CN116462655A - Process for preparing chloroethylene carbonate - Google Patents
Process for preparing chloroethylene carbonate Download PDFInfo
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- CN116462655A CN116462655A CN202310189025.XA CN202310189025A CN116462655A CN 116462655 A CN116462655 A CN 116462655A CN 202310189025 A CN202310189025 A CN 202310189025A CN 116462655 A CN116462655 A CN 116462655A
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- Prior art keywords
- reaction
- ethylene carbonate
- carbonate
- chloroethylene carbonate
- reactor
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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 48
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 70
- KMTRUDSVKNLOMY-UHFFFAOYSA-N Ethylene carbonate Chemical compound O=C1OCCO1 KMTRUDSVKNLOMY-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000047 product Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000000460 chlorine Substances 0.000 claims abstract description 20
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 20
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000003999 initiator Substances 0.000 claims abstract description 19
- 238000002360 preparation method Methods 0.000 claims abstract description 15
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 239000012043 crude product Substances 0.000 claims abstract description 12
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 238000000926 separation method Methods 0.000 claims abstract description 12
- 238000005112 continuous flow technique Methods 0.000 claims abstract description 3
- KZBUYRJDOAKODT-UHFFFAOYSA-N Chlorine Chemical compound ClCl KZBUYRJDOAKODT-UHFFFAOYSA-N 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
- 239000004342 Benzoyl peroxide Substances 0.000 claims description 6
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 6
- 239000000463 material Substances 0.000 claims description 6
- 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 5
- ZHNUHDYFZUAESO-UHFFFAOYSA-N Formamide Chemical compound NC=O ZHNUHDYFZUAESO-UHFFFAOYSA-N 0.000 claims description 4
- 239000004973 liquid crystal related substance Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 3
- 230000003068 static effect Effects 0.000 claims description 2
- -1 ethylene carbonate dichloride Chemical compound 0.000 abstract description 5
- 239000012535 impurity Substances 0.000 abstract description 4
- 230000003321 amplification Effects 0.000 abstract description 2
- 238000003199 nucleic acid amplification method Methods 0.000 abstract description 2
- 230000035484 reaction time Effects 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 8
- 230000000694 effects Effects 0.000 description 6
- 239000007789 gas Substances 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000002156 mixing Methods 0.000 description 4
- VAYTZRYEBVHVLE-UHFFFAOYSA-N 1,3-dioxol-2-one Chemical compound O=C1OC=CO1 VAYTZRYEBVHVLE-UHFFFAOYSA-N 0.000 description 3
- 238000005660 chlorination reaction Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- DDXGMOVCPFHPIV-UHFFFAOYSA-N carbonic acid;chloroethene Chemical compound ClC=C.OC(O)=O DDXGMOVCPFHPIV-UHFFFAOYSA-N 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 230000001276 controlling effect Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- IXCSERBJSXMMFS-UHFFFAOYSA-N hydrogen chloride Substances Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 description 2
- 229910000041 hydrogen chloride Inorganic materials 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- YBBRCQOCSYXUOC-UHFFFAOYSA-N sulfuryl dichloride Chemical compound ClS(Cl)(=O)=O YBBRCQOCSYXUOC-UHFFFAOYSA-N 0.000 description 2
- 230000008016 vaporization Effects 0.000 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 1
- 239000006227 byproduct Substances 0.000 description 1
- NBBQZEHDCMOZCN-UHFFFAOYSA-N carbonic acid;1,2-dichloroethane Chemical compound OC(O)=O.ClCCCl NBBQZEHDCMOZCN-UHFFFAOYSA-N 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000012320 chlorinating reagent Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- GJBRNHKUVLOCEB-UHFFFAOYSA-N tert-butyl benzenecarboperoxoate Chemical compound CC(C)(C)OOC(=O)C1=CC=CC=C1 GJBRNHKUVLOCEB-UHFFFAOYSA-N 0.000 description 1
- 238000009834 vaporization Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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
- C07D317/42—Halogen atoms or nitro radicals
-
- 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
Abstract
The invention discloses a preparation method of chloroethylene carbonate. It is a continuous flow process comprising: s1: introducing ethylene carbonate and an initiator into the reaction unit, and then introducing chlorine to react to obtain a product A; the temperature of the reaction unit is 80-140 ℃; the mol ratio of the ethylene carbonate to the chlorine is 1:1.2-2.0; the pressure of the reaction is 4-18 bar; the residence time of the reaction is 5 s-60 s; s2: introducing the product A into a cooling unit, and then performing gas-liquid separation to obtain a chloroethylene carbonate crude product; the temperature of the cooling unit is 50-70 ℃. The invention shortens the reaction time, has high conversion rate of the ethylene carbonate, high reaction selectivity, low impurity content of the ethylene carbonate dichloride and high yield of the ethylene carbonate, solves the difficult problem of difficult amplification of the process, and realizes the efficient, safe, rapid, energy-saving and easy-to-amplify production of the ethylene carbonate dichloride.
