CN114940670A - Process system for producing high-purity carbonic ester solvent of lithium battery - Google Patents
Process system for producing high-purity carbonic ester solvent of lithium battery Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/36—Alkylene carbonates; Substituted alkylene carbonates
- C07D317/38—Ethylene carbonate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- 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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- C07—ORGANIC CHEMISTRY
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- C07C68/06—Preparation of esters of carbonic or haloformic acids from organic carbonates
- C07C68/065—Preparation of esters of carbonic or haloformic acids from organic carbonates from alkylene carbonates
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- 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
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention discloses a process system for producing a high-purity carbonic ester solvent of a lithium battery, wherein ethylene oxide and carbon dioxide serving as raw materials enter a vinyl carbonate working section, undergo a cycloaddition reaction under the catalysis of an immobilized ionic liquid, and are separated and purified to obtain high-purity vinyl carbonate; feeding the ethylene carbonate and methanol into a dimethyl carbonate working section, carrying out alcoholysis reaction rectification under the catalysis of alkali metal oxide, and carrying out pressure swing azeotropic rectification separation and a dimethyl carbonate refining system to obtain high-purity dimethyl carbonate; dimethyl carbonate and ethanol are subjected to ester exchange reaction rectification under the catalytic action of alkali metal oxide, high-purity ethyl methyl carbonate and diethyl carbonate are obtained through an ethyl methyl carbonate and diethyl carbonate refining system, and the dimethyl carbonate is recycled after being purified by partition extraction rectification and a dimethyl carbonate refining system.
Description
Technical Field
The invention relates to the field of high-purity solvents for battery electrolytes, relates to production methods of ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate, and particularly relates to a process system for producing high-purity carbonate solvents for lithium batteries.
Background
Under the background of 'carbon peak reaching' and 'carbon neutralization', the new energy industry is rapidly developed, and a lithium battery as a new energy battery is rapidly developed in recent years. The electrolyte is the 'blood' of the lithium ion battery, determines the comprehensive performance of the lithium ion battery, and consists of three parts, namely lithium salt, a solvent and an additive. Wherein the high-purity solvent is a mixed system consisting of five carbonate (ethylene carbonate (EC), Propylene Carbonate (PC), dimethyl carbonate (DMC), Ethyl Methyl Carbonate (EMC) and diethyl carbonate (DEC)). In recent years, high-purity ethyl methyl carbonate and diethyl carbonate are used as important solvents of lithium ion battery electrolytes, and production process methods thereof become attention objects. The quality of the battery-grade carbonate applied to an electrolyte solvent must be strictly controlled before the battery-grade carbonate is used, the purity requirement is generally more than 99.99 percent, even the purity reaches 99.995 percent, the requirement of the lithium ion battery electrolyte solvent can be met, the moisture of an organic solvent is strictly controlled, and the preparation of qualified lithium battery electrolyte is decisively influenced.
The synthesized ethylene carbonate is mainly obtained by performing cycloaddition reaction on ethylene oxide and carbon dioxide, wherein a catalyst is closely related to reaction conditions, and the production of dimethyl carbonate has multiple ways and has industrial application prospects as follows: transesterification of ethylene carbonate or propylene carbonate with methanol, urea alcoholysis and methanol carbonylation based on coal chemical routes. The mainstream process for the production of ethyl methyl carbonate and diethyl carbonate is obtained by transesterification of dimethyl carbonate with ethanol.
CN112142599A discloses a method and a system for producing a low-energy-consumption and green carbonate product, wherein the production process is divided into a vinyl carbonate unit, dimethyl carbonate and methyl ethyl carbonate unit, but key information such as the purity of the produced carbonate is not disclosed, the high purity requirements of the products of methyl ethyl carbonate and diethyl carbonate under a limited separation tower cannot be guaranteed, and a KI solution is adopted as a catalyst to carry out cycloaddition reaction in the reaction process of the vinyl carbonate.
CN114380692A discloses a method for preparing energy-saving electronic grade carbonate, wherein dimethyl carbonate is used as a raw material in the focusing process, methyl ethyl carbonate and diethyl carbonate are produced through ester exchange with ethanol, an anti-disproportionation reactor is used for realizing the anti-disproportionation reaction of dimethyl carbonate and diethyl carbonate into methyl ethyl carbonate, the energy consumption of the methyl ethyl carbonate process is 2.9t/t carbonate product under the conditions of heat pump rectification and heat integration rectification, and the power consumption is 168kWh/t carbonate product.
The production process of the carbonic ester is mainly divided into the steps of adding ethylene oxide and carbon dioxide into ethylene carbonate/propylene carbonate, carrying out ester exchange on the ethylene carbonate/propylene carbonate and methanol to generate dimethyl carbonate and byproduct ethylene glycol/propylene glycol, and carrying out ester exchange on the dimethyl carbonate and ethanol to produce ethyl methyl carbonate and diethyl carbonate. The homogeneous catalyst adopted in the process is difficult to separate from the carbonic ester product, and the homogeneous catalyst can bring about the problem of environmental solid waste. The invention aims to construct a high-purity solvent production system of ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate by adopting a heterogeneous catalyst, and reduce the energy consumption of the high-purity carbonate system by adopting reactive distillation, extraction bulkhead distillation, heat pump distillation and heat integration distillation.
