CN114716402A - High-purity vinylene carbonate and production method and application thereof - Google Patents
High-purity vinylene carbonate and production method and application thereof Download PDFInfo
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Abstract
The invention relates to the technical field of organic synthesis, and particularly relates to high-purity vinylene carbonate and a production method and application thereof. The production method comprises a chlorination reaction step, a dechlorination reaction step and a purification step, wherein the chlorination reaction comprises the following steps: performing chlorination reaction under ultraviolet irradiation by using ethylene carbonate as a raw material and chlorine as a chlorinating agent, wherein the molar ratio of the chlorine to the ethylene carbonate is 0.4-0.6: 2-3. The invention can obviously reduce the energy consumption by reducing the proportion of chlorine to ethylene carbonate.
Description
Technical Field
The invention relates to the technical field of organic synthesis, and particularly relates to high-purity vinylene carbonate and a production method and application thereof.
Background
In recent years, new energy automobiles and high-performance batteries are rapidly developed, and the rapid development of the vinylene carbonate industry is driven.
Vinylene carbonate (VC for short) is an important organic intermediate, and has the following excellent properties: the performance of the battery is effectively improved, the compatibility of the positive electrode and the negative electrode and the stability of the negative electrode are improved, the capacity of the positive electrode is improved, and the cycle life of the lithium ion battery is prolonged. Vinylene carbonate is mainly used as an additive and a surface coating component of low-temperature electrolyte of a lithium battery, can also be used for immobilized enzyme and used as a monomer of vinylene carbonate polymers such as poly (ethylene carbonate), and is widely applied to the fields of batteries, bioengineering, food processing, clinical medicine, organic synthesis and the like.
The industrial production of vinylene carbonate mainly comprises two steps: the first step is to generate monochloroethylene carbonate by chlorination reaction of vinylene carbonate (taking chlorine as a chlorinating agent and being carried out under ultraviolet irradiation), and the second step is to generate vinylene carbonate by removing chlorine atoms in monochloroethylene carbonate by dehalogenating agents such as triethylamine, ammonia gas, alkali metal hydroxide and the like. The vinylene carbonate synthesized by the method has the advantages of mild conditions, simple and convenient operation and easy control, and is a production method generally adopted in the industry at present.
However, the method for producing high-purity vinylene carbonate needs to carry out three-stage rectification treatment on a vinylene carbonate crude product with the purity of about 60% (the first-stage distillation is carried out in a desolventizing tower, the purity of the product is about 97% after the first-stage distillation treatment, the second-stage distillation is carried out in a lightness-removing tower or a rough distillation tower, the purity of the product is about 98% after the second-stage distillation treatment, the purity of the product is about 98.5% after the third-stage rectification treatment in a rectifying tower, the energy consumption is high (about 3600kg steam/t product), the purity of the obtained product is only 98.5%, the application requirement in the electronic field cannot be met, in order to further improve the purity of the product, two times of rectification treatment are needed to improve the purity of the product to about 99.5%, and the energy consumption is further increased (about 8000kg steam/t product), resulting in poor economics of scale-up production processes.
Disclosure of Invention
In view of this, the present invention aims to provide a high-purity vinylene carbonate, a production method thereof and an application thereof, so as to reduce the energy consumption for producing vinylene carbonate.
In a first aspect, the present invention provides a process for producing vinylene carbonate, comprising a chlorination reaction step, a dechlorination reaction step and a purification step, the chlorination reaction comprising: performing chlorination reaction under the irradiation of ultraviolet light by using ethylene carbonate as a raw material and chlorine as a chlorinating agent, wherein the molar ratio of the chlorine to the ethylene carbonate is 0.4-0.6: 2-3.
Optionally, the temperature of the chlorination reaction is 60-70 ℃, preferably 65-70 ℃; the time of the chlorination reaction is 1 to 2 hours, preferably 1.2 to 2 hours.
Optionally, the production method further comprises the steps of: and respectively using water and alkali liquor to recover hydrogen chloride gas and chlorine gas in the liquid after the chlorination reaction.
Optionally, the dechlorination reaction comprises: and adding a removing agent and a polymerization inhibitor into the chlorination reaction liquid to perform dechlorination.
Optionally, the removal agent is triethylamine.
Optionally, the mole ratio of the removing agent to the chloroethylene carbonate contained in the chlorination reaction liquid is 1: 1-1: 1.5, preferably 1: 2-1: 1.5.
optionally, the polymerization inhibitor is butyl-p-cresol (BHT for short).
Optionally, the mass ratio of the polymerization inhibitor to the chloroethylene carbonate contained in the chlorination reaction liquid is 0.1: 100-0.5: 100, preferably 0.2: 100-0.5: 100.
optionally, the temperature of the dechlorination reaction is 60-70 ℃, preferably 65-70 ℃; the dechlorination time is 4-5h, preferably 4.5-5 h.
Optionally, the molar ratio of the vinylene carbonate to the chloroethylene carbonate contained in the chlorination reaction liquid is 1: 1-1: 1.5, preferably 1: 2-1: 1.5.
optionally, the purifying comprises melt crystallization.
Alternatively, a falling film crystallizer is used for melt crystallization.
In another aspect, the present invention also provides vinylene carbonate produced by the production method as described above.
In still another aspect, the invention also provides the application of the vinylene carbonate prepared by the production method in the lithium ion battery.
