CN113527252B - Method for synthesizing vinylene carbonate for electrolyte - Google Patents
Method for synthesizing vinylene carbonate for electrolyte Download PDFInfo
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- CN113527252B CN113527252B CN202111092875.5A CN202111092875A CN113527252B CN 113527252 B CN113527252 B CN 113527252B CN 202111092875 A CN202111092875 A CN 202111092875A CN 113527252 B CN113527252 B CN 113527252B
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- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 27
- 239000003792 electrolyte Substances 0.000 title claims abstract description 18
- 230000002194 synthesizing effect Effects 0.000 title claims description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 86
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 67
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 57
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims abstract description 43
- 229910000041 hydrogen chloride Inorganic materials 0.000 claims abstract description 43
- OYOKPDLAMOMTEE-UHFFFAOYSA-N 4-chloro-1,3-dioxolan-2-one Chemical compound ClC1COC(=O)O1 OYOKPDLAMOMTEE-UHFFFAOYSA-N 0.000 claims abstract description 42
- 239000002994 raw material Substances 0.000 claims abstract description 37
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 36
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 36
- 239000003999 initiator Substances 0.000 claims abstract description 27
- 239000007789 gas Substances 0.000 claims abstract description 20
- 238000000746 purification Methods 0.000 claims abstract description 15
- 238000005086 pumping Methods 0.000 claims abstract description 11
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 56
- 239000000460 chlorine Substances 0.000 claims description 56
- 229910052801 chlorine Inorganic materials 0.000 claims description 56
- 238000010521 absorption reaction Methods 0.000 claims description 43
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 33
- 239000000047 product Substances 0.000 claims description 28
- 239000000945 filler Substances 0.000 claims description 22
- 239000003513 alkali Substances 0.000 claims description 19
- 238000000066 reactive distillation Methods 0.000 claims description 19
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 18
- 239000007864 aqueous solution Substances 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 239000002253 acid Substances 0.000 claims description 13
- 239000003963 antioxidant agent Substances 0.000 claims description 13
- 230000003078 antioxidant effect Effects 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 12
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 9
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 9
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 9
- 239000007791 liquid phase Substances 0.000 claims description 9
- 239000012071 phase Substances 0.000 claims description 9
- 238000001179 sorption measurement Methods 0.000 claims description 9
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 8
- 239000007795 chemical reaction product Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000010992 reflux Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- BZLVMXJERCGZMT-UHFFFAOYSA-N Methyl tert-butyl ether Chemical compound COC(C)(C)C BZLVMXJERCGZMT-UHFFFAOYSA-N 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 6
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 6
- XBDQKXXYIPTUBI-UHFFFAOYSA-N dimethylselenoniopropionate Natural products CCC(O)=O XBDQKXXYIPTUBI-UHFFFAOYSA-N 0.000 claims description 6
- 150000002978 peroxides Chemical class 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- IEJIGPNLZYLLBP-UHFFFAOYSA-N dimethyl carbonate Chemical compound COC(=O)OC IEJIGPNLZYLLBP-UHFFFAOYSA-N 0.000 claims description 5
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 4
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- WFUGQJXVXHBTEM-UHFFFAOYSA-N 2-hydroperoxy-2-(2-hydroperoxybutan-2-ylperoxy)butane Chemical compound CCC(C)(OO)OOC(C)(CC)OO WFUGQJXVXHBTEM-UHFFFAOYSA-N 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- OIFBSDVPJOWBCH-UHFFFAOYSA-N Diethyl carbonate Chemical compound CCOC(=O)OCC OIFBSDVPJOWBCH-UHFFFAOYSA-N 0.000 claims description 3
- JBTWLSYIZRCDFO-UHFFFAOYSA-N ethyl methyl carbonate Chemical compound CCOC(=O)OC JBTWLSYIZRCDFO-UHFFFAOYSA-N 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- -1 pentaerythritol ester Chemical class 0.000 claims description 3
- 235000019260 propionic acid Nutrition 0.000 claims description 3
- IUVKMZGDUIUOCP-BTNSXGMBSA-N quinbolone Chemical compound O([C@H]1CC[C@H]2[C@H]3[C@@H]([C@]4(C=CC(=O)C=C4CC3)C)CC[C@@]21C)C1=CCCC1 IUVKMZGDUIUOCP-BTNSXGMBSA-N 0.000 claims description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 3
- 150000003568 thioethers Chemical class 0.000 claims description 3
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 claims description 2
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 9
- 238000001308 synthesis method Methods 0.000 abstract description 6
- 238000010924 continuous production Methods 0.000 abstract description 3
- 238000007670 refining Methods 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- HIGQQEOWQNDHJD-UHFFFAOYSA-N 4,4-dichloro-1,3-dioxolan-2-one Chemical compound ClC1(Cl)COC(=O)O1 HIGQQEOWQNDHJD-UHFFFAOYSA-N 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 239000012043 crude product Substances 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 2