Disclosure of Invention
The invention aims to provide a process system for producing a high-purity carbonate solvent of a lithium battery, which adopts heterogeneous catalysts in three working sections of carbonate production, adopts reactive distillation in the working sections of dimethyl carbonate and ethyl methyl carbonate to reduce the energy consumption in the process, adopts extraction bulkhead distillation to realize process reinforcement in the separation process of dimethyl carbonate and methanol azeotrope, and adopts distillation heat integration and heat pump distillation in the purification process of carbonate to reduce the energy consumption in the separation and purification process of high-purity products.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: feeding Ethylene Oxide (EO) and carbon dioxide as raw materials into a working section of ethylene carbonate to perform cycloaddition reaction under the catalysis of immobilized ionic liquid, and separating and purifying to obtain high-purity ethylene carbonate; feeding the ethylene carbonate and methanol into a dimethyl carbonate working section to carry out alcoholysis reaction under the catalysis of alkali metal oxide, and separating and purifying to obtain high-purity dimethyl carbonate; dimethyl carbonate and ethanol are subjected to ester exchange reaction under the catalytic action of alkali metal oxide, and high-purity ethyl methyl carbonate/diethyl carbonate is obtained after the reaction is subjected to a separation and purification system. The method comprises the following specific steps:
and (2) allowing carbon dioxide and ethylene oxide to enter a first reactor filled with a heterogeneous catalyst, wherein the heterogeneous catalyst is an immobilized ionic liquid catalyst, a part of a reaction product discharged from the first reactor is circularly returned to the first reactor, a part of the reaction product enters a second reactor, a reaction product of the second reactor enters a flash evaporator, wherein a gas phase leaving a gas-liquid flash evaporator mainly contains ethylene oxide and carbon dioxide, a liquid phase mainly contains ethylene carbonate, and a gas phase stream passes through an absorption tower to remove ethylene oxide in the gas phase. And the liquid phase leaving the gas-liquid flash tank enters a subsequent refining unit to separate and purify the high-purity ethylene carbonate.
Ethylene carbonate and methanol are used as raw materials and enter a rectification tower for ethylene carbonate alcoholysis reaction for synchronous reaction and separation, and a heterogeneous catalyst is filled in the reaction rectification. The top of the reaction rectifying tower is azeotropic mixture of dimethyl carbonate and methanol, which is separated by subsequent pressure swing rectification, a condenser of the high-pressure tower provides heat for a reboiler of the reaction rectifying tower, a heat pump is adopted in the low-pressure tower for rectification to reduce the process energy consumption, a tower kettle of the high-pressure tower extracts a dimethyl carbonate crude product and then enters a dimethyl carbonate rectifying tower for subsequent separation, high-purity dimethyl carbonate (with the mass fraction of 99.99%) is extracted from the side line of the dimethyl carbonate rectifying tower, a tower kettle of the alcoholysis reaction rectifying tower is a mixture of ethylene carbonate and ethylene glycol and enters an ethylene glycol separating tower for separation of a byproduct, and the ethylene carbonate returns to the ethylene carbonate alcoholysis reaction rectifying tower.
Dimethyl carbonate and raw material ethanol enter a pre-reactor to carry out primary reaction, then enter an ester exchange reaction rectifying tower to carry out further reaction, a mixture of dimethyl carbonate and methanol is extracted from the top of the reaction rectifying tower, and a mixture of dimethyl carbonate/ethyl methyl carbonate/diethyl carbonate is extracted from the bottom of the tower. The azeotrope enters an extraction bulkhead for rectification and separation, methanol is extracted from the feed side of a partition plate in an extraction bulkhead rectifying tower, dimethyl carbonate is extracted from the other side of the partition plate, and an extractant at the bottom of the tower is recycled. The tower kettle of the reaction rectifying tower sequentially enters a dimethyl carbonate recovery tower and a ethyl methyl carbonate/diethyl carbonate rough separation tower for separation, wherein a rough separation tower condenser and a dimethyl carbonate recovery tower reboiler are used for heat integration and energy conservation. The obtained crude products of the methyl ethyl carbonate and the diethyl carbonate respectively enter a light-removing and heavy-removing tower to be combined to realize the production of electronic grade methyl ethyl carbonate and diethyl carbonate (the mass fraction is 99.99 wt%). The indirect heat pump rectification is adopted in the ethyl methyl carbonate/diethyl carbonate light-weight removal and heavy-weight removal tower to save energy in the process, the molecular sieve dehydration is carried out before the ethyl methyl carbonate/diethyl carbonate enters the product tank, and the saturated molecular sieve is subjected to stripping regeneration by hot nitrogen after water absorption. When the market demand of ethyl methyl carbonate is vigorous, diethyl carbonate and dimethyl carbonate pass through a reverse disproportionation reactor to produce ethyl methyl carbonate.
The solvent system for producing the high-purity carbonate of the lithium battery is characterized in that a heterogeneous immobilized ionic liquid catalyst is adopted in the addition reaction of the ethylene oxide and the carbon dioxide, wherein the heterogeneous immobilized ionic liquid catalyst can be SiO 2 、TiO 2 And the SBA-16 molecular sieve is used as a carrier to immobilize quaternary ammonium salt or imidazole ionic liquid.
The system for producing the high-purity carbonate solvent for the lithium battery is characterized in that the alcoholysis reaction of ethylene carbonate and methanol is realized in reactive distillation, wherein a catalytic packing is filled in a rectifying tower of the alcoholysis reaction, and a heterogeneous catalyst filled in the catalytic packing can be selected from strong-base quaternary ammonium ion exchange resin (Amberlyst A-26(OH)) or alkali metal oxide ZrO (ZrO) with a heterogeneous catalyst carrying hydroxyl counter ions 2 -Al 2 O 3 。
The system for producing the high-purity carbonate solvent for the lithium battery is characterized in that the transesterification reaction of dimethyl carbonate and ethanol is realized in a reaction rectifying tower, wherein the reaction rectifying tower is filled with a catalytic filler, and a heterogeneous catalyst filled in the catalytic filler can be selected from alkali metal oxide MgO/HZSM-5 and modified K coated by polyethylene glycol 2 CO 3 。
The system for producing the high-purity carbonic ester solvent for the lithium battery is characterized in that azeotrope separation of dimethyl carbonate and methanol in a working section of ethyl methyl carbonate and diethyl carbonate products is realized by extraction bulkhead rectification, wherein the extraction bulkhead rectification consists of an extraction rectification section, a side product section and an extractant recovery section, and the extractant is preferably aniline, N-methyl pyrrolidone and sulfolane.