As mentioned above, the high-purity vinylene carbonate and the preparation method and the application thereof have the following beneficial effects:
(1) the invention can obviously reduce the energy consumption by reducing the proportion of chlorine to ethylene carbonate.
(2) The production method of the invention can carry out continuous production on the whole, thereby saving time; by-products generated in each step of reaction are timely discharged out of the system, further complication of the reaction and the intermediate process is avoided, and the yield and the purity of the product are improved; the method has the advantages of avoiding the residue of reactants, reducing separation procedures, reducing the complexity and cost of production and controlling key technical indexes such as moisture and the like to a lower level.
(3) The vinylene carbonate has high purity and can be used in the fields of lithium ion batteries and the like.
Drawings
FIG. 1 is a schematic configuration diagram of a production system of example 1;
fig. 2 is a schematic configuration diagram of a production system of embodiment 2.
Reference numerals
In the attached drawings, a primary reaction unit-1, a first photolysis reaction tower-11, a second photolysis reaction tower-12, a deacidification tower-13, a secondary reaction unit-2, a first reaction kettle-21, a second reaction kettle-22, a washing tower-23, a purification unit-3, a desolventizing tower-31, a crude distillation tower-32, 33-falling film crystallizer, a byproduct recovery unit-4, a water washing tower-41, an alkali absorption tower-42, a triethylamine recovery unit-5, a drying device-51, a dissolving tank-52, a filtering device-53, a reaction tank-54 and a centrifugal device-55.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
The invention provides a method for producing vinylene carbonate, which comprises a chlorination reaction step, a dechlorination reaction step and a purification step, and specifically comprises the following steps:
taking ethylene carbonate as a raw material, taking chlorine as a chlorinating agent, carrying out chlorination reaction for 1-2h under ultraviolet irradiation at the temperature of 60-70 ℃, wherein the molar ratio of the chlorine to the ethylene carbonate is 0.4-0.6: 2-3, respectively recovering hydrogen chloride gas and chlorine gas in the liquid after the chlorination reaction by using water and alkali liquor;
adding a removing agent triethylamine and a polymerization inhibitor butyl-p-cresol into the chlorination reaction liquid, and carrying out dechlorination reaction for 4-5h at the temperature of 60-70 ℃, wherein the molar ratio of the removing agent to chlorinated ethylene carbonate contained in the chlorination reaction liquid is 1: 1-1: 1.5, the mass ratio of the polymerization inhibitor to the chloroethylene carbonate contained in the chlorination reaction liquid is 0.1: 100-0.5: 100, respectively;
the purification comprises melt crystallization, which is carried out using a falling film crystallizer.
The present invention will be described in detail below with reference to specific exemplary embodiments. It is also to be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the invention, and that insubstantial modifications and adaptations of the invention as described above will now occur to those skilled in the art. The specific process parameters and the like of the following examples are also only one example of suitable ranges, i.e., those skilled in the art can select the appropriate ranges through the description herein, and are not limited to the specific values exemplified below.
In the invention, the content of dichloroethylene carbonate is detected according to Q1327 HG003-2019 chloroethylene carbonate;
in the invention, the purity is detected according to GB/T27801-2011 vinylene carbonate;
in the invention, the energy consumption is calculated according to the general rule of comprehensive energy consumption calculation of GB/T2589 and 2020.
Example 1
Vinylene carbonate is produced by using a production system as shown in FIG. 1, which comprises a primary reaction unit 1, a secondary reaction unit 2, a purification unit 3, a byproduct recovery unit 4 and a triethylamine recovery unit 5.
First-order reaction unit 1 includes first photolysis reaction tower 11, second photolysis reaction tower 12 and deacidification tower 13, and first photolysis reaction tower 11 and second photolysis reaction tower 12 are provided with ultraviolet subassembly (not drawn) and temperature regulation subassembly (not drawn) as the container of chlorination in it as, and the ultraviolet subassembly is used for providing the ultraviolet condition for the chlorination, and the temperature regulation subassembly is used for controlling the temperature of chlorination. Photolysis towers are prior art and are not described in detail herein.
The first photolysis reaction tower 11 and the second photolysis reaction tower 12 are provided with a vinyl carbonate feed inlet, an air inlet, a liquid outlet and an air outlet, raw material molten state vinyl carbonate (EC) can be fed into the first photolysis reaction tower 11 and the second photolysis reaction tower 12 through the vinyl carbonate feed inlet, and chlorine can be introduced into the photolysis reaction tower through the air inlet. The multistage photolysis reaction tower is arranged, so that the chlorine can be completely reacted, and the yield is improved.
The upper part of the deacidification tower 13 is communicated with a discharge hole of the second photolysis reaction tower 12. The upper portion of deacidification tower 13 is provided with gas outlet, and its lower part is provided with the nitrogen gas import, can let in nitrogen gas in deacidification tower 13 through the nitrogen gas import, and then get rid of gaseous such as chlorine, hydrogen chloride in the obtained liquid of chlorination, improve the purity of final product, can also reduce the energy consumption of follow-up purification process simultaneously. The deacidification tower is prior art and is not described in detail herein.
The secondary reaction unit 2 includes a first reaction tank 21, a second reaction tank 22, and a washing tower 23.