- 238000011049 filling Methods 0.000 description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- JPLNAQJTXYXDAV-UHFFFAOYSA-N 4,4,5-trichloro-1,3-dioxolan-2-one Chemical compound ClC1OC(=O)OC1(Cl)Cl JPLNAQJTXYXDAV-UHFFFAOYSA-N 0.000 description 1
- IKNZCYNFXKIQMI-UHFFFAOYSA-N acetylene;carbonic acid Chemical compound C#C.OC(O)=O IKNZCYNFXKIQMI-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/40—Vinylene carbonate; Substituted vinylene carbonates
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to the technical field of vinylene carbonate synthesis and purification, and discloses a vinylene carbonate synthesis method for electrolyte, which specifically comprises the following steps: pumping raw materials of ethylene carbonate and an initiator into a raw material preheater through a metering pump, feeding chlorine gas into a reaction rectifying tower from the bottom of the tower, reacting the chlorine gas with the ethylene carbonate in the reaction rectifying tower, feeding excess chlorine gas and a product hydrogen chloride into a vacuum pump through a gas phase outlet of a condenser, and pumping chloroethylene carbonate into a vinylene carbonate synthesis kettle; the synthesis and rectification processes of the chloroethylene carbonate are integrated, the synthesis and the refining of the chloroethylene carbonate are simultaneously carried out through the reaction rectification tower, the reaction heat emitted in the reaction process is used for rectification, the integral synthesis time is shortened, the continuous production of the chloroethylene carbonate is realized, the material back mixing is effectively reduced, the main reaction selectivity is obviously improved, and the occurrence of side reactions is reduced.
Description
Technical Field
The invention relates to the technical field of vinylene carbonate synthesis, in particular to a method for synthesizing vinylene carbonate for electrolyte.
Background
The vinylene carbonate is synthesized by three main process routes, and each process route takes the vinylene carbonate as a starting material. The method comprises the following steps: ethylene carbonate is used as a raw material, hydrogen atoms on the ethylene carbonate are substituted with chlorine gas to produce dichloroethylene carbonate, and chlorine is eliminated to produce vinylene carbonate. The method 2 comprises the following steps: using ethylene carbonate as a raw material, and using sulfuryl chloride or chlorine gas as a chlorinating agent, substituting hydrogen atoms on the ethylene carbonate to generate monochloroethylene carbonate, and then eliminating chlorine to generate vinylene carbonate. The method 3 comprises the following steps: the ethylene carbonate is taken as a raw material, and catalytic dehydrogenation is directly carried out to generate vinylene carbonate. After the vinylene carbonate crude product is prepared, the vinylene carbonate product is obtained by separation means such as filtration, reduced pressure rectification and the like.
Currently, the method 2 is mostly used in industry for producing vinylene carbonate, and the reaction process is shown in fig. 2.
In the process of synthesizing chloroethylene carbonate, chloroethylene carbonate serving as a reaction product can further react with chlorine to generate dichloroethylene carbonate, the boiling point of the dichloroethylene carbonate is close to that of the chloroethylene carbonate, the dichloroethylene carbonate is difficult to separate, and acetylene carbonate can be generated in the subsequent synthesis of vinylene carbonate, so that the product purity is reduced, and the overall yield is reduced. Meanwhile, ethylene carbonate is chlorinated into a strong exothermic reaction, and the reaction rate is gradually accelerated along with the rise of the problem, so that in the traditional process for carrying out the reaction in a reaction kettle, if heat is not transferred in time, temperature runaway in the reaction kettle can be caused, and potential safety hazards are caused.
For example, the Chinese patent web publication CN105859677A discloses a preparation method of monochloroethylene carbonate, which comprises the following steps: in the tower reactor, a filling layer is arranged every 1 m along the height direction of the tower, a bracket is arranged, the bottom of each bracket is provided with a first mercury immersion lamp, and a liquid uniform distributor and a second mercury immersion lamp are respectively arranged above each layer of filling; preheating ethylene carbonate to 60 ℃, adding an initiator and a catalyst, and heating to 60 ℃ to obtain ethylene carbonate liquid containing the initiator and the catalyst; introducing nitrogen from the tower bottom to replace the air in the tower, and emptying nitrogen tail gas; drying and dehydrating chlorine, heating to 65 ℃, introducing chlorine into the bottom and the middle of the tower respectively, adding ethylene carbonate liquid containing an initiator and a catalyst from the top of the tower, carrying out gas-liquid countercurrent contact reaction, collecting liquid monochloroethylene carbonate at the bottom of the tower, and treating tail gas at the top of the tower to obtain hydrochloric acid and chlorinated paraffin.