The system for producing the high-purity carbonic ester solvent for the lithium battery is characterized in that an outlet of an addition reactor at a working section of the ethylene carbonate is subjected to flash evaporation to remove unreacted carbon dioxide and ethylene oxide, wherein the ethylene oxide is absorbed by using water as an absorbent, and the purification of the high-purity ethylene carbonate product is realized by combining an ethylene carbonate light impurity removal tower, an ethylene carbonate light impurity removal tower and an ethylene carbonate heavy impurity removal tower.
The system for producing the high-purity carbonate solvent for the lithium battery is characterized in that partial heat integration is carried out between a side-line reboiler of an alcoholysis reaction rectifying tower and a condenser of a ethylene carbonate recovery tower in a dimethyl carbonate production section.
The system for producing the lithium battery high-purity carbonate solvent is characterized in that heat integration is carried out between a condenser of a methyl ethyl carbonate/diethyl carbonate primary separation tower and a reboiler of a dimethyl carbonate recovery tower in a production working section of ethyl methyl carbonate and diethyl carbonate, and a light-ends removal tower and a heavy-ends removal tower of the ethyl methyl carbonate adopt heat pump rectification.
According to the invention, the feeding molar ratio of carbon dioxide to ethylene oxide in an ethylene carbonate working section is 1: 1-2: 1, the feeding molar ratio of ethylene carbonate to methanol in a dimethyl carbonate working section is 1: 3-1: 6, and the feeding molar ratio of dimethyl carbonate to ethanol in a methyl ethyl carbonate working section and a diethyl carbonate working section is 0.8: 1-2: 1. The conversion rate of ethylene oxide in the ethylene carbonate cycloaddition reactor is 95-100%, the conversion rate of ethylene carbonate in a dimethyl carbonate working section is 80-100%, the conversion rates of ethyl methyl carbonate and ethyl diethyl carbonate working section ethanol are 95-100%, and the selectivity of ethyl methyl carbonate is 60-95%. The feeding molar ratio of dimethyl carbonate to diethyl carbonate in the methyl ethyl carbonate reverse disproportionation reactor is 0.8: 1-1.2: 1, and the conversion rate of dimethyl carbonate is 50-80%. The mass fractions of ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate are more than or equal to 99.99 percent.
The beneficial effects of the invention are as follows:
(1) the production process of ethylene carbonate and dimethyl carbonate adopts an ethylene oxide route, and utilizes raw materials of carbon dioxide, methanol and ethanol to produce a byproduct of ethylene glycol besides high-purity carbonic ester, thereby meeting the carbon neutralization and carbon peak-reaching targets.
(2) And a heterogeneous alkaline catalysis technology is adopted in the reaction rectification and reaction bulkhead rectification of ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate/diethyl carbonate working sections, so that the problem of environmental solid waste of homogeneous catalysts sodium methoxide and sodium ethoxide is avoided.
(3) The energy-saving technology of reactive distillation, heat integration distillation, heat pump distillation and extraction bulkhead distillation systems is adopted in the process, and the energy consumption in the preparation process of the carbonic ester is obviously reduced.
Drawings
FIG. 1 is a process flow diagram for producing high purity ethylene carbonate. Wherein R101-a first reactor, R102-a second reactor, F101-a gas-liquid flash tank, a T101-ethylene oxide absorption tower, a T102-light component impurity removal tower, a T103-ethylene carbonate light removal tower and a T104-ethylene carbonate heavy removal tower.
FIG. 2 is a process flow diagram for producing high-purity dimethyl carbonate and by-producing ethylene glycol by using ethylene carbonate and methanol as raw materials. The device comprises a T201-ethylene carbonate alcoholysis reaction rectifying tower, a T202-dimethyl carbonate and methanol azeotrope separation high-pressure tower, a T203-dimethyl carbonate and methanol azeotrope separation low-pressure tower, a T204-dimethyl carbonate refining tower, a T205-ethylene carbonate recovery tower, a HI-SR-ethylene carbonate recovery tower condenser and a reaction rectifying tower side-line reboiler for heat integration.
FIG. 3 is a process flow chart for producing high-purity ethyl methyl carbonate and diethyl carbonate and by-producing methanol by using dimethyl carbonate and ethanol as raw materials. Wherein, R301-dimethyl carbonate and ethanol ester exchange reaction pre-reactor, R302-diethyl carbonate and dimethyl carbonate inverse disproportionation reactor, T301-dimethyl carbonate and ethanol ester exchange reaction rectifying tower, T302-dimethyl carbonate and methanol azeotrope separation extraction bulkhead rectifying tower, T303-dimethyl carbonate refining tower, T304-dimethyl carbonate recovery tower, T305-ethyl methyl carbonate/diethyl carbonate preliminary separation tower, T306-ethyl methyl carbonate lightness-removing tower, T307-ethyl methyl carbonate heaving tower, T308-diethyl carbonate lightness-removing tower and T309-diethyl carbonate heaving tower.
Detailed Description
The present invention will be described in more detail by the following embodiments with reference to the attached drawings, but the present invention is not limited by the scope of the claims of the present application.
