CN116003376A - Process and reaction system for continuously synthesizing chloroethylene carbonate - Google Patents
Process and reaction system for continuously synthesizing chloroethylene carbonate Download PDFInfo
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- CN116003376A CN116003376A CN202310148001.XA CN202310148001A CN116003376A CN 116003376 A CN116003376 A CN 116003376A CN 202310148001 A CN202310148001 A CN 202310148001A CN 116003376 A CN116003376 A CN 116003376A
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- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 title claims abstract description 88
- 238000006243 chemical reaction Methods 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 32
- 230000002194 synthesizing effect Effects 0.000 title abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 122
- 238000005660 chlorination reaction Methods 0.000 claims abstract description 114
- 238000002425 crystallisation Methods 0.000 claims abstract description 65
- 230000008025 crystallization Effects 0.000 claims abstract description 65
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 46
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000000460 chlorine Substances 0.000 claims abstract description 41
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 41
- 238000007654 immersion Methods 0.000 claims abstract description 35
- 238000000926 separation method Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000004945 emulsification Methods 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 76
- 239000007789 gas Substances 0.000 claims description 70
- 238000003860 storage Methods 0.000 claims description 55
- 230000001804 emulsifying effect Effects 0.000 claims description 43
- 239000007787 solid Substances 0.000 claims description 30
- CBWUNQZJGJFJLZ-UHFFFAOYSA-N [Cl].Cl Chemical compound [Cl].Cl CBWUNQZJGJFJLZ-UHFFFAOYSA-N 0.000 claims description 17
- 239000012065 filter cake Substances 0.000 claims description 17
- 238000010521 absorption reaction Methods 0.000 claims description 13
- 239000003513 alkali Substances 0.000 claims description 13
- 230000001678 irradiating effect Effects 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 9
- 239000012295 chemical reaction liquid Substances 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 238000011084 recovery Methods 0.000 claims description 6
- 239000000523 sample Substances 0.000 claims description 2
- 238000010517 secondary reaction Methods 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 3
- 230000000977 initiatory effect Effects 0.000 abstract description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 2
- 238000007146 photocatalysis Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- BIYFBWRLDKOYMU-UHFFFAOYSA-N 1-(3,4-dichlorophenyl)-2-(ethylamino)propan-1-one Chemical compound CCNC(C)C(=O)C1=CC=C(Cl)C(Cl)=C1 BIYFBWRLDKOYMU-UHFFFAOYSA-N 0.000 abstract 1
- 239000000376 reactant Substances 0.000 description 20
- 238000009833 condensation Methods 0.000 description 18
- 230000005494 condensation Effects 0.000 description 18
- 238000007599 discharging Methods 0.000 description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 7
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 7
- 239000000463 material Substances 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- HIGQQEOWQNDHJD-UHFFFAOYSA-N 4,4-dichloro-1,3-dioxolan-2-one Chemical compound ClC1(Cl)COC(=O)O1 HIGQQEOWQNDHJD-UHFFFAOYSA-N 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000004321 preservation Methods 0.000 description 4
- 239000011780 sodium chloride Substances 0.000 description 4
- 230000005587 bubbling Effects 0.000 description 3
- 125000001309 chloro group Chemical group Cl* 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000011541 reaction mixture Substances 0.000 description 3
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 2
- SBLRHMKNNHXPHG-UHFFFAOYSA-N 4-fluoro-1,3-dioxolan-2-one Chemical compound FC1COC(=O)O1 SBLRHMKNNHXPHG-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000007792 addition Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000007810 chemical reaction solvent Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- LGXVIGDEPROXKC-UHFFFAOYSA-N 1,1-dichloroethene Chemical group ClC(Cl)=C LGXVIGDEPROXKC-UHFFFAOYSA-N 0.000 description 1
- 239000002000 Electrolyte additive Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010924 continuous production Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
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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
- 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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process and a reaction system for continuously synthesizing chloroethylene carbonate, which belong to the field of organic chemical industry, wherein the method takes ethylene carbonate and chlorine as main raw materials, and adopts a multistage chlorination reaction device through photocatalysis initiation, and utilizes an ultrasonic gas-liquid emulsification device in a chlorination tower and the arrangement of an immersion type ultraviolet lamp to realize the efficient utilization of light and chlorine and shorten the reaction time; through the arrangement of the gas-liquid separation tank, the separated gas can be applied to the next stage of chlorination tower, so that the multi-stage application of chlorine is realized, and the utilization rate of the chlorine is improved; the crystallization temperature of the DTB crystallizer is regulated, so that the ethylene carbonate and DCEC are effectively separated, and high-purity chloroethylene carbonate is obtained; the chlorine and the ethylene carbonate can be recycled, the whole-course continuous self control of the ethylene carbonate chlorination is realized, the instability of the process is greatly reduced, the raw material utilization rate is low, and the product quality is poor, so that the method is suitable for industrial production.
Description
Technical Field
The invention belongs to the field of organic chemical industry, and particularly relates to a process and a reaction system for continuously synthesizing chloroethylene carbonate.