The chlorine gas in the tower reactor mentioned in the above patent enters the tower from the bottom of the tower, and the reaction product chloroethylene carbonate is also produced from the bottom of the rectifying tower, and from the view point of the concentration distribution of the materials in the tower reactor, the concentration gradient of the chloroethylene carbonate is gradually increased from the top to the bottom, and the concentration gradient of the chlorine gas is also gradually increased from the top to the bottom, so that the chloroethylene carbonate in the lower part of the reactor is further reacted with the chlorine gas to generate dichloroethylene carbonate and trichloroethylene carbonate, and the yield of the reaction is reduced.
For another example, chinese patent network publication No. CN109942536A discloses a method for preparing high-purity chloroethylene carbonate by reactive distillation, which adopts a reactive distillation apparatus, and the structure of the apparatus comprises: the reaction rectifying kettle is characterized in that an output pipe at the top of the reaction rectifying kettle is connected with the input end of a condenser, the output end of the condenser is connected with a storage tank, a finished product tank and a tail gas absorption tank, a return pipe is arranged on the storage tank, and the return pipe is connected to the upper end part of the reaction rectifying kettle; sampling and detecting the bottom of the reaction rectifying still, rectifying the product when the mass fraction of the dichloroethylene carbonate obtained by detection is less than or equal to 1%, and refluxing the distillate at the top of the reaction rectifying still into the reaction rectifying still through a storage tank and a reflux pipe after the distillate enters a condenser to be cooled; and sampling and detecting the output end of the condenser, and collecting the liquid material which is cooled and separated in the condenser into a finished product tank when the mass fraction of the chloroethylene carbonate in the distillate is more than or equal to 95%.
The synthesis process of the reaction rectification device adopted in the patent is divided into two steps, wherein the first step is synthesis of chloroethylene carbonate, and the second step is rectification of chloroethylene carbonate, so that although the selectivity of the reaction is effectively improved, the occurrence of side reactions is reduced, the reaction and the rectification are realized in one device, but the continuous production of chloroethylene carbonate is not realized.
Based on the above, the invention designs a vinylene carbonate synthesis method for an electrolyte, so as to solve the above-mentioned problems.
Disclosure of Invention
The invention aims to provide a method for synthesizing vinylene carbonate for an electrolyte, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a vinylene carbonate synthesis method for electrolyte realizes vinylene carbonate synthesis and purification through a synthesis and purification device, and specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater through a metering pump, controlling the outlet temperature of the raw material preheater to be 40-70 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower, wherein the adding mass of the initiator is 0.1-1% of the mass of the ethylene carbonate;
s2, feeding chlorine into the reaction rectifying tower from the bottom of the tower, wherein the molar weight of the introduced chlorine is 1-1.1 times of that of ethylene carbonate, controlling the temperature of a tower kettle of the reaction rectifying tower at 50-80 ℃ by adjusting the heat conduction oil flow of a reboiler, and controlling the vacuum degree of the reaction rectifying tower at 2-10 Kpa by a vacuum pump;
s3, the chlorine and the ethylene carbonate are in countercurrent contact with each other on the surface of a filler in the reactive distillation tower for reaction, the reaction heat is used for heating a liquid phase, so that the reaction products of chlorinated ethylene carbonate and hydrogen chloride rise together with the chlorine, part of the chlorinated ethylene carbonate and hydrogen chloride flow back after being cooled by a condenser at the top of the reactive distillation tower, and the other part of the chlorinated ethylene carbonate enters a chlorinated ethylene carbonate buffer tank;
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump through a gas phase outlet of a condenser, allowing the excess chlorine and the product hydrogen chloride to enter an acid absorption tower through an outlet of the vacuum pump, absorbing the product hydrogen chloride through demineralized water to prepare a 30% hydrochloric acid aqueous solution, allowing the residual trace hydrogen chloride and excess chlorine to enter an alkali absorption tower, allowing the trace hydrogen chloride and the excess chlorine to pass through a 48% sodium hydroxide aqueous solution in the alkali absorption tower to prepare a sodium hypochlorite aqueous solution, and introducing the residual nonabsorbent gas into an active carbon absorption tower for absorption;
s5, adding the chloroethylene carbonate into a vinylene carbonate synthesis kettle, starting stirring, adding the solvent, triethylamine and the antioxidant, controlling the reaction temperature to be 60-80 ℃, and reacting for 8 hours.