The invention relates to a process system for producing a high-purity carbonate solvent for a lithium battery, which is divided into ethylene carbonate, dimethyl carbonate, methyl ethyl carbonate and diethyl carbonate units, and the specific implementation mode is as follows:
ethylene carbonate unit: raw materials of ethylene oxide and carbon dioxide enter a first reactor and are converted into ethylene carbonate under the catalysis of immobilized ionic liquid, and in order to improve the conversion rate of the raw materials of ethylene oxide, a part of stream which is discharged from the first reactor is recycled back to the first reactor, and a part of stream enters a second reactor. The reaction temperature of the reactor is 90-160 ℃, the reaction pressure is 2-6 MPa, the reaction product out of the second reactor enters a flash tank for primary separation of light components such as carbon dioxide and ethylene oxide and cycloaddition reaction product ethylene carbonate, the gas phase stream leaving the gas-liquid flash tank enters an absorption tower for absorption of ethylene oxide, wherein the absorbent adopts water, the liquid phase stream leaving the gas-liquid flash drum enters a light component impurity removing tower to further remove light impurity components such as carbon dioxide, ethylene oxide and the like, the product at the bottom of the tower enters a ethylene carbonate light component removing tower to be refined, the stream at the top of the light component removing tower is circularly returned to the light component impurity removing tower to further recover ethylene carbonate, the stream at the bottom of the light component removing tower enters a heavy component removing tower, wherein the stream at the top of the heavy component removal tower returns to the light component removal tower, high-purity ethylene carbonate product is extracted from the side line, and ethylene carbonate high-boiling residue is extracted from the tower kettle. Wherein the pressure at the top of the light component removal tower is 1-10 kPa, the temperature at the top of the tower is 100-150 ℃, and the energy consumption in the process is reduced by adopting indirect heat pump rectification; the tower top pressure of the de-heavy tower is 1-10 kPa, the tower top temperature is 100-150 ℃, and the energy consumption in the process is reduced by adopting indirect heat pump rectification.
Dimethyl carbonate unit: ethylene carbonate and methanol raw materials respectively enter an alcoholysis reaction rectifying tower above and below a reaction rectifying section, alcoholysis reaction of the ethylene carbonate and the methanol is carried out in the reaction rectifying tower, reaction products are dimethyl carbonate and ethylene glycol, the molar ratio of the ethylene carbonate and the methanol which are fed in the reaction is 1: 3-1: 6, the reaction rectifying section in the reaction rectifying tower is a catalytic filler filled with a solid catalyst, the pressure at the top of the reaction rectifying tower is 80-300 kPa, the temperature at the top of the reaction rectifying tower is 50-100 ℃, and the reflux ratio at the top of the reaction rectifying tower is 1-10; the top product of the reactive distillation tower is an azeotrope of dimethyl carbonate and methanol, and the bottom of the tower is a mixture of ethylene carbonate and ethylene glycol. The azeotrope of dimethyl carbonate and methanol is fed into high pressure tower and low pressure tower for pressure varying rectification to separate the azeotrope of dimethyl carbonate and methanol. The dimethyl carbonate crude product is extracted from the tower bottom of the high-pressure tower and enters a dimethyl carbonate refining tower, methanol is extracted from the tower bottom of the low-pressure tower and circulates to a reaction rectifying tower, the low-pressure tower adopts a heat pump rectifying mode to save energy, the high-purity dimethyl carbonate product is extracted from the side line of the dimethyl carbonate refining tower, and the azeotropic mixture of the methanol and the dimethyl carbonate is extracted from the tower top of the dimethyl carbonate refining tower and returns to the high-pressure tower for recovery. The method comprises the steps of enabling a tower kettle of a ethylene carbonate alcoholysis reaction rectifying tower to be a mixture of ethylene carbonate and ethylene glycol, enabling the mixture to enter an ethylene carbonate recovery tower to separate the ethylene carbonate and the ethylene glycol, wherein a byproduct ethylene glycol is obtained at the tower top, enabling the ethylene carbonate at the tower kettle to circularly return to the reaction rectifying tower, enabling the pressure at the tower top of the ethylene carbonate recovery tower to be 10-50 kPa, enabling the temperature at the tower top to be 110-180 ℃ and enabling the reflux ratio to be 1-10. Partial heat integration is carried out between the condenser of the ethylene carbonate recovery tower and the side line reboiler of the alcoholysis reaction rectifying tower.
Ethyl methyl carbonate, diethyl carbonate unit: dimethyl carbonate and ethanol enter a pre-reactor to perform ester exchange pre-reaction, the reaction pressure of the pre-reactor is 0.3-0.5 MPa, the residence time of the pre-reactor is 0.1-1 hr, and the feeding molar ratio of dimethyl carbonate to methanol in the feeding material of the pre-reactor is 0.8: 1-2: 1. The reaction product of the pre-reactor enters reactive distillation for further ester exchange reaction and is reactedThe reaction and separation are carried out in a rectifying tower, the reactive rectifying tower is divided into a public rectifying section, a reactive rectifying section and a public stripping section, the pressure of the reactive rectifying tower is 50-200 kPa, the temperature of the top of the reactive rectifying tower is 60-100 ℃, and the reflux ratio of the reactive rectifying tower is 2-8. The heterogeneous catalyst in the pre-reactor and the reaction rectifying tower is preferably alkali metal oxide MgO/HZSM-5, strong acid type ion exchange resin Lewatit K1221, Nafion SAC-13, modified K coated by polyethylene glycol 2 CO 3 . The top of the reaction rectifying tower is an azeotrope of dimethyl carbonate and methanol, the azeotrope of dimethyl carbonate and methanol enters an extraction bulkhead rectifying tower to separate the dimethyl carbonate from the methanol, wherein an extracting agent adopts aniline, sulfolane and N-methyl pyrrolidone, the methanol is taken out from the top of the tower at the feeding side of the extraction bulkhead rectifying tower, the mass fraction of the methanol is 99.99%, the dimethyl carbonate is taken out from the top of the tower at the other side, the mass fraction of the dimethyl carbonate is 99.5%, and the extracting agent extracted from the bottom of the tower is recycled and supplemented; the operating pressure of the extraction bulkhead rectifying tower is 80-150 kPa, and the operating temperatures of the tops of the two sides of the tower are 60-70 ℃ and 80-100 ℃ respectively. In order to reduce the energy consumption of the extraction bulkhead rectification process, the feeding is divided into three branch streams to exchange heat with the streams of the extraction bulkhead rectification tower top and the tower bottom product, the steam recompression is adopted at the tower top of the methanol product to heat the first branch feeding branch, the steam at the tower top of the dimethyl carbonate product side preheats the feeding of the second branch, and the extraction agent stream is returned from the tower bottom of the extraction bulkhead rectification tower to preheat the third branch feeding stream.