Description
The present application claims priority from chinese patent application CN202210199593.3, with application date 2022, 3 and 2. The present application refers to the entirety of the above-mentioned chinese patent application.
Technical Field
The invention relates to a preparation method of chloroethylene carbonate.
Background
At present, the preparation method of chloroethylene carbonate mainly comprises the following steps:
chinese patent CN104844556B discloses a method for continuously preparing vinylene carbonate by using a tubular reactor, in the step (1), sulfuryl chloride and ethylene carbonate are used as raw materials, and chloroethylene carbonate is synthesized in the tubular reactor under the action of an initiator, although the method can effectively improve the productivity, the cost of using sulfuryl chloride as a chlorinating agent is higher, sulfur dioxide and hydrogen chloride waste gas are simultaneously generated, and the tail gas treatment is difficult.
Chinese patent CN106749155B discloses a method for preparing vinylene carbonate by micro-channel reaction, which uses liquid chlorine and ethylene carbonate as raw materials, and adds initiator to synthesize chloroethylene carbonate in micro-channel reactor.
Chinese patent CN113336737a discloses a method for preparing high-purity chloroethylene carbonate by continuous two-stage liquid phase reaction, which adopts liquid chlorine for chlorination, the system pressure reaches 2.0-3.5 MPa, the usage amount is greatly excessive, the usage amount of initiator reaches more than 8%, and the cost is high.
Chinese patent CN112979607a discloses a method for continuously preparing chloroethylene carbonate, which uses liquid chlorine to perform chlorination, and although the cost of ultraviolet light initiation is low, the reaction for preparing chloroethylene carbonate is performed in a microchannel reactor, so that no suitable large-flux industrialized equipment is available at present, the investment of equipment needs to be increased on the premise of achieving the same productivity, and the investment cost is higher.
In the prior art, a kettle type reactor is used for preparing chloroethylene carbonate, chlorine can only be slowly and continuously introduced, heat and mass transfer are poor, hysteresis exists in heat exchange, and the safety risk of the process is increased.
In addition, in the prior art, the intermittent kettle type reactor is used for preparing chloroethylene carbonate, and as the reaction belongs to an exothermic reaction, the solubility of chlorine in a liquid phase can be greatly increased by increasing the reaction pressure, so that the reaction is greatly accelerated, the reaction is more severe, the heat release quantity can be increased suddenly, the coking polymerization can be caused by local overheating, and the safety risk of the whole process can be greatly increased by high temperature and high pressure; the batch tank reactor has serious back mixing conditions, and the back mixing can reduce the concentration of reactants, simultaneously increase the concentration of products, reduce apparent selectivity and simultaneously cause a series of side reactions.
Disclosure of Invention
The invention aims to overcome the defects of poor heat and mass transfer, hysteresis quality of heat exchange and safety risk of the process in the prior art, and provides a preparation method of chloroethylene carbonate. The preparation method of the invention has the advantages of greatly shortened reaction time, high conversion rate of the ethylene carbonate, high reaction selectivity, low impurity content of the ethylene carbonate dichloride, high yield of the ethylene carbonate, and solves the difficult problem of difficult amplification of the process, thereby realizing the efficient, safe, rapid, energy-saving and easy-to-amplify production of the ethylene carbonate dichloride.