Preferably, synthetic purification device includes raw material preheater and reaction rectifying column, raw material preheater is connected with the reaction rectifying column middle part, reaction rectifying column bottom is equipped with the reboiler, reaction rectifying column top exit linkage has the condenser, the liquid phase exit linkage of condenser has chlorinated ethylene carbonate buffer tank, chlorinated ethylene carbonate buffer tank exit linkage has vinylene carbonate synthesis cauldron, the gaseous phase exit linkage of condenser has the vacuum pump, the export of vacuum pump is connected with the entry of acid absorption tower, the export of acid absorption tower is connected with the entry of alkali absorption tower, the export of alkali absorption tower is connected with the entry of active carbon adsorption tower, the export evacuation of active carbon adsorption tower.
Preferably, the reactive distillation tower is provided with section fillers, each section of filler is a meter, the fillers are silk screen fillers, a distributor is arranged in the middle of each section of filler, an LED ultraviolet lamp is arranged on the distributor and used for irradiating the fillers, a reboiler is arranged at the tower bottom of the reactive distillation tower, a condenser is arranged at the tower top, and the power of the LED ultraviolet lamp is 50-500 KW.
Preferably, the initiator is one or more of peroxide, and the peroxide can be benzoyl peroxide, benzoyl tert-butyl peroxide, methyl ethyl ketone peroxide or azobisisobutyronitrile.
Preferably, the reflux ratio of S3 is 1 (1-3), the purity of chloroethylene carbonate is more than 99%, and the selectivity of chloroethylene carbonate is calculated to be more than 98%.
Preferably, the mass ratio of the chloroethylene carbonate, the solvent, the triethylamine and the antioxidant in the S5 is 1 (3-5): 0.5-1): 0.001-0.01.
Preferably, the antioxidant is one or more of 2, 6-tri-tert-butyl-4-methylphenol, bis (3, 5-tri-tert-butyl-4-hydroxyphenyl) thioether and tetra- [ beta- (3, 5-tri-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
Preferably, the solvent is one or more of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, methyl tert-butyl ether, tetrahydrofuran, acetonitrile, chloroform and dichloromethane.
Compared with the prior art, the invention has the beneficial effects that:
the synthesis and rectification processes of the chloroethylene carbonate are integrated, the synthesis and the refining of the chloroethylene carbonate are simultaneously carried out through the reaction rectification tower, the reaction heat is released in the reaction process and is used for rectification, the equipment investment is reduced, the overall synthesis time is shortened, the process energy consumption is reduced, the continuous production of the chloroethylene carbonate is realized, the material back-mixing is effectively reduced through the design of the feeding position of the reaction rectification tower, the main reaction selectivity is obviously improved, and the occurrence of side reactions is reduced.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the description below are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic flow diagram of a synthesis apparatus according to the present invention;
FIG. 2 is a schematic diagram of a prior art vinylene carbonate production reaction.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1, the present invention provides a technical solution of a method for synthesizing vinylene carbonate for electrolyte, wherein vinylene carbonate is synthesized and purified by a synthesis and purification device, and the method specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater 1 through a metering pump, controlling the outlet temperature of the raw material preheater to be 40-70 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower 2, wherein the adding mass of the initiator is 0.1% -1% of the mass of the ethylene carbonate;
s2, feeding chlorine into the reaction rectifying tower 2 from the bottom of the tower, wherein the molar weight of the introduced chlorine is 1-1.1 times of that of ethylene carbonate, controlling the temperature of a tower kettle of the reaction rectifying tower 2 at 50-80 ℃ by adjusting the heat conduction oil flow of the reboiler 3, and controlling the vacuum degree of the reaction rectifying tower 2 at 2-10 Kpa by a vacuum pump 5;
s3, the chlorine and the ethylene carbonate react in countercurrent contact on the surface of the packing in the reactive distillation tower 2, the reaction heat is used for heating the liquid phase, so that the reaction products of chlorinated ethylene carbonate and hydrogen chloride rise together with the chlorine, and after being cooled by a condenser 4 at the top of the reactive distillation tower 2, part of the chlorine and the hydrogen chloride flow back to enter a chlorinated ethylene carbonate buffer tank 9;
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump 5 through a gas phase outlet of a condenser 4, allowing the excess chlorine and product hydrogen chloride to enter an acid absorption tower 6 through an outlet of the vacuum pump 5, absorbing the product hydrogen chloride through demineralized water to prepare a 30% hydrochloric acid aqueous solution, allowing the rest trace hydrogen chloride and excess chlorine to enter an alkali absorption tower 7, allowing the trace hydrogen chloride and excess chlorine to be absorbed by a 48% sodium hydroxide aqueous solution in the alkali absorption tower 7 to prepare a sodium hypochlorite aqueous solution, and introducing the rest unabsorbed gas into an active carbon absorption tower 8 for absorption;
s5, pumping the chloroethylene carbonate into a vinylene carbonate synthesis kettle 10, starting stirring, simultaneously adding a solvent, triethylamine and an antioxidant, controlling the reaction temperature to be 60-80 ℃, reacting for 8 hours to obtain a vinylene carbonate crude product, and purifying and separating to obtain a vinylene carbonate product.