The method comprises the following steps of enabling a tower kettle of a rectifying tower for transesterification reaction of dimethyl carbonate and ethanol to be a mixture of dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate, enabling the mixture to enter a dimethyl carbonate recovery tower to recover dimethyl carbonate serving as a raw material, enabling a product at the top of a dimethyl carbonate tower to return to a pre-reactor, enabling the product at the tower kettle of the dimethyl carbonate recovery tower to enter a separation tower of ethyl methyl carbonate and diethyl carbonate to separate ethyl methyl carbonate and diethyl carbonate, enabling the operating pressure of the dimethyl carbonate recovery tower to be 20-60 kPa, enabling the temperature at the top of the dimethyl carbonate tower to be 40-60 ℃, enabling the temperature at the tower kettle to be 60-100 ℃ and enabling the reflux ratio to be 1-4. The top product stream of the methyl ethyl carbonate and diethyl carbonate separation tower is a crude methyl ethyl carbonate product, and after entering a subsequent methyl ethyl carbonate lightness-removing tower and a methyl ethyl carbonate weight-removing tower for further separation and purification, a high-purity methyl ethyl carbonate product is collected from the side of methyl ethyl carbonate; the diethyl carbonate crude product is fed into a subsequent diethyl carbonate lightness-removing tower and a diethyl carbonate heaving tower for further rectification and purification, and the high-purity diethyl carbonate product is extracted from the side line of the diethyl carbonate heaving tower. The pressure of the methyl ethyl carbonate and diethyl carbonate separation tower is 80-150 kPa, the temperature of the top of the tower is 100-120 ℃, the temperature of the bottom of the tower is 115-130 ℃, and the reflux ratio is 1-3. The pressure of the methyl ethyl carbonate lightness-removing tower and the methyl ethyl carbonate heaving tower is 20-60 kPa, the temperature of the top of the tower is 65-70 ℃, the operation temperature of the tower kettle is 70-75 ℃, the reflux ratio of the methyl ethyl carbonate lightness-removing tower is 30-60, the reflux ratio of the methyl ethyl carbonate heaving tower is 30-60, and the reflux ratio of the methyl ethyl carbonate heaving tower is 90-150. The pressure of a diethyl carbonate lightness-removing tower and a diethyl carbonate weight-removing tower is 20-60 kPa, the temperature of the top of the tower is 80-85 ℃, the temperature of a tower kettle is 85-95 ℃, the reflux ratio of the diethyl carbonate lightness-removing tower is 20-50, the reflux ratio of the diethyl carbonate weight-removing tower is 40-80, in order to reduce the energy consumption in the separation and purification process of ethyl methyl carbonate and diethyl carbonate, a condenser of a primary separation tower of ethyl methyl carbonate and diethyl carbonate and a reboiler of a dimethyl carbonate recovery tower are subjected to heat integration, and the ethyl methyl carbonate lightness-removing tower and the ethyl methyl carbonate weight-removing tower are rectified by an indirect heat pump.
Diethyl carbonate and dimethyl carbonate inverse disproportionation unit: dimethyl carbonate and diethyl carbonate can be further used for generating ethyl methyl carbonate through an anti-disproportionation reactor, the feeding molar ratio of diethyl carbonate to dimethyl carbonate is 0.8: 1-1.2: 1, the reaction pressure is 400-600 kPa, the temperature of the reactor is 100-150 ℃, the reaction residence time is 0.8-2 hr, and the conversion rate of dimethyl carbonate at the outlet of the anti-disproportionation reactor is 40-65%. The heterogeneous catalyst filled in the anti-disproportionation reactor is an alkali metal oxide, preferably magnesium-based substituted mesoporous aluminum phosphate (MgAPO).
Example 1
In the invention, the feed flow rate of the raw material ethylene oxide is 6000kg/hr, the mass ratio of the raw material ethylene oxide to the original feed of carbon dioxide is 1: 1.05, the flow rate of the circulating stream is 28700kg/hr, and the epoxy enters the first reactorEthane and CO 2 The mass ratio of the ethylene carbonate to the ethylene oxide is 1: 1.08, immobilized ionic liquid is adopted in a fixed bed reactor, wherein the ionic liquid adopts quaternary ammonium salt, the carrier adopts SBA-16 molecular sieve, the pressure of the reactor is 150 ℃, the reaction pressure is 5MPa, the flow rate of ethylene oxide in the material flow at the outlet of the first reactor is 6313kg/hr, the flow rate of ethylene oxide is 2842kg/hr, the flow rate of carbon dioxide is 3145kg/hr, the flow rate of ethylene carbonate after passing through the second reactor is 11966kg/hr, the flow rate of carbon dioxide is 320kg/hr, the flow rate of ethylene oxide is 14kg/hr, the mass fraction of ethylene carbonate after passing through a gas-liquid flash unit is 99.9%, the flow rate of impurities at the top of a carbon dioxide and ethylene oxide light impurity removal tower is 5kg/hr, the flow rate of a stream returned from a subsequent ethylene carbonate light impurity removal tower is 200kg/hr, and the flow rate of products at the bottom of the light impurity removal tower is 12160kg/hr, and (2) the ethylene carbonate enters an ethylene carbonate lightness-removing tower to remove light components, the flow rate of a product at the top of the ethylene carbonate lightness-removing tower is 200kg/hr, the flow rate of a product at the bottom of the ethylene carbonate lightness-removing tower is 12160kg/hr, the flow rate at the top of the ethylene carbonate heavy component removing tower is 200kg/hr, the flow rate of the product at the bottom of the tower is 10kg/hr, 99.99 percent of ethylene carbonate products are extracted from a side line, and the flow rate is 19150 kg/hr.