Background
In recent years, with the change of world energy structures, the research of electric energy storage and battery technology is increasingly carried out, and the production of high-quality battery raw materials is also a bottleneck which puzzles the development of battery technology. Chloroethylene carbonate (CEC), also known as 4-chloro-1, 3-dioxapentacyclic-2-ketone, has an English name Chloroethylene carbonate, is light yellow liquid at normal temperature, can be slowly decomposed after being placed for a long time at a temperature exceeding 40 ℃, and is a synthetic raw material of lithium battery electrolyte additives, fluoroethylene carbonate (FEC) and Vinylene Carbonate (VC).
The synthesis process of chloroethylene carbonate (CEC) mainly comprises the following two steps:
among them, the sulfonyl chloride method has been eliminated because of the large amount of acid gas generated and the large pollution, and the current market mainstream technology is the chlorine method for producing chloroethylene carbonate. Aiming at the problems of long time and low efficiency caused by illumination adopted by a chlorine method, a plurality of chlorine production processes are designed and invented by vast technical researchers.
Patent CN114437016a discloses a method for producing chloroethylene carbonate, which adopts a kettle type process and adopts a nitrogen partial pressure mode to reduce the concentration of chlorine and HCl in a kettle so as to inhibit polymerization, decomposition, addition and other series of side reactions in a reaction kettle, but has the problems of low light efficiency, incapability of large-scale production, low utilization rate of chlorine atoms and the like.
Patent CN103772344a discloses a method for photochemically synthesizing chloroethylene carbonate and a photochemical reactor, the invention is provided with a jacketed sink in the immersion type photoreactor, and an immersion up-bubbling photochemical reactor with a high-pressure mercury lamp is arranged in the jacketed sink for photochemically synthesizing chloroethylene carbonate; under the protection of inert gas, the traditional highly toxic reaction solvent is removed, so that the raw material ethylene carbonate and chlorine are in direct contact reaction, and the reaction solvent is not needed.
The patent CN114163413A discloses a method for preparing high-purity chloroethylene carbonate by continuous double-stage liquid phase reaction, which is characterized in that liquid chlorine, ethylene carbonate and a catalyst are subjected to double-stage liquid phase reaction at high temperature and high pressure to produce chloroethylene carbonate, and the chloroethylene carbonate, the dichloroethylene carbonate and unreacted ethylene carbonate are separated from reaction products by high-vacuum rectification to obtain the high-purity chloroethylene carbonate.
Patent CN114192078A discloses a bubbling reaction device and a method for continuously producing chloroethylene carbonate, the invention designs a multistage bubbling device serial reaction device, the reaction chlorinating agent is fed in steps and steps, the ethylene carbonate is fed in one step, the device can solve the continuous discharging of the ethylene carbonate, but the following points are also that (1) the chloroethylene carbonate stays in the reactor all the time, the concentration is gradually increased from the first reactor, the proportion of the polychlorinated ethylene carbonate is gradually increased, and finally the chloroselectivity is obviously reduced; (2) The ethylene carbonate reaction liquid and the chlorinated reagent are reversely convected and fed, the concentration of ethylene carbonate is reduced from top to bottom, the concentration of chlorinated products is increased, the concentration of chlorinated reagents is increased, and the materials are convected in feeding and discharging, so that the problems of dead volume, increase of polychlorinated impurities and the like of the materials are easily caused; (3) The gas distributor is adopted in the single bubbling reaction device, so that the gas-liquid short-time distribution can be realized, but the chlorination reaction is an hour-level reaction, the gas-liquid mixture is completely separated again within minutes, and the single gas distributor can not improve the reaction efficiency.
Disclosure of Invention
Aiming at the problems of complex process, long operation period, low light and chlorine utilization rate, low product yield and incapability of large-scale and continuous production in the existing photo-induced chlorination industrial production process of ethylene carbonate, the invention aims to provide a process and a reaction system for continuously synthesizing chloroethylene carbonate.