Example 1:
a technical scheme of a vinylene carbonate synthesis method for electrolyte is provided, which realizes vinylene carbonate synthesis and purification through a synthesis and purification device, and specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater 1 through a metering pump, controlling the outlet temperature of the raw material preheater to be 40 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower 2, wherein the adding mass of the initiator is 0.1 percent of the mass of the ethylene carbonate;
s2, chlorine enters the reaction rectifying tower 2 from the bottom of the tower, the introduced chlorine has the molar weight 1 time that of the ethylene carbonate, the temperature of the tower kettle of the reaction rectifying tower 2 is controlled at 50 ℃ by adjusting the heat conducting oil flow of the reboiler 3, and the vacuum degree of the reaction rectifying tower 2 is controlled at 2Kpa by the vacuum pump 5;
s3, the chlorine and the ethylene carbonate are in countercurrent contact with each other on the surface of a filler in the reactive distillation tower 2 for reaction, the reaction heat is used for heating a liquid phase, so that the reaction products of chlorinated ethylene carbonate and hydrogen chloride rise together with the chlorine, part of the chlorinated ethylene carbonate and hydrogen chloride flow back after being cooled by a condenser 4 at the top of the reactive distillation tower 2, and part of the chlorinated ethylene carbonate enters a chlorinated ethylene carbonate buffer tank 9;
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump 5 through a gas phase outlet of a condenser 4, allowing the excess chlorine and product hydrogen chloride to enter an acid absorption tower 6 through an outlet of the vacuum pump 5, absorbing the product hydrogen chloride through demineralized water to prepare a 30% hydrochloric acid aqueous solution, allowing the rest trace hydrogen chloride and excess chlorine to enter an alkali absorption tower 7, allowing the trace hydrogen chloride and excess chlorine to be absorbed by a 48% sodium hydroxide aqueous solution in the alkali absorption tower 7 to prepare a sodium hypochlorite aqueous solution, and introducing the rest unabsorbed gas into an active carbon absorption tower 8 for absorption;
s5, pumping the chloroethylene carbonate into a vinylene carbonate synthesis kettle 10, starting stirring, simultaneously adding a solvent, triethylamine and an antioxidant, controlling the reaction temperature to be 60 ℃, reacting for 8 hours to obtain a vinylene carbonate crude product, and purifying and separating to obtain a vinylene carbonate product.
Example 2:
a technical scheme of a vinylene carbonate synthesis method for electrolyte is provided, which realizes vinylene carbonate synthesis and purification through a synthesis and purification device, and specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater 1 through a metering pump, controlling the outlet temperature of the raw material preheater to be 70 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower 2, wherein the adding mass of the initiator is 1% of the mass of the ethylene carbonate;
s2, feeding chlorine into the reactive distillation tower 2 from the bottom of the tower, wherein the molar weight of the introduced chlorine is 1.1 times of that of the ethylene carbonate, controlling the temperature of the tower kettle of the reactive distillation tower 2 at 80 ℃ by adjusting the heat conduction oil flow of the reboiler 3, and controlling the vacuum degree of the reactive distillation tower 2 at 10Kpa by a vacuum pump 5;
s3, carrying out countercurrent contact reaction on chlorine and ethylene carbonate on the surface of a filler in a reaction rectifying tower 2, wherein the reaction heat is used for liquid phase heating, so that chlorinated ethylene carbonate and hydrogen chloride which are reaction products rise together with the chlorine, and after cooling through a condenser 4 at the top of the reaction rectifying tower 2, part of the chlorine and the hydrogen chloride flows back, and part of the chlorine and the hydrogen chloride enters a chlorinated ethylene carbonate buffer tank 9, wherein the reflux ratio is 1 (1-3), the purity of the chlorinated ethylene carbonate is more than 99%, and the selectivity of the chlorinated ethylene carbonate is calculated to be more than 98%;
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump 5 through a gas phase outlet of a condenser 4, allowing the excess chlorine and the product hydrogen chloride to enter an acid absorption tower 6 through an outlet of the vacuum pump 5, absorbing the product hydrogen chloride through desalted water to prepare a 30% hydrochloric acid aqueous solution, allowing the rest trace hydrogen chloride and the excess chlorine to enter an alkali absorption tower 7, allowing the trace hydrogen chloride and the excess chlorine to be prepared into a sodium hypochlorite aqueous solution through a 48% sodium hydroxide aqueous solution in the alkali absorption tower 7, and introducing the rest unabsorbed gas into an active carbon adsorption tower 8 for adsorption;
s5, pumping the chloroethylene carbonate into a vinylene carbonate synthesis kettle 10, starting stirring, simultaneously adding a solvent, triethylamine and an antioxidant, controlling the reaction temperature to be 80 ℃, reacting for 8 hours to obtain a vinylene carbonate crude product, and purifying and separating to obtain a vinylene carbonate product.