Example 2
The original feeding molar ratio of the ethylene carbonate to the methanol is 1: 2.05, the feeding molar ratio of the ethylene carbonate to the methanol entering a reaction rectifying tower is 1: 3.6, the reaction rectifying tower is divided into a public rectifying section, a reaction rectifying section and a public stripping section, the number of the common rectifying section tower plates is 3, the number of the reaction rectifying section tower plates is 25, the number of the public stripping section tower plates is 10, and the reaction rectifying section is filled with catalytic fillers, wherein the filled catalysts are strong-base quaternary ammonium ion exchange resins (Amberlyst A-26(OH)), the reflux ratio of the reaction rectifying tower is 2.5, the tower jacking pressure of the reaction rectifying tower is 0.1MPa, and the single-pass conversion rate of the ethylene carbonate in the reaction rectifying tower is 95%. The tower top of the reactive distillation tower is an azeotrope of dimethyl carbonate and methanol, wherein the mass fraction of the methanol is 71 percent, the mass fraction of the dimethyl carbonate is 29 percent, the azeotrope enters a high-pressure tower, the operating pressure of the high-pressure tower is 0.9MPa, the reflux ratio is 2, the tower top temperature is 132 ℃, the total tower plate number of the high-pressure tower is 20, the feeding position is at the 6 th tower plate, the mass fraction of the methanol in a tower top product is 83 percent, the mass fraction of the dimethyl carbonate is 17 percent, the tower top product enters a low-pressure tower, and the dimethyl carbonate with the mass fraction of 99.5 percent is extracted from a tower bottom and enters a subsequent dimethyl carbonate refining tower for further refining. The operating pressure of the low-pressure tower is 0.1MPa, the reflux ratio is 2.5, the temperature at the top of the tower is 64 ℃, the number of tower plates of the low-pressure tower is 27, the feeding position is the 8 th tower plate, and the azeotrope of dimethyl carbonate and methanol at the top of the tower returns to the high-pressure tower. The operating pressure of the dimethyl carbonate refining tower is 0.1MPa, the reflux ratio is 62, the total number of tower plates is 40, the feeding position is 20, the side line extraction position is 10, and the mass fraction of the side line extraction dimethyl carbonate is 99.99%.
Example 3
The initial feeding ratio of the dimethyl carbonate to the ethanol is 1: 1.15, the initial feeding ratio of the dimethyl carbonate to the ethanol entering the pre-reactor after the dimethyl carbonate circulating stream is calculated to be 1: 1.6, the pressure of the pre-reactor is 0.4Mpa, the residence time of reaction raw materials in the pre-reactor is 0.6hr, the operating temperature of the pre-reactor is 105 ℃, the reaction product of the pre-reactor enters a reaction rectifying tower, the number of tower plates of a public rectifying section of the reaction residence tower is 40, the number of tower plates of a reaction rectifying section is 30, the number of tower plates of a public stripping section is 15, the reaction rectifying section is filled with catalytic filler, the catalyst filled in the catalytic filler and the pre-reactor are alkali metal oxide MgO/HZSM-5, the operating pressure of the reaction rectifying tower is 0.1MPa, the operating temperature of the top of the reaction rectifying tower is 63 ℃, the temperature of the bottom of the reaction rectifying tower is 105 ℃, the operating reflux ratio is 3.5, and the product at the top is an azeotrope of the dimethyl carbonate and the methanol, wherein the mass fraction of the methanol is 0.7, the tower bottom is a mixture of dimethyl carbonate, methyl ethyl carbonate and diethyl carbonate, and the mass fraction is 0.32: 0.57: 0.11. The product stream at the top of the reactive distillation column enters an extraction bulkhead distillation column to separate dimethyl carbonate from methanol, the operating pressure of the extraction bulkhead distillation column is 0.1MPa, the temperature at the top of the feed side column is 64.5 ℃, the reflux ratio is 0.4, the temperature at the top of the dimethyl carbonate product side column is 90.2 ℃, the reflux ratio is 0.9, the operating temperature at the bottom of the column is 195 ℃, the extractant adopts aniline, and the structural parameters of the extraction bulkhead distillation column are as follows: the number of trays on the feed side of the partition board is 40, the number of trays on the discharge side of dimethyl carbonate is 40, the number of trays on the extraction agent recovery section is 10, the feed position of the extraction agent aniline on the feed side of the partition board is the 4 th tray, the feed position of dimethyl carbonate and methanol azeotrope is 30, and the fraction of the feed side of the gas phase partition board rising on the extraction agent recovery section is 0.7. Dimethyl carbonate and methanol azeotrope are divided into three branches for preheating, the preheating quantity fraction provided by the methanol product, the dimethyl carbonate product and the circulating extracting agent to the three branches is 0.1: 0.26: 0.64, the compression ratio of a compressor is 1.6 when the top of the methanol product adopts steam recompression to feed and preheat, and the temperature of dimethyl carbonate and methanol azeotrope entering an extraction bulkhead rectifying tower is 69 ℃. The mass fraction of the methanol product extracted from the top of the rectifying feed side of the extraction partition wall is 99.99%, the mass fraction of the dimethyl carbonate extracted from the dimethyl carbonate side is 99.5%, and the mass fraction of the extractant aniline extracted from the tower bottom is 99.999% for recycling. In order to obtain high-purity dimethyl carbonate for recycling, dimethyl carbonate extracted by the extraction bulkhead rectifying tower enters a dimethyl carbonate refining tower, an azeotrope of dimethyl carbonate and methanol at the tower top returns to the extraction bulkhead for rectification, a high-boiling-point substance of dimethyl carbonate and an extracting agent is extracted at the tower bottom, and 99.95% of dimethyl carbonate in mass fraction is recycled to the pre-reactor for use after being extracted from the side line. The operating pressure of the dimethyl carbonate refining tower is 0.1Mpa, the operating reflux ratio is 60, the temperature of the top of the tower is 63.5 ℃, the temperature of the bottom of the tower is 92.5 ℃, the number of dimethyl carbonate tower plates is 40, the feeding position is 20, and the lateral line extraction position is 10.