The invention aims to achieve the aim, and the aim is achieved by the following technical scheme:
a process for the continuous synthesis of chloroethylene carbonate comprising the steps of:
(1) adding ethylene carbonate and chlorine with preheating temperature of 65-70 ℃ into a first-stage chlorination tower with the temperature of 65-70 ℃, performing ultrasonic emulsification, irradiating and reacting for 2-8 hours under an ultraviolet lamp with the wavelength of 320-400 nm, escaping a gas-liquid mixture from the top of the first-stage chlorination tower, performing gas-liquid separation to obtain hydrogen chloride-chlorine mixed gas and reaction liquid, crystallizing the reaction liquid, and filtering to obtain a filter cake and crystallization recovery liquid;
(2) adding the filter cake obtained in the step (1) and the hydrogen chloride-chlorine mixed gas obtained in the step (1) into a secondary chlorination tower, performing ultrasonic emulsification, performing irradiation reaction for 2-8 hours under an ultraviolet lamp with the wavelength of 320-400 nm, escaping a gas-liquid mixture from the top of the secondary chlorination tower, and performing gas-liquid separation to obtain the hydrogen chloride-chlorine mixed gas Q 2 And reaction liquid, crystallizing and filtering the reaction liquid to obtain a filter cake L 2 And a crystallization recovery liquid;
(3) the filter cake L obtained in the step (2) 2 And the hydrogen chloride-chlorine mixed gas Q obtained in the step (2) 2 Adding the raw materials into a three-stage chlorination tower, performing ultrasonic emulsification, performing irradiation reaction for 2-8 hours under an ultraviolet lamp with the wavelength of 320-400 nm, escaping a gas-liquid mixture from the top of the three-stage chlorination tower, and performing gas-liquid separation to obtain hydrogen chloride-chlorine mixed gas Q 3 And reaction liquid, crystallizing and filtering the reaction liquid to obtain a filter cake L 3 And a crystallization recovery liquid; the hydrogen chloride-chlorine gas mixture Q 3 Introducing into an alkali absorption tower, and filtering a filter cake L 3 Can be used for entering the first-stage chlorination tower.
The mass ratio of the chlorine to the ethylene carbonate in the step (1) is 1: 5-6.5; the hydrogen chloride-chlorine mixed gas enters a lower-stage chlorination tower for mechanically applying reaction; the filter cake is a mixture of ethylene carbonate and chloroethylene carbonate, and is used for entering a lower-level chlorination tower; the crystallization recovery liquid is chloroethylene carbonate.
The mass rate ratio of the ethylene carbonate to the chlorine in the primary chlorination tower is 4.5-6.5: 1, the mass rate ratio of the filter cake and the hydrogen chloride-chlorine mixed gas in the secondary chlorination tower is 6.0-8.0: 1, third stage Chlorination tower filter cake L 2 And hydrogen chloride-chlorine gas mixture Q 2 The mass rate ratio of the addition is 6.5-8.5: 1.
the primary reaction crystallization temperature is-10-0 ℃, the secondary reaction crystallization temperature is 5-15 ℃, and the tertiary reaction crystallization temperature is 20-30 ℃.
Preferably, the primary chlorination tower immersion ultraviolet lamp is used for reacting for 2-4 hours under irradiation, the secondary chlorination tower immersion ultraviolet lamp is used for reacting for 4-6 hours under irradiation, and the tertiary chlorination tower immersion ultraviolet lamp is used for reacting for 6-8 hours under irradiation.
The invention realizes the process through the following reaction system: the reaction system comprises a three-stage serial chlorination reaction device and an alkali absorption tower, and the chlorination reaction device has the following specific structure: the first discharge port of the top of the primary chloro-tower is connected with a primary gas-liquid separation tank through a pipeline, the first liquid discharge port of the primary gas-liquid separation tank is connected with a primary DTB crystallizer through a pipeline, the first gas outlet of the primary gas-liquid separation tank is connected with the chlorine gas feed port of the next stage chloro-tower in series through a pipeline, the first solid discharge port of the primary DTB crystallizer is connected with a primary EC heat-preserving storage tank through a pipeline, the first CEC discharge port of the primary DTB crystallizer is connected with a primary CEC storage tank through a pipeline, the primary EC heat-preserving storage tank is connected with the ethylene carbonate feed port of the next stage chloro-tower device in series through a pipeline, and the third gas outlet of the final tertiary gas-liquid separation tank is connected with an alkali absorption tower through a pipeline.
The bottom of the primary chlorination tower is also provided with a first chlorine gas feed inlet and a first ethylene carbonate feed inlet, and a first ultrasonic gas-liquid emulsifying device and a first immersion ultraviolet lamp are arranged in the primary chlorination tower; the first ultrasonic gas-liquid emulsifying device is uniformly distributed in a plurality of chlorination towers, the average interval is 1-2 m, the single power is 500-1000 w, and the first ultrasonic gas-liquid emulsifying device is provided with a gas distributor and an ultrasonic probe; the first immersion ultraviolet lamps are 320-400 nm in wavelength, are connected in parallel in multiple stages, are distributed in the tower at average intervals of 1-2 m, and have single power of 80-100 w.
According to the invention, reactants obtained from the chlorination tower are rapidly separated through the gas-liquid separation tank, the separated gas can be applied to the next-stage chlorination tower, so that the multi-stage application of chlorine is realized, the utilization rate of the chlorine is improved, meanwhile, HCl generated by the reaction can dilute the concentration of the chlorine, the reaction rate is reduced, and the rapid separation and application of mixed gas can ensure that the reaction rate change rate in a single chlorination tower is smaller and is easier to control; the DTB crystallizer can realize the rapid separation of the ethylene carbonate and the chloroethylene carbonate, ensure that the discharging amount of the chloroethylene carbonate product and a small amount of DCEC along with the discharging of the chloroethylene carbonate in a single chlorination system are not accumulated in the next set, ensure the purity of the raw material ethylene carbonate in the next system, and ensure the controllable product quality.