The first reaction vessel 21 and the second reaction vessel 22 are dechlorination reaction vessels, and both are provided with a feed inlet, a discharge outlet and a temperature regulation assembly (not shown). The feed inlet of the first reaction kettle 21 is communicated with the lower part of the deacidification tower 13, and the discharge outlet of the first reaction kettle is communicated with the feed inlet of the second reaction kettle 23. The raw material removing agent triethylamine, the polymerization inhibitor butyl-p-cresol (BHT) and the solvent vinylene carbonate can be fed into the reaction kettle through the feeding hole, the chlorinated reaction liquid processed by the deacidification tower 13 can be fed into the first reaction kettle 21 through the feeding hole, and the material reacted by the first reaction kettle 21 can be fed into the second reaction kettle 22 through the feeding hole. The temperature regulating component is used for regulating the temperature of dechlorination reaction. Through setting up multistage reation kettle, can make the dechlorination more thorough, improve the yield. The reaction kettle is the prior art and is not described in detail here.
The first end of the washing tower 23 is communicated with a discharge hole of the second reaction kettle 22, and the first end of the washing tower is also communicated with a dimethyl carbonate liquid inlet pipeline. Dimethyl carbonate can be introduced into the washing tower 23 through a dimethyl carbonate liquid inlet pipeline, vinylene carbonate can be dissolved by the dimethyl carbonate, triethylamine cannot be dissolved, triethylamine can be recycled, and the utilization rate of the triethylamine is improved. The scrubber is prior art and will not be described further herein. The conveying assembly may be a conveyor belt, which is prior art and will not be described herein.
The purification unit 3 comprises a desolventizing tower 31 and a falling film crystallizer 32 which are communicated, wherein the falling film crystallizer 32 is communicated with the lower part or the bottom of the desolventizing tower 31 through a circulating pump (not shown). The desolventizing tower and the falling film crystallizer are both in the prior art and are not described in detail herein. Impurities can be further removed through the desolventizing tower 31, the purity of the final product is improved, the purity of the final product can be improved through the falling film crystallizer 32, and the energy consumption is reduced. By communicating the falling film crystallizer 32 with the lower part or the bottom of the desolventizing tower 32 through the circulating pump, part of the vinylene carbonate which is not melted and crystallized can be distilled by the desolventizing tower 31 and then enter the falling film crystallizer 32 again for melting and crystallization, so that the yield is improved.
The byproduct recovery unit 4 includes a water absorption tower 41 and an alkali absorption tower 42, a first end of the water absorption tower 41 is communicated with the gas outlet of the first photolysis reaction tower 11, the gas outlet of the second photolysis reaction tower 12 and the gas outlet of the deacidification tower 13, and a second end is communicated with the alkali absorption tower 42. Water can be introduced into the water absorption tower 41 through a water inlet pipeline, and the water can dissolve the chlorinated reaction product hydrogen chloride to obtain hydrochloric acid and the water absorption tower 41. The alkali absorption tower 42 is provided with a waste gas outlet, which is provided with an alkali liquor inlet pipeline (not shown), through which a sodium hydroxide aqueous solution can be introduced into the alkali absorption tower 42, and the sodium hydroxide aqueous solution can react with chlorine gas which does not participate in the chlorination reaction to generate sodium hypochlorite.
The triethylamine recovery unit 5 comprises a drying device 51 and a dissolving tank 52 which are connected through a transmission assembly (not shown), the dissolving tank 52 is communicated with a filtering device 53, the filtering device 53 is provided with a liquid outlet, the liquid outlet is communicated with a reaction tank 54, the reaction tank 54 is communicated with a centrifugal device 55, the centrifugal device 55 is provided with a triethylamine outlet, and the triethylamine outlet is communicated with the feed inlets of the first reaction kettle 21 and/or the second reaction kettle 22. The conveying assembly may be a conveyor belt, which is prior art and will not be described herein.
The drying device 51 is connected to the second end of the washing column 24 via a transfer assembly (not shown) which is provided with a dimethyl carbonate (DMC) vent. The drying device 51 is used to dry the chlorotriethylamine salt solid washed by the washing tower 24 to remove a detergent dimethyl carbonate (DMC) attached to the surface thereof. The drying device 51 may be a forced air dryer, which is a prior art and will not be described herein.
The dissolving tank 52 is connected to a water inlet pipe (not shown), through which water can be introduced into the dissolving tank 52 to dissolve impurities such as flocculent organic matters attached to the solid surface of the chlorotetraethylamine salt, and the impurities are filtered and removed by a filter device 53 connected to the dissolving tank 52.
The reaction tank 54 is provided with a solid caustic soda inlet, through which sodium hydroxide can be fed into the reaction tank 54, so that the chlorotriethylamine salt entering the reaction tank 54 and the sodium hydroxide undergo a displacement reaction to generate triethylamine. Because the solubility of triethylamine in water is low, triethylamine can be separated by a centrifugal device 55 communicated with the reaction tank, and the separated triethylamine can be sent to the first reaction kettle 21 and/or the second reaction kettle 22 through a triethylamine outlet, so that the triethylamine can be recycled.
All the communication pipelines are provided with switch valves (not shown).
The vinylene carbonate is produced by adopting the production system shown in figure 1, and the specific steps are as follows:
ethylene carbonate heated to a molten state in advance is put into the first photolysis reaction tower 11 and the second photolysis reaction tower 12, and chlorine gas is introduced into the first photolysis reaction tower 11 and the second photolysis reaction tower 12 through the gas inlet; the molar ratio of the total chlorine gas to the total ethylene carbonate in the first photolysis reaction tower 11 and the second photolysis reaction tower 12 is 0.4: 2, the chlorine gas and the ethylene carbonate in the first photolysis reaction tower 11 respectively account for 2/3 of the total amount.