Dimethyl carbonate, ethyl methyl carbonate and diethyl carbonate discharged from the tower bottom of the reaction rectifying tower enter a dimethyl carbonate recovery tower, the operating pressure of the dimethyl carbonate recovery tower is 30kPa, the reflux ratio is 8, the temperature of a condensed liquid at the top of the tower is 50 ℃, the temperature of the tower bottom is 77 ℃, the number of tower plates of the dimethyl carbonate recovery tower is 50, the feeding position is 20, the purity of dimethyl carbonate extracted from the top of the tower is 99.5 percent, the dimethyl carbonate is circularly returned to a pre-reactor, a mixture of ethyl methyl carbonate and diethyl carbonate is extracted from the tower bottom, the mass fraction of the ethyl methyl carbonate is 84 percent, and heat integration is carried out between a reboiler of the dimethyl carbonate and a condenser of a subsequent ethyl methyl carbonate/diethyl carbonate separation tower. The mixture of ethyl methyl carbonate and diethyl carbonate enters a ethyl methyl carbonate/diethyl carbonate separation tower for primary separation, the operation pressure of the ethyl methyl carbonate/diethyl carbonate primary separation tower is 0.1Mpa, the reflux ratio is 2.5, the temperature at the top of the tower is 107 ℃, the temperature at the bottom of the tower is 130 ℃, the number of tower plates of the ethyl methyl carbonate/diethyl carbonate primary separation tower is 50, the feeding position is 30, the top of the tower is ethyl methyl carbonate with the content of 99.9 percent, and the bottom of the tower is diethyl carbonate with the content of 99.9 percent. The product at the top of the primary separation tower enters a methyl ethyl carbonate lightness-removing tower to remove light dimethyl carbonate, the operating pressure of the methyl ethyl carbonate light component removing tower is 30kPa, the reflux ratio is 50, the temperature at the top of the tower is 68 ℃, the temperature at the bottom of the tower is 72 ℃, the number of tower plates of the methyl ethyl carbonate light component removing tower is 50, the feeding position is 20, the product at the top of the lightness-removing tower returns to a dimethyl carbonate recovery tower, the product at the bottom of the tower enters a methyl ethyl carbonate heaving tower to remove heavy diethyl carbonate, the operating pressure of the methyl ethyl carbonate heaving tower is 25kPa, the reflux ratio is 140, the temperature at the top of the tower is 68 ℃, the temperature at the bottom of the tower is 73 ℃, the number of tower plates of the methyl ethyl carbonate heaving tower is 50, the feeding position is 30, the side-draw position is 20, the stream at the top of the tower is the methyl ethyl carbonate light component and returns to the methyl ethyl carbonate lightness-removing tower, the heavy methyl ethyl carbonate/diethyl carbonate primary separation tower, in order to reduce the energy consumption in the process, an indirect heat pump rectification is adopted in the ethyl methyl carbonate light removal tower and the ethyl methyl carbonate heavy removal tower, and the compression ratio of a compressor is 1.5. Feeding a product at the tower bottom of a diethyl carbonate/diethyl carbonate primary separation tower into a diethyl carbonate lightness-removing tower to remove light components of ethyl methyl carbonate, wherein the operation pressure of the diethyl carbonate lightness-removing tower is 30kPa, the operation reflux ratio is 30, the temperature of a condensed liquid at the tower top is 50 ℃, the temperature of the tower bottom is 93 ℃, the number of tower plates of the diethyl carbonate lightness-removing tower is 50, the feeding position is 20, the product at the tower top is a diethyl carbonate light component returned to the ethyl methyl carbonate/diethyl carbonate primary separation tower, the product at the tower bottom enters a diethyl carbonate de-weighting tower, the operation pressure of the diethyl carbonate de-weighting tower is 30kPa, the operation reflux ratio is 50, the temperature of the condensed liquid at the tower top is 50 ℃, the temperature of the tower bottom is 93 ℃, the number of tower plates of the diethyl carbonate de-weighting tower is 50, the feeding position is 30, the product at the tower top of the diethyl carbonate de-weighting tower is circulated to the ethyl methyl carbonate/diethyl carbonate crude separation tower, 99.99% of diethyl carbonate is extracted from a lateral line, the withdrawal position is the 20 th tray.
In the process of the anti-disproportionation reactor, the feeding molar ratio of dimethyl carbonate to diethyl carbonate is 1: 1, a catalyst filled in the anti-disproportionation reactor is mesoporous aluminum phosphate (MgAPO), the operating pressure of the anti-disproportionation reactor is 450kPa, the reaction temperature is 110 ℃, the material retention time in the anti-disproportionation reactor is 1.15hr, the conversion rate of dimethyl carbonate in the anti-disproportionation reactor is 60%, and the outlet material flow of the anti-disproportionation reactor is sent to the dimethyl carbonate, methyl ethyl carbonate and diethyl carbonate separation system for separation and purification.