According to the invention, ethylene carbonate and chlorine are fed in the same direction from the bottom, and by combining the arrangement of the ultrasonic gas-liquid emulsifying device and the immersion ultraviolet lamp in the chlorination tower, the materials can be uniformly and rapidly mixed and dissolved, the light utilization rate is improved, and the reaction rate is greatly improved; along with the rising of materials in the tower, the concentration of chloroethylene carbonate is gradually increased, and the concentration of ethylene carbonate and chlorine is gradually reduced, so that the problems of single-strand material lifting and the increase of polychlorinated compounds such as dichloroethylene carbonate (DCEC) and the like during reverse convection feeding are avoided.
Compared with the prior art, the invention has the following advantages:
according to the invention, ethylene carbonate and chlorine are used as main raw materials, and are subjected to photocatalysis initiation, and through a multistage chlorination reaction device, the efficient utilization of light and chlorine is realized by utilizing the arrangement of an ultrasonic gas-liquid emulsifying device and an immersion ultraviolet lamp in a chlorination tower, so that the reaction time is shortened; through the arrangement of the gas-liquid separation tank, the separated gas can be applied to the next stage of chlorination tower, so that the multi-stage application of chlorine is realized, and the utilization rate of the chlorine is improved; the crystallization temperature of the DTB crystallizer is regulated, so that the ethylene carbonate and DCEC are effectively separated, and high-purity chloroethylene carbonate is obtained; the chlorine and the ethylene carbonate can be recycled, the whole-course continuous self control of the ethylene carbonate chlorination is realized, the instability of the process is greatly reduced, the raw material utilization rate is low, and the product quality is poor, so that the method is suitable for industrial production.
Drawings
FIG. 1 is a schematic diagram showing the equipment connections of a reaction system for continuously synthesizing chloroethylene carbonate according to the present invention;
in the figure, a 1-primary chlorination tower; 2-a first discharge port; 3-a first-stage gas-liquid separation tank; 4-a first gas outlet; 5-a first liquid discharge port; 6-stage DTB crystallizer; 7-a first CEC discharge port; 8-stage CEC storage tank; 9-a first solid discharge port; 10-a first-stage EC heat-preserving storage tank; 11-a first chlorine feed inlet; 12-a first ethylene carbonate feed inlet; 13-a first ultrasonic gas-liquid emulsifying device; 14-a first immersion ultraviolet lamp; 15-a secondary chlorination tower; 16-a second discharge port; 17-a secondary gas-liquid separation tank; 18-a second gas outlet; 19-a second liquid discharge port; a 20-secondary DTB crystallizer; 21-a second CEC discharge port; 22-secondary CEC storage tank; 23-a second solids discharge port; 24-a secondary EC heat-preserving storage tank; 25-a second chlorine feed inlet; 26-a second ethylene carbonate feed inlet; 27-a second ultrasonic gas-liquid emulsifying device; 28-a second immersion ultraviolet lamp; 29-third-stage chlorination tower; 30-a third discharge port; 31-a three-stage gas-liquid separation tank; 32-a third gas outlet; 33-a third liquid discharge port; 34-three-stage DTB crystallizer; 35-a third CEC discharge port; 36-three level CEC storage tank; 37-a third solids discharge port; 38-three-stage EC heat preservation storage tank; 39-a third chlorine feed inlet; 40-a third ethylene carbonate feed inlet; 41-a third ultrasonic gas-liquid emulsifying device; 42-a third immersion ultraviolet lamp; 43-alkali absorption tower.
Detailed Description
The foregoing is further elaborated by the following description of embodiments of the present invention, which are given by way of example only, and should not be construed as limiting the scope of the present invention. All techniques implemented based on the above description of the invention are within the scope of the invention.