And opening the ultraviolet light assembly and the temperature regulating assembly, heating the ethylene carbonate in the first photolysis reaction tower 11 to 60 ℃, wherein the wavelength of the ultraviolet light is 365nm, and performing chlorination reaction on chlorine and the ethylene carbonate under the irradiation of the ultraviolet light.
After 1 hour, the on-off valve on the pipeline between the first photolysis reaction tower 11 and the second photolysis reaction tower 12 is opened, the ultraviolet light assembly and the temperature regulation assembly are opened, the ethylene carbonate in the second photolysis reaction tower 12 is heated to 60 ℃, and the wavelength of the ultraviolet light is 365 nm. Chlorine and ethylene carbonate are subjected to chlorination reaction under the irradiation of ultraviolet light. Because ethylene carbonate is excessive, the generation amount of dichloroethylene carbonate is very small, namely, the generation amount of high-boiling-point material dichloroethylene carbonate is reduced by reducing the ratio of chlorine gas to ethylene carbonate, and the energy consumption in the subsequent purification process is further obviously reduced.
After 1h, obtaining chlorination reaction liquid, opening a switch valve on a pipeline between an air outlet of the first photolysis reaction tower 11 and an air outlet of the second photolysis reaction tower 12 and a first end of the water absorption tower 41 and a switch valve on a pipeline between a second end of the water absorption tower 41 and the alkali absorption tower 42, introducing water into the water absorption tower 41, introducing a sodium hydroxide aqueous solution with the concentration of 30 wt% into the alkali absorption tower 42, dissolving a chlorination reaction product, namely hydrogen chloride gas, to obtain hydrochloric acid, and reacting the sodium hydroxide aqueous solution with chlorine which does not participate in chlorination reaction to generate sodium hypochlorite.
In this process, the gas outlet of the photolysis reaction tower 11 of the first photolysis reaction tower 11, the switching valve on the pipeline between the liquid outlet of the second photolysis reaction tower 12 and the deacidification tower 13 are opened, the switching valve on the pipeline between the deacidification tower 13 and the water absorption tower 41 is opened, nitrogen is introduced into the deacidification tower 13, the nitrogen entering the deacidification tower 13 from the lower part is in countercurrent contact with the liquid entering the deacidification tower 13 from the upper part, and then the chlorine and the hydrogen chloride in the liquid are discharged, so that a liquid phase crude product of the Chlorinated Ethylene Carbonate (CEC) is obtained. The chlorinated reaction liquid fed into the deacidification tower 13 had a content of ethylene dichlorocarbonate of 0.76 wt%.
Then, the on-off valve on the pipeline between the deacidification tower 13 and the first reaction kettle 21 is opened, and the removing agent triethylamine, the polymerization inhibitor butyl-p-cresol (BHT) and the solvent vinylene carbonate are fed into the first reaction kettle 21 and the second reaction kettle 22, wherein the molar ratio of the total amount of triethylamine in the first reaction kettle 21 and the second reaction kettle 22 to the total amount of high-purity chloroethylene carbonate (CEC) is 1: 1, the molar ratio of the total amount of the vinylene carbonate to the total amount of the high-purity chloroethylene carbonate (CEC) is 1: 1, the mass ratio of the total amount of butyl-p-cresol (BHT) to the total amount of high-purity Chlorinated Ethylene Carbonate (CEC) is 0.1: 100.
in the process, the temperature regulating assembly is opened, the materials in the first reaction kettle 21 are heated to 60 ℃, and high-purity chloroethylene carbonate (CEC) and triethylamine entering the first reaction kettle 21 are subjected to dechlorination reaction for 4 hours in the presence of vinylene carbonate to obtain a dechlorination reaction product (triethylamine salt containing chlorine).
And then, opening a switch valve on a pipeline between the first reaction kettle 21 and the second reaction kettle 22, enabling the obtained liquid to enter the second reaction kettle 22, in the process, opening a temperature regulating component to heat the materials in the second reaction kettle 23 to 60 ℃, and continuing dechlorination of the unreacted materials in the second reaction kettle 21 for 4 hours to obtain a dechlorination reaction product.
Then, a switch valve on a pipeline between the second reaction kettle 22 and the washing tower 23 is opened, and a detergent dimethyl carbonate is introduced into the washing tower 23, wherein the dimethyl carbonate can dissolve vinylene carbonate and cannot dissolve chlorotriethylamine salt, so that the chlorotriethylamine salt is removed, and the purity of a final product is improved.
Starting a transmission assembly between the washing tower 23 and the drying device 51, drying the chlorotetraethylamine salt solid attached with dimethyl carbonate (DMC) and flocculent organic matters by the drying device 51, removing the attached dimethyl carbonate (DMC), then starting the transmission assembly between the drying device 51 and the dissolving tank 52, introducing water into the dissolving tank 52, then opening a switch valve on a pipeline between the dissolving tank 52 and the filtering device 53, filtering the liquid mixture in the filtering device 53 to remove flocculent organic matters attached with the chlorotetraethylamine salt, then opening a switch valve on a pipeline between the filtering device 53 and the reaction tank 54, adding sodium hydroxide into the reaction tank 53, introducing the liquid containing the chlorotetraethylamine salt into the reaction tank 54, performing a displacement reaction with the sodium hydroxide to generate triethylamine, then opening a switch valve on a pipeline between the reaction tank 54 and the centrifugal device 55, and the mixed liquid enters a centrifugal device 55, is subjected to filtration treatment and then is separated to obtain triethylamine liquid, a switch valve on a pipeline between the centrifugal device 55 and the first reaction kettle 21 and/or the second reaction kettle 22 is opened, and the triethylamine liquid enters the first reaction kettle 21 and/or the second reaction kettle 22 through a triethylamine outlet to continuously participate in dechlorination reaction, so that the triethylamine is recycled.