The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the above described solution or modify it to an equivalent solution. Therefore, any simple modifications or equivalent substitutions made according to the technical solution of the present invention belong to the protection scope of the present invention.
Claims (10)
1. A process system for producing a high-purity carbonate solvent for a lithium battery is characterized in that three working sections are adopted for ethylene carbonate, dimethyl carbonate and ethyl methyl carbonate/diethyl carbonate, wherein the ethylene carbonate is obtained by taking ethylene oxide and carbon dioxide as raw materials through cycloaddition reaction and an ethylene carbonate refining unit; the dimethyl carbonate is prepared by taking ethylene carbonate and methanol as raw materials and performing alcoholysis reaction rectification and subsequent dimethyl carbonate refining processes, wherein ethylene glycol is a byproduct in the process, and unreacted ethylene carbonate and methanol are recycled after the subsequent separation and purification processes; the methyl ethyl carbonate and the diethyl carbonate are prepared by taking dimethyl carbonate and ethanol as raw materials, carrying out ester exchange reaction in a pre-reactor and a reaction rectifying tower and carrying out subsequent refining processes of the methyl ethyl carbonate and the diethyl carbonate, and the dimethyl carbonate is recycled after separation and purification processes.
2. The system for manufacturing a high purity carbonate solvent for lithium battery as claimed in claim 1, wherein the cycloaddition reaction of ethylene oxide is carried out in a two-stage reactor using a catalystThe agent is a heterogeneous catalyst, preferably SiO is used 2 、TiO 2 SBA-16 molecular sieve supported quaternary ammonium salt or imidazole ionic liquid; the alcoholysis reaction of ethylene carbonate is carried out in a reaction rectifying tower, and the catalyst filled in the catalytic packing is preferably strong-base quaternary ammonium ion exchange resin (amberlystA-26(OH)) with hydroxide counter ions and ZrO 2 -Al 2 O 3 (ii) a The ester exchange reaction of dimethyl carbonate is carried out in a reaction rectifying tower, and the catalyst filled in the catalytic filler is preferably alkali metal oxide MgO/HZSM-5, modified K coated by polyethylene glycol 2 CO 3 。
3. The system of claim 1, wherein the alcoholysis reaction of ethylene carbonate and methanol is carried out in a reactive distillation column, wherein the recovery section of dimethyl carbonate is implemented by a combination of a high-pressure column and a low-pressure column, and the low-pressure column is directly rectified by a heat pump to reduce energy consumption in the process.
4. The system for producing a high-purity carbonate solvent for a lithium battery as claimed in claim 1, wherein a side-line heat integration is performed between the rectification column for alcoholysis reaction of ethylene carbonate and methanol and the ethylene carbonate recovery column in the dimethyl carbonate production section.
5. The system for manufacturing a high purity carbonate solvent for lithium battery as claimed in claim 1, wherein the separation section of the azeotrope of dimethyl carbonate and methanol in the section of preparing ethyl methyl carbonate and diethyl carbonate by transesterification of dimethyl carbonate and ethanol is implemented in an extractive bulkhead rectification column, which is composed of three sections, namely a bulkhead feed column section, a bulkhead dimethyl carbonate product column section and an extractant recovery column section, wherein the extractant used in the bulkhead rectification column is preferably aniline, N-methyl pyrrolidone, sulfolane; and the extraction bulkhead rectifying tower respectively adopts the separator feeding side tower top steam, the separator dimethyl carbonate side tower top steam and the extractant circulating stream to preheat the feeding of the dimethyl carbonate and methanol azeotrope.
6. The process system for producing a high-purity carbonate solvent for a lithium battery as claimed in claim 1, wherein the process of separating and purifying the ethyl methyl carbonate in the production process of ethyl methyl carbonate and diethyl carbonate adopts indirect heat pump rectification to save energy.
7. The system for manufacturing a high purity carbonate solvent for lithium battery as claimed in claim 1, wherein the high purity ethylene carbonate, dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate are taken out from the ethylene carbonate de-weighting tower, the dimethyl carbonate refining tower, the ethyl methyl carbonate de-weighting tower and the diethyl carbonate de-weighting tower respectively.
8. The process system for producing a high purity carbonate solvent for lithium batteries as claimed in claim 1, wherein the feeding molar ratio of ethylene oxide to carbon dioxide in the feeding of the ethylene carbonate section is 1: 1 to 1: 2; the feeding mol ratio of the ethylene carbonate to the methanol in the feeding in the dimethyl carbonate working section is 1: 1-1: 4; the feeding mol ratio of dimethyl carbonate to ethanol in the feeding in the working sections of ethyl methyl carbonate and diethyl carbonate is 1: 1-1.5: 1.
9. The system of claim 1, wherein the dimethyl carbonate and the diethyl carbonate are converted into ethyl methyl carbonate by an inverse disproportionation reactor, wherein the molar ratio of dimethyl carbonate to diethyl carbonate in the feed of the inverse disproportionation reactor is 0.9: 1-1.1: 1.
10. The process system for producing the high-purity carbonate solvent for the lithium battery as claimed in claim 1, wherein the pressure of the first reactor and the second reactor in the ethylene carbonate section ring addition reactor is 3-6 Mpa; the pressure of the alcoholysis reaction rectifying tower in the dimethyl carbonate working section is 0.1-0.15 MPa; the pressure of a pre-reactor in the working sections of ethyl methyl carbonate and diethyl carbonate is 0.3 to 0.5Mpa, and the pressure of a rectification tower of the ester exchange reaction is 0.1 to 0.15 Mpa; the pressure of the reverse disproportionation reactor is 0.3 MPa-0.6 MPa.
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