Referring to fig. 1, ethylene carbonate and chlorine are respectively introduced into a first-stage chlorination tower 1 through a first ethylene carbonate feed port 12 and a first chlorine feed port 11, emulsified by a first ultrasonic gas-liquid emulsifying device 13 in the tower, and reacted under the irradiation of a first immersion type ultraviolet lamp 14 in the tower, the obtained reactant is introduced into a first-stage gas-liquid separation tank 3 from a first tower top discharge port 2, the separated gas is introduced into a second chlorine feed port 25 of a second-stage chlorination tower 15 through a first gas outlet 4, the separated liquid flows into a first-stage DTB crystallizer 6 from a first liquid discharge port 5 for condensation crystallization, the liquid obtained after crystallization is introduced into a first-stage CEC storage tank 8 through a first CEC discharge port 7, the precipitated solid is introduced into a first-stage EC thermal insulation storage tank 10 through a first solid discharge port 9, and the first-stage EC thermal insulation storage tank 10 is communicated with a second ethylene carbonate feed port 26 of the second-stage chlorination tower 15;
the mixed gas and solid which are applied to the secondary chlorination tower 15 are emulsified by a second ultrasonic gas-liquid emulsifying device 27 in the tower, the obtained reactant is led into a secondary gas-liquid separating tank 17 from a second discharging hole 16 at the top of the tower and is led into a third chlorine gas feeding hole 39 of a tertiary chlorination tower 29 by a second gas outlet 18, the separated liquid flows into a secondary DTB crystallizer 20 from a second liquid discharging hole 19 for condensation crystallization, the liquid obtained after crystallization is led into a secondary CEC storage tank 22 by a second CEC discharging hole 21, the separated solid is led into a secondary EC heat-preserving storage tank 24 by a second solid discharging hole 23, and the secondary EC heat-preserving storage tank 24 is communicated with a third ethylene carbonate feeding hole 40 of the tertiary chlorination tower 29;
the mixed gas and solid applied to the third-stage chlorination tower 29 are emulsified by a third ultrasonic gas-liquid emulsifying device 41 in the tower, the obtained reactant is led into a third-stage gas-liquid separation tank 31 from a third discharge port 30 at the top of the tower under the irradiation of a third immersion ultraviolet lamp 42, the separated gas is led into an alkali absorption tower 43 through a third gas outlet 32, the separated liquid flows into a third-stage DTB crystallizer 34 from a third liquid discharge port 33 for condensation crystallization, the liquid obtained after crystallization is led into a third-stage CEC storage tank 36 through a third CEC discharge port 35, the precipitated solid is led into a third-stage EC heat preservation storage tank 38 through a third solid discharge port 37, and the third-stage EC heat preservation storage tank 38 is communicated with the first ethylene carbonate feed port 12 of the first-stage chlorination tower 1.
Example 1
100kg of ethylene carbonate preheated to 65℃and 20kg of chlorine were mixed at 4.5:1, introducing the mixture into a first-stage chlorination tower heated to 65 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for 2 hours, introducing the obtained reactant into a first-stage gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a second-stage chlorination tower for reaction, introducing the separated liquid into a first-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the first-stage DTB crystallizer to be minus 10 ℃, introducing the liquid obtained after crystallization into a first-stage CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a first-stage EC heat-preserving storage tank with the temperature of 65 ℃, and introducing the mixture into a second-stage chlorination tower for application;
the mixture and the mixed gas applied to the secondary chlorination tower are mixed according to the rate ratio of 6:1, introducing the mixture into a secondary chlorination tower heated to 65 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for 2 hours, introducing the obtained reactant into a secondary gas-liquid separating tank from the discharge of the tower top, introducing the separated gas into a tertiary chlorination tower for reaction, introducing the separated liquid into a secondary DTB crystallizer for condensation crystallization, setting the crystallization temperature of the secondary crystallizer to be 5 ℃, introducing the liquid obtained after crystallization into a secondary CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a secondary EC heat-preserving tank with the temperature of 65 ℃, and introducing the mixture into the tertiary chlorination tower for application;
the mixture and the mixture applied to the third-stage chlorination tower are mixed according to the rate ratio of 6.5:1, introducing the mixture into a three-stage chlorination tower heated to 65 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, carrying out reaction for 2 hours under the irradiation of an immersion ultraviolet lamp in the tower, introducing the obtained reactant into a three-stage gas-liquid separation tank from the top discharge of the tower, introducing the separated gas into a hydrogen chloride and chlorine gas mixed gas, introducing the mixed gas into an alkali absorption tower to obtain a solution containing sodium chloride, introducing the separated liquid into a three-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the three-stage crystallizer to be 20 ℃, introducing the liquid obtained after crystallization into a three-stage CEC storage tank, separating out the mixture of EC and a small amount of chloroethylene carbonate, storing the mixture in the three-stage EC heat-preserving storage tank at 65 ℃, and introducing the mixture into a first-stage chlorination tower for application, wherein the mass and purity results of all components in each stage CEC storage tank are shown in Table 1.
Example 2
280kg of ethylene carbonate preheated to 70℃and 43kg of chlorine were reacted in a reaction mixture of 6.5:1, introducing the mixture into a first-stage chlorination tower heated to 70 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for reaction for 8 hours, introducing the obtained reactant into a first-stage gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a second-stage chlorination tower for reaction, introducing the separated liquid into a first-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the first-stage DTB crystallizer to be 0 ℃, introducing the liquid obtained after crystallization into a first-stage CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a first-stage EC heat-preserving storage tank with the temperature of 70 ℃, and introducing the mixture into the second-stage chlorination tower for application;
the mixture and the mixed gas applied to the secondary chlorination tower are mixed according to the rate ratio of 8:1, introducing the mixture into a secondary chlorination tower heated to 70 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for reaction for 8 hours, introducing the obtained reactant into a secondary gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a tertiary chlorination tower for reaction, introducing the separated liquid into a secondary DTB crystallizer for condensation crystallization, setting the crystallization temperature of the secondary crystallizer to 15 ℃, introducing the liquid obtained after crystallization into a secondary CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a secondary EC heat-preserving storage tank with the temperature of 70 ℃, and introducing the mixture into the tertiary chlorination tower for application;
the mixture and the mixture applied to the third-stage chlorination tower are mixed according to the rate ratio of 8.5:1, feeding the mixture into a three-stage chlorination tower heated to 70 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, reacting for 8 hours under the irradiation of an immersion ultraviolet lamp in the tower, feeding the obtained reactant from the top discharge of the tower into a three-stage gas-liquid separation tank, feeding the separated gas which is the mixed gas of hydrogen chloride and chlorine into an alkali absorption tower, and obtaining a solution containing sodium chlorideThe separated liquid flows into a three-stage DTB crystallizer for condensation crystallization, the crystallization temperature of the three-stage crystallizer is set to be 30 ℃, the liquid obtained after crystallization is led into a three-stage CEC storage tank, and the separated solid G is separated out 3 The mixture of EC and a small amount of chloroethylene carbonate is stored in a three-stage EC heat-insulating storage tank with the temperature of 70 ℃ and can be fed into a first-stage chloro tower for application, and the mass and purity results of each component in each stage CEC storage tank are shown in Table 2.
