, includes preheater (1), dimethyl carbonate synthesizer (2), degasser (5), flash drum (8), its characterized in that: the material inlet of the dimethyl carbonate synthesizer (2) is connected with the preheater (1), the dimethyl carbonate synthesizer (2) is provided with a material circulating system, a material inlet at the bottom of the degassing tower (5) is connected with a bottom outlet of the dimethyl carbonate synthesizer (2), the top of the degassing tower (5) is provided with a condenser (6) and a reflux tank (7), a bottom outlet of the degassing tower (5) is connected with a bottom inlet of a flash tank (8), a bottom outlet of the flash tank (8) is connected with a crude dimethyl carbonate pump (11) through a flash evaporation discharging pump (9) and a crude dimethyl carbonate tank (10), the material circulating system comprises a circulating reaction pump (4) and a dimethyl carbonate reaction intermediate tank (3), and a circulating material outlet of the dimethyl carbonate synthesizer (2) is connected with the circulating material inlet through the dimethyl carbonate reaction intermediate tank (3) and the circulating reaction pump (4).
2. The apparatus for synthesizing dimethyl carbonate according to claim 1, wherein: the dimethyl carbonate synthesizer (2) is a fixed bed reactor, and a catalyst loaded with palladium-based metal is filled in the dimethyl carbonate synthesizer (2).
3. The apparatus for synthesizing dimethyl carbonate according to claim 1, wherein: the dimethyl carbonate synthesizer (2) is a tubular reactor.
4. The apparatus for synthesizing dimethyl carbonate according to claim 1, wherein: the degassing tower (5) is a packed tower, and the number of tower plates in the packed tower is 10-25.
5. The apparatus for synthesizing dimethyl carbonate according to claim 1, wherein: the upper part of the flash tank (8) is provided with 1-4 sections of fillers.
6. A method for synthesizing dimethyl carbonate, which employs the apparatus for synthesizing dimethyl carbonate according to any one of claims 2 to 5, characterized in that: the method is suitable for synthesizing dimethyl carbonate by taking methyl nitrite and carbon monoxide as raw materials, and comprises the following steps:
step one, dimethyl carbonate synthesis method
Preheating raw material mixed gas, conveying the raw material mixed gas to a dimethyl carbonate synthesizer (2) for synthesis reaction, performing circulation reaction on part of reaction materials among a material circulation system, and conveying a final reaction product to a degassing tower (5) from a bottom outlet of the dimethyl carbonate synthesizer (2) for degassing treatment;
step two, degassing treatment method
A reaction product from a bottom outlet of a dimethyl carbonate synthesizer (2) is subjected to degassing treatment in a degassing tower (5), a gas-phase product obtained at the top of the degassing tower (5) is a mixture of nitric oxide and nitrogen, the mixture of nitric oxide and nitrogen is treated by a condenser (6) and a reflux tank (7), then is conveyed to a methyl nitrite regeneration tower for methyl nitrite regeneration and then is recycled, and a liquid-phase product obtained at the bottom of the degassing tower (5) is dimethyl carbonate, dimethyl oxalate, methanol, methylal and methyl formate, and is conveyed to a flash tank (8) for treatment;
step three, flash evaporation treatment method
And (3) degassing the liquid-phase product from the outlet at the bottom of the degassing tower (5) in a flash tank (8), conveying the light-component material obtained from the top of the flash tank (8) to an alkaline washing tower for treatment, recovering methanol, and purifying the crude dimethyl carbonate obtained from the bottom of the flash tank (8).
7. The method for synthesizing dimethyl carbonate according to claim 6, wherein: in the dimethyl carbonate synthesis method, the volume composition of the raw material gas mixture is carbon monoxide: methyl nitrite: nitrogen = 1;
the temperature of the mixed raw material gas after the raw material mixed gas is preheated is 75-95 ℃;
the reaction temperature of the dimethyl carbonate synthesizer (2) is 100-140 ℃, and the reaction pressure is 0.1-1 MPa.
8. The method for synthesizing dimethyl carbonate according to claim 6, wherein: in the degassing treatment method, in order to prevent heavy component materials from being brought out from the top of a degassing tower (5) by gas phase materials in the degassing process, methanol is injected into the upper part of the top of the degassing tower (5), and the gas phase materials are subjected to condensation treatment and recovery;
the temperature of the condensed material in the condenser (6) is 10-30 ℃, and the pressure of the condensed material is 0.1-1 MPa.
9. The method for synthesizing dimethyl carbonate according to claim 6, wherein: in the flash evaporation treatment method, in order to prevent the heavy component material from being brought out of the flash evaporation tank (8) by the gas phase material in the flash evaporation process, methanol is injected into the upper part of the flash evaporation tank (8), and the temperature and the pressure of flash evaporation are controlled;
the temperature of the flash evaporation is 43-55 ℃, and the pressure of the flash evaporation is 0.1-0.2 MPa;
the flash-evaporated light component comprises the following components in percentage by mass: methyl formate: methanol: 50-60% of dimethyl carbonate, 1-10% of dimethyl carbonate, 0.05-0.5% of dimethyl carbonate, 30-40% of dimethyl carbonate, and 0.05-0.5% of dimethyl carbonate;
the mass ratio of the flash evaporated crude dimethyl carbonate is as follows: dimethyl carbonate: 70-78% and 0.5-2% of dimethyl oxalate = 20-28%.
CN202211129911.5A 2022-09-16 2022-09-16 Device and method for synthesizing dimethyl carbonate Pending CN115193364A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0625104A (en) * 1991-07-19 1994-02-01 Ube Ind Ltd Continuous production of dimethyl carbonate
CN104529783A (en) * 2014-12-17 2015-04-22 南京工业大学 Efficient and safe method for synthesizing carbonic ester by oxidative carbonylation
CN207958189U (en) * 2018-02-09 2018-10-12 杨晓利 Utilize the reaction unit of Dimethyl Carbonate Synthesis from Methanol
CN110776424A (en) * 2019-10-09 2020-02-11 中盐安徽红四方股份有限公司 Refining apparatus and process using DMC

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH0625104A (en) * 1991-07-19 1994-02-01 Ube Ind Ltd Continuous production of dimethyl carbonate
CN104529783A (en) * 2014-12-17 2015-04-22 南京工业大学 Efficient and safe method for synthesizing carbonic ester by oxidative carbonylation
CN207958189U (en) * 2018-02-09 2018-10-12 杨晓利 Utilize the reaction unit of Dimethyl Carbonate Synthesis from Methanol
CN110776424A (en) * 2019-10-09 2020-02-11 中盐安徽红四方股份有限公司 Refining apparatus and process using DMC

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