Example 3:
a technical scheme of a vinylene carbonate synthesis method for electrolyte is provided, which realizes vinylene carbonate synthesis and purification through a synthesis and purification device, and specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater 1 through a metering pump, controlling the outlet temperature of the raw material preheater to be 50 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower 2, wherein the adding mass of the initiator is 0.1-1% of the mass of the ethylene carbonate;
s2, feeding chlorine into the reactive distillation tower 2 from the bottom of the tower, wherein the molar weight of the introduced chlorine is 1.05 times of that of the ethylene carbonate, controlling the temperature of a tower kettle of the reactive distillation tower 2 at 70 ℃ by adjusting the heat-conducting oil flow of the reboiler 3, and controlling the vacuum degree of the reactive distillation tower 2 at 6Kpa by a vacuum pump 5;
s3, the chlorine and the ethylene carbonate are in countercurrent contact with each other on the surface of a filler in the reactive distillation tower 2 for reaction, the reaction heat is used for heating a liquid phase, so that the reaction products of chlorinated ethylene carbonate and hydrogen chloride rise together with the chlorine, part of the chlorinated ethylene carbonate and hydrogen chloride flow back after being cooled by a condenser 4 at the top of the reactive distillation tower 2, and part of the chlorinated ethylene carbonate enters a chlorinated ethylene carbonate buffer tank 9;
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump 5 through a gas phase outlet of a condenser 4, allowing the excess chlorine and product hydrogen chloride to enter an acid absorption tower 6 through an outlet of the vacuum pump 5, absorbing the product hydrogen chloride through demineralized water to prepare a 30% hydrochloric acid aqueous solution, allowing the rest trace hydrogen chloride and excess chlorine to enter an alkali absorption tower 7, allowing the trace hydrogen chloride and excess chlorine to be absorbed by a 48% sodium hydroxide aqueous solution in the alkali absorption tower 7 to prepare a sodium hypochlorite aqueous solution, and introducing the rest unabsorbed gas into an active carbon absorption tower 8 for absorption;
s5, adding chloroethylene carbonate into a vinylene carbonate synthesis kettle 10, starting stirring, adding a solvent, triethylamine and an antioxidant, controlling the reaction temperature at 70 ℃, reacting for 8 hours to obtain a vinylene carbonate crude product, and purifying and separating to obtain a vinylene carbonate product, wherein the mass ratio of chloroethylene carbonate to the solvent to the triethylamine to the antioxidant is (3-5) to (0.5-1) to (0.001-0.01).
Wherein, synthetic purification device includes raw materials pre-heater 1 and reaction rectifying tower 2, raw materials pre-heater 1 is connected with 2 middle parts of reaction rectifying tower, 2 bottoms in reaction rectifying tower are equipped with reboiler 3, 2 top exit linkage in reaction rectifying tower have condenser 4, the liquid phase exit linkage of condenser 4 has chlorinated ethylene carbonate buffer tank 9, 9 exit linkage in chlorinated ethylene carbonate buffer tank have vinylene carbonate synthetic kettle 10, the gas phase exit linkage of condenser 4 has vacuum pump 5, the export of vacuum pump 5 is connected with the entry of acid absorption tower 6, the export of acid absorption tower 6 is connected with the entry of alkali absorption tower 7, the export of alkali absorption tower 7 is connected with the entry of active carbon adsorption tower 8, the export evacuation of active carbon adsorption tower 8.