Example 3
280kg of ethylene carbonate preheated to 67℃and 50kg of chlorine were reacted in a reaction vessel at 5:1, introducing the mixture into a first-stage chlorination tower heated to 67 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for 3 hours, introducing the obtained reactant into a first-stage gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a second-stage chlorination tower for reaction, introducing the separated liquid into a first-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the first-stage DTB crystallizer to be minus 5 ℃, introducing the liquid obtained after crystallization into a first-stage CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a first-stage EC heat-preserving storage tank with the temperature of 65 ℃, and introducing the separated gas into a second-stage chlorination tower for application;
the mixture and the mixed gas applied to the secondary chlorination tower are used in a rate ratio of 7:1, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, reacting for 5h under the irradiation of an immersion ultraviolet lamp in the tower, discharging the obtained reactant from the tower top, introducing the obtained reactant into a secondary gas-liquid separating tank, introducing the separated gas into a third-stage chlorination tower for reaction, introducing the separated liquid into a secondary DTB crystallizer for condensation crystallization, setting the crystallization temperature of the secondary crystallizer to be 10 ℃, introducing the liquid obtained after crystallization into a secondary CEC storage tank, and separating out solid G 2 The mixture of EC and a small amount of chloroethylene carbonate is stored in a secondary EC heat-preserving storage tank with the temperature of 70 ℃ and is fed into a tertiary chloro tower for application;
the mixture and the mixture applied to the third-stage chlorination tower are mixed according to the rate ratio of 7.5:1, introducing the mixture into a three-stage chlorination tower heated to 70 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, carrying out reaction for 7 hours under the irradiation of an immersion ultraviolet lamp in the tower, introducing the obtained reactant into a three-stage gas-liquid separation tank from the top discharge of the tower, introducing the separated gas into a hydrogen chloride and chlorine gas mixed gas, introducing the mixed gas into an alkali absorption tower to obtain a solution containing sodium chloride, introducing the separated liquid into a three-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the three-stage crystallizer to be 25 ℃, introducing the liquid obtained after crystallization into a three-stage CEC storage tank, separating out the mixture of EC and a small amount of chloroethylene carbonate, storing the mixture in the three-stage EC heat-preserving storage tank at 67 ℃, and introducing the mixture into a first-stage chlorination tower for application, wherein the mass and purity results of all components in each stage CEC storage tank are shown in Table 3.
Example 4
400kg of ethylene carbonate preheated to 66℃and 72kg of chlorine were reacted in a reaction mixture of 5.5:1, introducing the mixture into a first-stage chlorination tower heated to 66 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, irradiating with an immersion ultraviolet lamp in the tower for reaction for 4 hours, introducing the obtained reactant into a first-stage gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a second-stage chlorination tower for reaction, introducing the separated liquid into a first-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the first-stage DTB crystallizer to be-8 ℃, introducing the liquid obtained after crystallization into a first-stage CEC storage tank, storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate into a first-stage EC heat-preserving storage tank with the temperature of 69 ℃, and introducing the separated gas into a second-stage chlorination tower for application;
the mixture and the mixture applied to the secondary chlorination tower are mixed at a rate ratio of 7.5:1, introducing the mixture into a secondary chlorination tower heated to 69 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for reacting for 5.5 hours, introducing the obtained reactant into a secondary gas-liquid separating tank from the top discharge of the tower, introducing the separated gas into a tertiary chlorination tower for reaction, introducing the separated liquid into a secondary DTB crystallizer for condensation crystallization, setting the crystallization temperature of the secondary crystallizer to be 12 ℃, introducing the liquid obtained after crystallization into a secondary CEC storage tank, and storing the separated solid which is a mixture of EC and a small amount of chloroethylene carbonate into the secondary EC heat-preserving storage tank with the temperature of 70 ℃ and introducing the third chlorination tower for application;
the mixture and the mixed gas applied to the third-stage chlorination tower are mixed according to the rate ratio of 8:1, introducing the mixture into a three-stage chlorination tower heated to 70 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, carrying out reaction for 7.5 hours under the irradiation of an immersion ultraviolet lamp in the tower, introducing the obtained reactant into a three-stage gas-liquid separation tank from the top discharge of the tower, introducing the separated gas into a hydrogen chloride and chlorine mixed gas, introducing the gas into an alkali absorption tower to obtain a solution containing sodium chloride, introducing the separated liquid into a three-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the three-stage crystallizer to be 28 ℃, introducing the liquid obtained after crystallization into a three-stage CEC storage tank, separating out the solid which is a mixture of EC and a small amount of chloroethylene carbonate, storing the solid in the three-stage EC storage tank at 66 ℃, and introducing the solid into a first-stage chlorination tower for application, wherein the mass and purity results of the components in each stage CEC storage tank are shown in Table 4.