And opening a switch valve on a pipeline between the washing tower 24 and the desolventizing tower 31, feeding the washed liquid into the desolventizing tower 31, and removing the detergent dimethyl carbonate (DMC) by distillation in the desolventizing tower 31. The temperature of the desolventizing treatment was 30 ℃ and the pressure was 7 kPa.
Subsequently, a pipeline between the desolventizing tower 31 and the falling film crystallizer 32 is opened, and the liquid (taking the handling capacity of 10kg as an example) treated by the desolventizing tower 31 enters the falling film crystallizer 32 for melt crystallization, wherein the melt crystallization comprises melting, sweating and crystallization steps, and specifically comprises the following steps:
s1: preheating equipment:
pouring 10kg of VC crystallization raw material to be treated with the purity of 97% (temperature is 30-35 ℃) into a raw material tank, starting a falling film crystallizer and circulating cooling and heating medium preheating equipment, and controlling the temperature of the circulating cooling and heating medium to be 18-24 ℃;
s2: pre-cooling materials: starting a crystallization circulating pump, conveying the VC crystallization raw material in the raw material tank to the falling film crystallizer for circulating conveyance, and controlling the flow of circulating material to be 0.2-0.6m3The pressure is 0.02-0.07MPa, the motor frequency is 13-18Hz, and the temperature of the circulating material is rapidly reduced to 19-23 ℃;
s3: carrying out first falling film crystallization:
and (3) a crystallization process: reducing the temperature of a circulating cooling and heating medium by 1-3 ℃ step by step at the speed of 0.1-2 ℃/min, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing the mother liquor to obtain 3kg of mother liquor, sampling to obtain the mother liquor with the purity of 91%, filling and storing the mother liquor, accumulating a certain amount of the mother liquor, directly crystallizing to obtain 1.7kg of recovery liquid and 1.3kg of residual liquid, wherein the product purity of the recovery liquid can reach about 98%, the recovery liquid can be crystallized and purified together with the VC crystallization raw material with the purity of 97% next time, and the residual liquid can be sent to a rectification unit;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 19-20 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the sweating liquid is discharged after the sweating is finished and weighed to obtain 0.5kg, the purity of the sweating liquid is 99.2% by sampling, and the sweating liquid can be filled, stored and added into the crystallization raw material with the next purity of 97%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 28-34 ℃ to melt a crystallization product, controlling the melting time for 30min, discharging and weighing a first-stage crystallization product after the melting is finished to obtain 6.5kg, and sampling to measure that the purity of the first-stage crystallization product is 99.4%;
s4: carrying out second falling film crystallization:
and (3) a crystallization process: sending 6.5kg of primary crystallization product with the purity of 99.4% into a falling film crystallizer for circulation, reducing the temperature of a circulating cooling and heating medium by 1-3 ℃ step by step at 0.1-2 ℃/min for crystallization, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing to obtain 0.9kg of secondary mother liquor, sampling to obtain the purity of the secondary mother liquor of 99.3%, and performing crystallization and purification on the secondary mother liquor together with the VC crystallization raw material with the purity of 97% at the next time;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 19-24 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the second-stage sweating liquid is discharged after the sweating is finished and weighed to obtain 0.6kg, the purity of the second-stage sweating liquid is 99.3% by sampling, and the second-stage sweating liquid can be crystallized and purified together with the VC crystallization raw material with the next purity of 99.4%;
melting process: and (2) gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 30-35 ℃ to melt and crystallize the product, controlling the melting time for 30min, discharging and weighing the secondary crystallization product after the melting is finished to obtain 5kg (the weight of the product is 8.7kg after the recovery liquid and the secondary perspiration liquid are utilized), and sampling to obtain the secondary crystallization product (the vinylene carbonate crystal on the tube wall of the crystallization tube of the falling film crystallizer obtained by circulating and crystallizing the vinylene carbonate crystal on the tube wall of the crystallization tube of the falling film crystallizer after the vinylene carbonate crystal on the tube wall of the crystallization tube of the falling film crystallizer is melted in the first crystallization process) with the purity of 99.99%.
Vinylene carbonate was produced according to the procedure of this example, and the energy consumption was 1760kg steam/t vinylene carbonate end product, calculated up to 3000t product, wherein the energy consumption in the purification process was 1280kg steam/t vinylene carbonate end product.