The reaction rectifying tower 2 is provided with 10 sections of fillers, each section of fillers is 2 meters, the fillers are filled by a silk screen, a distributor is arranged in the middle of each section of fillers, an LED ultraviolet lamp is arranged on the distributor and used for irradiating the fillers, a tower kettle of the rectifying tower is provided with a reboiler 3, a condenser 4 is arranged at the top of the tower, and the power of the LED ultraviolet lamp is 50-500 KW.
The initiator is one or more of peroxide, and the peroxide can be benzoyl peroxide, benzoyl peroxide tert-butyl ester, methyl ethyl ketone peroxide and azobisisobutyronitrile.
Wherein the reflux ratio in the S3 is 1 (1-3), the purity of the chloroethylene carbonate is more than 99%, and the selectivity of the chloroethylene carbonate is calculated to be more than 98%.
Wherein the mass ratio of the chloroethylene carbonate, the solvent, the triethylamine and the antioxidant in the S5 is 1 (3-5) to 0.5-1) to 0.001-0.01.
Wherein the antioxidant is one or a mixture of more of 2, 6-tri-tert-butyl-4-methylphenol, bis (3, 5-tri-tert-butyl-4-hydroxyphenyl) thioether and tetra [ beta- (3, 5-tri-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
Wherein the solvent is one or more of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, methyl tert-butyl ether, tetrahydrofuran, acetonitrile, chloroform and dichloromethane.
The specific embodiment is as follows:
the ethylene carbonate (500 KG/h) and the initiator azobisisobutyronitrile (5 KG/h) are pumped into the raw material preheater 1 through a metering pump, the outlet temperature of the raw material preheater 1 is controlled to be 60 ℃, the preheated material enters from the middle part of the reaction rectifying tower 2, and liquid chlorine is gasified by a chlorine gas generator and then is delivered in 138 m3The flow rate of chlorine gas continuously rises from the bottom of the reaction rectifying tower 2, the chlorine gas reacts with descending vinyl carbonate and an initiator under the illumination condition of an LED ultraviolet lamp, the product vinyl chloride is heated and gasified, then rises along with the chlorine gas, the chlorine gas enters a condenser 4 from the top of the reaction rectifying tower 2, the condensed material is refluxed into the reaction rectifying tower 2 to continue to react under the control of a reflux ratio of 1:1, part of the condensed material is extracted into a vinyl chloride buffer tank 9, the vinyl chloride buffer tank 9 is sampled and analyzed regularly, the average content of the vinyl chloride is 99.4%, a gas phase outlet at the top of the condenser 4 sequentially enters an acid absorption tower 6, an alkali absorption tower 7 and an active carbon absorption tower 8, and the tail gas recovery efficiency is 100%. After the liquid level of the chlorinated ethylene carbonate buffer tank 9 reaches 80%, the chlorinated ethylene carbonate buffer tank is thrown into a vinylene carbonate synthesis kettle 10 at one time, and the metered addition amount is as follows: 3500 kg. Adding dimethyl carbonate (12250 kg) and 2, 6-tri-tert-butyl-4-methylphenol (12 kg) as solvents into a head tank, starting a vinylene carbonate synthesis kettle 10 to stir (300 r/min) and heat after the addition is finished, controlling the temperature in the kettle to be 75 ℃, dropwise adding triethylamine (580 kg/h) into the vinylene carbonate synthesis kettle 10 through the head tank after the temperature in the kettle reaches a preset temperature, stopping dropwise adding for 3h, continuing to react for 5 h, then sampling and analyzing, stopping reaction after the purity of chloroethylene carbonate in the kettle is less than 0.5%, and refining materials in the kettle in a rectification system.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for synthesizing vinylene carbonate for electrolyte is characterized by comprising the following steps: the vinylene carbonate synthesis and purification are realized through a synthesis and purification device, and the method specifically comprises the following steps:
s1, pumping raw material ethylene carbonate and an initiator into a raw material preheater (1) through a metering pump, controlling the outlet temperature of the raw material preheater to be 40-70 ℃, and feeding the raw material ethylene carbonate and the initiator from the middle upper part of a reaction rectifying tower (2), wherein the adding mass of the initiator is 0.1-1% of the mass of the ethylene carbonate;
s2, feeding chlorine into the reaction rectifying tower (2) from the bottom of the tower, controlling the temperature of a tower kettle of the reaction rectifying tower (2) at 50-80 ℃ by adjusting the heat conduction oil flow of the reboiler (3) and controlling the vacuum degree of the reaction rectifying tower (2) at 2-10 Kpa through a vacuum pump (5), wherein the molar weight of the fed chlorine is 1-1.1 times that of the ethylene carbonate;