Example 5
400kg of ethylene carbonate preheated to 66℃and 67kg of chlorine were reacted in a reaction mixture of 6:1, introducing the mixture into a first-stage chlorination tower heated to 66 ℃, emulsifying by an ultrasonic gas-liquid emulsifying device in the tower, irradiating with an immersion ultraviolet lamp in the tower to react for 2.5 hours, introducing the obtained reactant into a first-stage gas-liquid separation tank from the discharge of the tower top, introducing the separated gas into a second-stage chlorination tower for reaction, introducing the separated liquid into a first-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the first-stage DTB crystallizer to be minus 3 ℃, introducing the liquid obtained after crystallization into a first-stage CEC storage tank, wherein the precipitated solid is a mixture of EC and a small amount of chloroethylene carbonate, storing in the first-stage EC heat-preserving storage tank with the temperature of 67 ℃, and introducing the second-stage chlorination tower for reaction;
the mixture and the mixture applied to the secondary chlorination tower are mixed according to a rate ratio of 6.5:1, introducing the mixture into a secondary chlorination tower heated to 67 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, irradiating the mixture with an immersion ultraviolet lamp in the tower for 4.5 hours, introducing the obtained reactant into a secondary gas-liquid separation tank from the top discharge of the tower, introducing the separated gas into a tertiary chlorination tower for reaction, introducing the separated liquid into a secondary DTB crystallizer for condensation crystallization, setting the crystallization temperature of the secondary crystallizer to 8 ℃, introducing the liquid obtained after crystallization into a secondary CEC storage tank, and storing the precipitated solid which is a mixture of EC and a small amount of chloroethylene carbonate in the secondary EC heat preservation storage tank with the temperature of 66 ℃ and introducing the third chlorination tower for application;
the mixture and the mixed gas applied to the third-stage chlorination tower are mixed according to the rate ratio of 7:1, introducing the mixture into a three-stage chlorination tower heated to 66 ℃, emulsifying the mixture by an ultrasonic gas-liquid emulsifying device in the tower, carrying out reaction for 6.5 hours under the irradiation of an immersion ultraviolet lamp in the tower, introducing the obtained reactant into a three-stage gas-liquid separation tank from the top discharge of the tower, introducing the separated gas into a hydrogen chloride and chlorine mixed gas, introducing the gas into an alkali absorption tower to obtain a solution containing sodium chloride, introducing the separated liquid into a three-stage DTB crystallizer for condensation crystallization, setting the crystallization temperature of the three-stage crystallizer to be 22 ℃, introducing the liquid obtained after crystallization into a three-stage CEC storage tank, separating out solid which is a mixture of EC and a small amount of chloroethylene carbonate, storing the solid in the three-stage EC storage tank at 66 ℃, and introducing the solid into a first-stage chlorination tower for application, wherein the mass and purity results of each component in each stage CEC storage tank are shown in Table 5.
While the foregoing describes the embodiments of the present invention, it is not intended to limit the scope of the present invention, and various modifications or variations may be made by those skilled in the art without the need for inventive effort on the basis of the technical solutions of the present invention.
Claims (7)
1. A process for the continuous synthesis of chloroethylene carbonate, characterized in that: the method comprises the following steps:
(1) adding ethylene carbonate and chlorine with preheating temperature of 65-70 ℃ into a first-stage chlorination tower with the temperature of 65-70 ℃, performing ultrasonic emulsification, irradiating and reacting for 2-8 hours under an ultraviolet lamp with the wavelength of 320-400 nm, escaping a gas-liquid mixture from the top of the first-stage chlorination tower, performing gas-liquid separation to obtain hydrogen chloride-chlorine mixed gas and reaction liquid, crystallizing the reaction liquid, and filtering to obtain a filter cake and crystallization recovery liquid;
(2) adding the filter cake obtained in the step (1) and the hydrogen chloride-chlorine mixed gas obtained in the step (1) into a secondary chlorination tower to repeat the process of the step (1) to obtain a filter cake L 2 And hydrogen chloride-chlorine gas mixture Q 2 ；
(3) The filter cake L obtained in the step (2) 2 And the hydrogen chloride-chlorine mixed gas Q obtained in the step (2) 2 Adding a three-stage chlorination tower into the raw materials, repeating the process of the step (1), and obtaining the hydrogen chloride-chlorine mixed gas Q 3 Introducing into an alkali absorption tower, and filtering a filter cake L 3 Can be used for entering the first-stage chlorination tower.