Example 2
As shown in fig. 2, the present embodiment is different from embodiment 1 in that: the temperature of the desolventizing treatment is 40 ℃, and the pressure is 9 kPa; a crude distillation column 33 is provided on a communicating pipe between the desolventizing column 31 and the falling film crystallizer 32, and the falling film crystallizer 32 communicates with the lower part or bottom of the crude distillation column 33 via a circulating pump (not shown). Impurities such as polymerization inhibitor butyl-p-cresol (BHT) and poly (ethylene carbonate) can be removed by distillation through the crude distillation tower 3, and the purity of the final product is further improved. The temperature of the crude distillation column 32 was 58 ℃ and the pressure was 3 kPa;
the molar ratio of the total chlorine gas to the total ethylene carbonate in the first photolysis reaction tower 11 and the second photolysis reaction tower 12 is 0.6: 3, heating the first photolysis reaction tower 11 and the second photolysis reaction tower 12 to 60 ℃, enabling the ultraviolet wavelength to be 365nm and the chlorination reaction time to be 1h, and enabling the ultraviolet wavelength and the chlorination reaction time to enter a chlorination reaction liquid of the deacidification tower 13, wherein the content of ethylene dichlorocarbonate is 0.66 wt%;
the molar ratio of the total amount of triethylamine as a removing agent to the total amount of high-purity chloroethylene carbonate (CEC) is 1: 1, the mass ratio of the total amount of polymerization inhibitor butyl-p-cresol (BHT) to the total amount of high-purity Chlorinated Ethylene Carbonate (CEC) is 0.1: 100, respectively;
the materials in the first reaction kettle 21 and the second reaction kettle 22 are heated to 60 ℃, and the dechlorination reaction time is 4 hours;
s1: pouring 10kg of VC crystallization raw material to be treated with the purity of 98% (the temperature is 30-35 ℃) into a raw material tank, starting a falling film crystallizer and circulating cold and heat medium preheating equipment, and controlling the temperature of the circulating cold and heat medium to be 20-23 ℃;
s2: pre-cooling materials: starting a crystallization circulating pump, conveying the VC crystallization raw material in the raw material tank to the falling film crystallizer for circulating conveyance, and controlling the flow of circulating material to be 0.2-0.6m3The pressure is 0.02-0.07MPa, the motor frequency is 13-18Hz, and the temperature of the circulating material is rapidly reduced to 20-25 ℃;
s3: carrying out first falling film crystallization:
and (3) a crystallization process: reducing the temperature of the circulating cooling and heating medium to 1-3 ℃ step by step at the speed of 0.1-2 ℃/min, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing mother liquor to obtain 1.8kg of direct crystallization to obtain 1.2kg of recovery liquid and 0.6kg of residual liquid, wherein the product purity of the recovery liquid can reach about 98.5%, the recovery liquid can be crystallized and purified together with the VC crystallization raw material with the next purity of 98%, and the residual liquid can be sent to a secondary rectification unit;
sweating process: the temperature of the circulating cooling and heating medium is increased to 20-25 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the first-stage sweating liquid is discharged and weighed to obtain 0.3kg after the sweating is finished, the purity of the first-stage sweating liquid is measured by sampling to be 99.5%, and the first-stage sweating liquid can be filled, stored and added into the crystallization raw material with the next purity of 98%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 32-36 ℃ to melt the crystallized product, controlling the melting time for 30min, discharging and weighing the first-stage crystallized product after the melting is finished to obtain 7.9kg, and sampling to obtain the purity of the first-stage crystallized product of 99.4%;
s4: carrying out second falling film crystallization:
and (3) a crystallization process: sending 7.9kg of primary crystallization products with the purity of 99.4% into a falling film crystallizer for circulation, reducing the temperature of a circulating cooling and heating medium by 1-3 ℃ step by step at 0.1-2 ℃/min for crystallization, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing to obtain 1.6kg of secondary mother liquor, sampling to obtain the purity of the secondary mother liquor of 98.6%, and performing crystallization and purification on the secondary mother liquor and a VC crystallization raw material with the next purity of 98%;
the sweating process: gradually raising the temperature of the circulating cooling and heating medium to 20-25 ℃ at the speed of 0.1-2 ℃/min, keeping the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system unchanged, controlling the sweating time to be 40-50min, discharging and weighing the secondary sweating liquid after the sweating is finished to obtain 0.5Kg, sampling to obtain the purity of the secondary sweating liquid of 99.3%, and crystallizing and purifying the secondary sweating liquid and a primary crystallized product with the next purity of 99.4%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 28-34 ℃ to melt the crystallized product, controlling the melting time for 30min, discharging and weighing the secondary crystallized product after the melting is finished to obtain 5.8kg, and sampling to obtain the purity of the secondary crystallized product of 99.99%;
s4: carrying out third falling film crystallization:
and (3) a crystallization process: 5.8kg of secondary crystallization product with the purity of 99.99 percent is sent into a falling film crystallizer for circulation, the temperature of a circulating cooling and heating medium is reduced by 1 to 3 ℃ step by step at the speed of 0.1 to 2 ℃/min for crystallization, the crystallization time is controlled to be 80 to 90min, a crystallization circulating pump is stopped, 0.9kg of tertiary mother liquor is obtained by discharge and weighing, the purity of the tertiary mother liquor is 99.92 percent by sampling, and the tertiary mother liquor can be crystallized and purified together with the primary crystallization product with the purity of 99.4 percent at the next time;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 19-25 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the sweating is finished, the sweating liquid of the third-stage is discharged and weighed to obtain 0.7Kg, the purity of the third-stage sweating liquid is measured by sampling to be 99.95%, and the third-stage sweating liquid can be crystallized and purified together with the next second-stage crystallization product with the purity of 99.99%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 31-36 ℃ to melt and crystallize the product, controlling the melting time for 30min, discharging and weighing the third-stage crystallized product after the melting is finished to obtain 4.2kg (the weight of the product is about 7.3kg after the recycling liquid, the second-stage mother liquid, the first-stage mother liquid, the second-stage mother liquid and the third-stage sweat are utilized), and sampling to obtain the purity of the second-stage crystallized product to be 99.995%;
the energy consumption for purifying the VC crude product with the purity of 60 percent to the high-purity VC with the purity of 99.995 percent is 2500kg of steam per ton of the product.