s3, the chlorine and the ethylene carbonate are in countercurrent contact with each other on the surface of a filler in the reaction rectifying tower (2) for reaction, the reaction heat is used for heating a liquid phase, so that the reaction products of chloroethylene carbonate and hydrogen chloride rise together with the chlorine, and after being cooled by a condenser (4) at the top of the reaction rectifying tower (2), part of chloroethylene carbonate flows back, and part of chloroethylene carbonate enters a chloroethylene carbonate buffer tank (9);
s4, allowing excess chlorine and product hydrogen chloride to enter a vacuum pump (5) through a gas phase outlet of a condenser (4), allowing the excess chlorine and the product hydrogen chloride to enter an acid absorption tower (6) through an outlet of the vacuum pump (5), absorbing the product hydrogen chloride through demineralized water to prepare a 30% hydrochloric acid aqueous solution, allowing the residual trace hydrogen chloride and the residual chlorine to enter an alkali absorption tower (7), allowing the trace hydrogen chloride and the residual chlorine to pass through a 48% sodium hydroxide aqueous solution in the alkali absorption tower (7) to prepare a sodium hypochlorite aqueous solution, and introducing the residual nonabsorbed gas into an active carbon adsorption tower (8) for adsorption;
s5, adding chlorinated ethylene carbonate into a vinylene carbonate synthesis kettle (10), starting stirring, adding a solvent, triethylamine and an antioxidant, controlling the reaction temperature to be 60-80 ℃, and reacting for 8 hours;
the synthesis and purification device comprises a raw material preheater (1) and a reaction rectifying tower (2), wherein the raw material preheater (1) is connected with the middle part of the reaction rectifying tower (2), a reboiler (3) is arranged at the bottom of the reaction rectifying tower (2), a condenser (4) is connected with an outlet at the top of the reaction rectifying tower (2), a liquid phase outlet of the condenser (4) is connected with a chloroethylene carbonate buffer tank (9), an outlet of the chloroethylene carbonate buffer tank (9) is connected with a vinylene carbonate synthesis kettle (10), a gas phase outlet of the condenser (4) is connected with a vacuum pump (5), an outlet of the vacuum pump (5) is connected with an inlet of an acid absorption tower (6), an outlet of the acid absorption tower (6) is connected with an inlet of an alkali absorption tower (7), an outlet of the alkali absorption tower (7) is connected with an inlet of an active carbon absorption tower (8), and the outlet of the activated carbon adsorption tower (8) is emptied.
2. The method for synthesizing vinylene carbonate for electrolyte according to claim 1, wherein: 10 sections of fillers are arranged in the reactive distillation tower (2), each section of fillers is 2 meters, the fillers are silk screen fillers, a distributor is arranged in the middle of each section of fillers, an LED ultraviolet lamp is arranged on the distributor and used for irradiating the fillers, and the power of the LED ultraviolet lamp is 50-500 KW.
3. The method for synthesizing vinylene carbonate for electrolyte according to claim 1, wherein: the initiator is one or a mixture of more than one peroxide, and the peroxide can be benzoyl peroxide, benzoyl tert-butyl peroxide, methyl ethyl ketone peroxide or azobisisobutyronitrile.
4. The method for synthesizing vinylene carbonate for electrolyte according to claim 1, wherein: the reflux ratio in the S3 is 1 (1-3), and the purity of the chloroethylene carbonate is more than 99%.
5. The method for synthesizing vinylene carbonate for electrolyte according to claim 1, wherein: the mass ratio of the chloroethylene carbonate, the solvent, the triethylamine and the antioxidant in the S5 is 1 (3-5) to (0.5-1) to (0.001-0.01).
6. The method for synthesizing vinylene carbonate for electrolyte according to claim 5, wherein: the antioxidant is one or a mixture of 2, 6-tri-tert-butyl-4-methylphenol, bis (3, 5-tri-tert-butyl-4-hydroxyphenyl) thioether and tetra [ beta- (3, 5-tri-tert-butyl-4-hydroxyphenyl) propionic acid ] pentaerythritol ester.
7. The method for synthesizing vinylene carbonate for electrolyte according to claim 5, wherein: the solvent is one or more of dimethyl carbonate, ethyl methyl carbonate, diethyl carbonate, ethyl acetate, methyl tert-butyl ether, tetrahydrofuran, acetonitrile, chloroform and dichloromethane.
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