2. The process for the continuous synthesis of chloroethylene carbonate according to claim 1, characterized in that: the mass ratio of the chlorine to the ethylene carbonate in the step (1) is 1: 5-6.5; the hydrogen chloride-chlorine mixed gas enters a lower-stage chlorination tower for mechanically applying reaction; the filter cake is a mixture of ethylene carbonate and chloroethylene carbonate, and is used for entering a lower-level chlorination tower; the crystallization recovery liquid is chloroethylene carbonate.
3. The process for the continuous synthesis of chloroethylene carbonate according to claim 1, characterized in that: the mass rate ratio of the ethylene carbonate to the chlorine in the primary chlorination tower is 4.5-6.5: 1, the mass rate ratio of the filter cake and the hydrogen chloride-chlorine mixed gas in the secondary chlorination tower is 6.0-8.0: 1, third stage Chlorination tower filter cake L 2 And hydrogen chloride-chlorine gas mixture Q 2 The mass rate ratio of the addition is 6.5-8.5: 1.
4. the process for the continuous synthesis of chloroethylene carbonate according to claim 1, characterized in that: the primary reaction crystallization temperature is-10-0 ℃, the secondary reaction crystallization temperature is 5-15 ℃, and the tertiary reaction crystallization temperature is 20-30 ℃.
5. The process for the continuous synthesis of chloroethylene carbonate according to claim 1, characterized in that: the primary chlorination tower immersion ultraviolet lamp is used for reacting for 2-4 hours under irradiation, the secondary chlorination tower immersion ultraviolet lamp is used for reacting for 4-6 hours under irradiation, and the tertiary chlorination tower immersion ultraviolet lamp is used for reacting for 6-8 hours under irradiation.
6. The process for the continuous synthesis of chloroethylene carbonate according to claim 1, characterized in that: the process is realized through the following reaction system: the reaction system comprises a three-stage serial chlorination reaction device and an alkali absorption tower (43), and is characterized in that: the specific structure of the chlorination reaction device is as follows: the first discharge port (2) at the top of the primary chlorination tower (1) is connected with the primary gas-liquid separation tank (3) through a pipeline, the first liquid discharge port (4) of the primary gas-liquid separation tank (3) is connected with the primary DTB crystallizer (6) through a pipeline, the first gas outlet (4) of the primary gas-liquid separation tank (3) is connected with the chlorine gas feed port of the next stage chlorination tower in series through a pipeline, the first solid discharge port (9) of the primary DTB crystallizer (6) is connected with the primary EC heat-preserving storage tank (10) through a pipeline, the first CEC discharge port (7) of the primary DTB crystallizer (6) is connected with the primary storage tank (8) through a pipeline, the primary EC heat-preserving storage tank (10) is connected with the ethylene carbonate feed port of the next stage chlorination tower device in series through a pipeline, and the third gas outlet (32) of the final tertiary gas-liquid separation tank (31) is connected with the alkali absorption tower (43) through a pipeline.
7. The process for the continuous synthesis of chloroethylene carbonate according to claim 6, characterized in that: the tower bottom of the primary chlorination tower (1) is also provided with a first chlorine gas feed inlet (11) and a first ethylene carbonate feed inlet (12), and a first ultrasonic gas-liquid emulsifying device (13) and a first immersion ultraviolet lamp (14) are arranged in the primary chlorination tower (1); the first ultrasonic gas-liquid emulsifying device (13) is uniformly distributed in a plurality of chlorination towers, the average interval is 1-2 m, the single power is 500-1000 w, and the gas distributor and the ultrasonic probe are arranged; the first immersion ultraviolet lamps (14) are all 320-400 nm in wavelength, are connected in parallel in multiple stages, are distributed in a tower at average intervals of 1-2 m, and have single power of 80-100 w.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116854658A (en) * | 2023-07-11 | 2023-10-10 | 珠海光瑞新材料有限公司 | Method for producing chloroethylene carbonate |
| CN117229253A (en) * | 2023-11-16 | 2023-12-15 | 山东海化集团有限公司 | Method for continuously preparing high-purity chloroethylene carbonate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116854658A (en) * | 2023-07-11 | 2023-10-10 | 珠海光瑞新材料有限公司 | Method for producing chloroethylene carbonate |
| CN117229253A (en) * | 2023-11-16 | 2023-12-15 | 山东海化集团有限公司 | Method for continuously preparing high-purity chloroethylene carbonate |
| CN117229253B (en) * | 2023-11-16 | 2024-04-05 | 山东海化集团有限公司 | Method for continuously preparing high-purity chloroethylene carbonate |
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