Temperature adjustment in the crystallization process:
the primary crystallization is rapidly cooled to 35-22 ℃ and is slowly cooled to 22-0 ℃;
the second and third-stage crystallization is rapidly cooled to 35-22 ℃ and slowly cooled to 22-5 ℃.
Adjusting the temperature of a cooling medium of a falling film crystallization system by sweating:
the first-stage crystallization is rapidly heated to 0-18 ℃ and slowly heated to 18-22.5 ℃;
the second and third-stage crystallization are rapidly heated to 5-18 ℃ and slowly heated to 18-22.5 ℃.
Keeping the temperature of a cold and heat medium of a falling film crystallization circulation heat preservation system unchanged, controlling the sweating time to be 40-50min, and discharging sweat after sweating, weighing and sampling;
vinylene carbonate was produced in the manner of this example and the energy consumption was calculated up to 3000t of product, 2530kg steam/t vinylene carbonate end product, wherein the energy consumption in the purification process was 1970kg steam/t vinylene carbonate end product.
Example 3
The present embodiment is different from embodiment 2 in that: the temperature of the desolventizing treatment is 36 ℃, and the pressure is 6 kPa; the temperature of the crude distillation treatment is 50 ℃, and the pressure is 4 kPa; the molar ratio of the total chlorine gas to the total ethylene carbonate in the first photolysis reaction tower 11 and the second photolysis reaction tower 12 is 0.5: 2.5, heating the first photolysis reaction tower 11 and the second photolysis reaction tower 12 to 64 ℃, allowing chlorination reaction to take 1.5h, and allowing the mixture to enter a chlorination reaction liquid of the deacidification tower 13, wherein the content of ethylene dichlorocarbonate is 0.69 wt%;
the molar ratio of the total amount of triethylamine as a removing agent to the total amount of high-purity chloroethylene carbonate (CEC) is 1: 1.2, the mass ratio of the total amount of the polymerization inhibitor butyl-p-cresol (BHT) to the total amount of the high-purity Chlorinated Ethylene Carbonate (CEC) is 0.3: 100.
the materials in the first reaction kettle 21 and the second reaction kettle 22 are heated to 64 ℃, and the dechlorination reaction time is 4.5 hours;
s1: pouring 10kg of VC crystallization raw material to be treated with the purity of 98% (the temperature is 30-35 ℃) into a raw material tank, starting a falling film crystallizer and circulating cooling and heating medium preheating equipment, and controlling the temperature of the circulating cooling and heating medium to be 18-21 ℃;
s2: pre-cooling materials: starting a crystallization circulating pump, conveying the VC crystallization raw material in the raw material tank to the falling film crystallizer for circulating conveyance, and controlling the flow of circulating material to be 0.2-0.6m3The pressure is 0.02-0.07MPa, the motor frequency is 13-18Hz, and the temperature of the circulating material is rapidly reduced to 19-23 ℃;
s3: carrying out first falling film crystallization:
and (3) a crystallization process: reducing the temperature of the circulating cooling and heating medium to 1-3 ℃ step by step at the speed of 0.1-2 ℃/min, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing mother liquor to obtain 1.8kg of direct crystallization to obtain 1.2kg of recovery liquid and 0.6kg of residual liquid, wherein the product purity of the recovery liquid can reach about 98.5%, the recovery liquid can be crystallized and purified together with the VC crystallization raw material with the next purity of 98%, and the residual liquid can be sent to a secondary rectification unit;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 20-25 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the first-stage sweating liquid is discharged and weighed to obtain 0.3kg after the sweating is finished, the purity of the first-stage sweating liquid is measured by sampling to be 99.5%, and the first-stage sweating liquid can be filled, stored and added into the crystallization raw material with the next purity of 98%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 29-34 ℃ to melt the crystallized product, controlling the melting time for 30min, discharging and weighing the first-stage crystallized product after the melting is finished to obtain 7.9kg, and sampling to obtain the purity of the first-stage crystallized product of 99.4%;
s4: carrying out second falling film crystallization:
and (3) a crystallization process: sending 7.9kg of primary crystallization product with the purity of 99.4% into a falling film crystallizer for circulation, reducing the temperature of a circulating cooling and heating medium by 0.1-2 ℃/min step by 1-3 ℃ for crystallization, controlling the crystallization time to be 80-90min, stopping a crystallization circulating pump, discharging and weighing to obtain 1.6kg of secondary mother liquor, sampling to obtain the purity of 98.6% of the secondary mother liquor, and performing crystallization and purification on the secondary mother liquor together with the VC crystallization raw material with the purity of 98% next time;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 20-24 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the second-stage sweating liquid is discharged after the sweating is finished and weighed to obtain 0.5kg, the purity of the second-stage sweating liquid is 99.3% by sampling, and the second-stage sweating liquid can be crystallized and purified together with a first-stage crystallization product with the next purity of 99.4%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 31-35 ℃ to melt the crystallized product, controlling the melting time for 30min, discharging and weighing the secondary crystallized product after the melting is finished to obtain 5.8kg, and sampling to obtain the purity of the secondary crystallized product of 99.99%;
s4: carrying out third falling film crystallization:
and (3) a crystallization process: 5.8kg of secondary crystallization products with the purity of 99.99 percent are sent into a falling film crystallizer for circulation, the temperature of a circulating cooling and heating medium is gradually reduced by 1-3 ℃ at 0.1-2 ℃/min for crystallization, the crystallization time is controlled to be 80-90min, a crystallization circulating pump is stopped, 0.9kg of tertiary mother liquor is obtained by discharging and weighing, the purity of the tertiary mother liquor is 99.92 percent by sampling, and the tertiary mother liquor can be crystallized and purified together with a primary crystallization product with the purity of 99.4 percent at the next time;
the sweating process: the temperature of the circulating cooling and heating medium is increased to 19-25 ℃ step by step at the speed of 0.1-2 ℃/min, the temperature of the cooling and heating medium of the falling film crystallization circulating heat preservation system is kept unchanged, the sweating time is controlled to be 40-50min, the sweating is finished, the sweating liquid of the third-stage is discharged and weighed to obtain 0.7kg, the purity of the third-stage sweating liquid is 99.95% by sampling and measuring, and the third-stage sweating liquid can be crystallized and purified together with the next second-stage crystallization product with the purity of 99.99%;
melting process: gradually adjusting the temperature of a cooling medium of the falling film crystallization system to 30-35 ℃ to melt and crystallize the product, controlling the melting time for 30min, discharging and weighing the third-stage crystallized product after the melting is finished to obtain 4.2kg (the weight of the product is about 7.3kg after the recycling liquid, the second-stage mother liquid, the first-stage mother liquid, the second-stage mother liquid and the third-stage sweat are utilized), and sampling to obtain the purity of the second-stage crystallized product which is 99.995%;
the energy consumption for purifying the VC crude product with the purity of 60 percent to the high-purity VC with the purity of 99.995 percent is 2500kg of steam per ton of the product.
Temperature adjustment in the crystallization process:
the primary crystallization is rapidly cooled to 35-22 ℃ and is slowly cooled to 22-0 ℃;
the second and third-stage crystallization is rapidly cooled to 35-22 ℃ and slowly cooled to 22-5 ℃.
Adjusting the temperature of a cooling medium of a falling film crystallization system by sweating:
the first-stage crystallization is rapidly heated to 0-18 ℃ and slowly heated to 18-22.5 ℃;
the second and third-stage crystallization are rapidly heated to 5-18 ℃ and slowly heated to 18-22.5 ℃.
Keeping the temperature of a cold and heat medium of a falling film crystallization circulation heat preservation system unchanged, controlling the sweating time to be 40-50min, and discharging sweat after sweating, weighing and sampling;
vinylene carbonate was produced according to the example and calculated as up to 3000t product with an energy consumption of 2570kg steam/t vinylene carbonate end product, wherein the energy consumption in the purification process was 2010kg steam/t vinylene carbonate end product.
Comparative example 1
This comparative example differs from example 2 in that: the molar ratio of the total chlorine gas to the total ethylene carbonate in the first photolysis reaction tower 11 and the second photolysis reaction tower 12 is 0.8: 3; the chlorinated reaction liquid fed into the deacidification tower 13 had a content of ethylene dichlorocarbonate of 1.32% by weight.
Vinylene carbonate was produced in the manner of this comparative example and calculated as a product scaled up to 3000t with an energy consumption difference of 3240kg steam/t vinylene carbonate final product (purity of secondary crystalline product of 99.97%), wherein the energy consumption in the purification step was 2550kg steam/t vinylene carbonate final product.
As can be seen from example 2 and comparative example 1, the energy consumption of example 2 is significantly reduced as compared with comparative example 1, and thus it is shown that the present invention can significantly reduce the energy consumption by reducing the ratio of chlorine gas to ethylene carbonate.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Those skilled in the art can modify or change the above-described embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A method for producing vinylene carbonate is characterized by comprising a chlorination reaction step, a dechlorination reaction step and a purification step, wherein the chlorination reaction comprises the following steps: performing chlorination reaction under ultraviolet irradiation by using ethylene carbonate as a raw material and chlorine as a chlorinating agent, wherein the molar ratio of the chlorine to the ethylene carbonate is 0.4-0.6: 2-3.
2. The production method according to claim 1, wherein the temperature of the chlorination reaction is 60-70 ℃ and the time of the chlorination reaction is 1-2 h.
3. The production method according to claim 1, further comprising the steps of: and respectively using water and alkali liquor to recover hydrogen chloride gas and chlorine gas in the liquid after the chlorination reaction.
4. The production process according to claim 1, characterized in that the dechlorination reaction: and adding a removing agent and a polymerization inhibitor into the chlorination reaction liquid to perform dechlorination.
5. The production method according to claim 4, wherein the removal agent is triethylamine.
6. The production method according to claim 4, wherein the polymerization inhibitor is butyl-p-cresol.
7. The production method according to claim 1, wherein the purification comprises melt crystallization.
8. The production method according to claim 7, characterized in that the melt crystallization is carried out using a falling film crystallizer.
9. Vinylene carbonate produced by the production method according to any one of claims 1 to 8.
10. Use of vinylene carbonate produced by the production method according to any one of claims 1 to 8 in a lithium ion battery.
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| CN115036575A (en) * | 2022-08-10 | 2022-09-09 | 中创新航科技股份有限公司 | Electrolyte and lithium ion battery containing same |
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