The invention solves the technical problems by the following technical proposal:
the invention provides a preparation method of chloroethylene carbonate, which is a continuous flow process and comprises the following steps:
s1: introducing ethylene carbonate and an initiator into the reaction unit, and then introducing chlorine to react to obtain a product A; wherein, the liquid crystal display device comprises a liquid crystal display device,
the temperature of the reaction unit is 80-140 ℃;
the molar ratio of the ethylene carbonate to the chlorine is 1: (1.2-2.0);
the pressure of the reaction is 4-18 bar;
the residence time of the reaction is 5 s-60 s;
s2: introducing the product A into a cooling unit, and then performing gas-liquid separation to obtain a chloroethylene carbonate crude product; wherein the temperature of the cooling section is 50-70 ℃.
In S1, the temperature of the reaction unit is preferably 80 to 120℃and more preferably 100 to 120 ℃.
In S1, the ethylene carbonate is solid at normal temperature, the melting point is about 40 ℃, and the ethylene carbonate can be fed after being heated and melted.
In S1, the mixed solution of the ethylene carbonate and the initiator can be introduced into the reaction unit through a constant flow pump, and the constant flow pump is preferably a plunger metering pump.
In S1, the mixed solution of the ethylene carbonate and the initiator can be introduced in a stable manner by adopting a continuous flow.
In S1, the flow rate of the mixed solution of the ethylene carbonate and the initiator can be 10-20 g/min.
In S1, the initiator is an initiator conventional in the art, preferably one or more of Azobisisobutyronitrile (AIBN), azobisisoheptonitrile, azoiso Ding Qingji formamide, benzoyl Peroxide (BPO) and benzoyl tert-butyl peroxide, and more preferably azobisisobutyronitrile or benzoyl peroxide.
In S1, the initiator preferably accounts for 0.05 to 0.5%, more preferably 0.05 to 0.3%, and still more preferably 0.08 to 0.12% of the total weight of the ethylene carbonate.
In S1, the chlorine is generally obtained by vaporizing liquid chlorine through vaporization.
In S1, the chlorine is introduced into the reaction unit through a flow meter.
In S1, the flow rate of the chlorine gas can be 9-28 g/min.
In S1, the reaction in the reaction unit is generally free radical chlorination reaction.
In S1, the molar ratio of the ethylene carbonate to the chlorine is preferably 1: (1.2 to 1.8), more preferably 1: (1.4-1.6).
In S1, the pressure of the reaction is preferably 4 to 15bar, more preferably 5 to 10bar. The pressure of the reaction system is improved, and the reaction can be greatly accelerated.
In S1, the pressure of the reaction is typically regulated by a back pressure valve.
In S1, the residence time of the reaction is preferably 10 to 50S, more preferably 20 to 30S.
In S1, the reaction unit may include a number of reactor modules. When the reactor modules are more than two, the reactor modules form a reactor module group by being connected in series or in parallel.
Wherein the reactor modules or the reactor module group can realize feeding, mixing, heat exchange and reaction.
Wherein the reactor module or the reactor module group can be provided with a plurality of material inlets and a plurality of material outlets.
Wherein the reactor module or the reactor module group can set a plurality of temperature zones.
In S1, the reactor module may comprise several continuous flow reactors, preferably comprising one or more of microreactors, tubular reactors, cascade mixers and static mixers. When the number of the reactors is more than two, the reactors are connected in series.
Wherein, the continuous flow reactor can also set a plurality of temperature zones.
Wherein the tubular reactor can be one or more of a single tube, a plurality of tubes connected in parallel, a hollow tube and a filling tube. The tubular reactor is a continuous operation reactor with a tubular shape and a large length-diameter ratio.
In S2, the temperature of the cooling unit is preferably 50 to 60 ℃, and more preferably 50 to 55 ℃.
In S2, the gas-liquid separation may be a gas-liquid separation method conventional in the art.
S2, the gas-liquid separation can further comprise a tail gas treatment step. The tail gas treatment step is used for treating hydrogen chloride and chlorine.
In S2, the crude chloroethylene carbonate can be directly used in the next process.
In S2, the crude product of the chloroethylene carbonate is preferably rectified to obtain a pure product of the chloroethylene carbonate. The purity of the chloroethylene carbonate pure product is 99% or more.
In the invention, the reaction unit adopts a modularized design (modular design), and molten ethylene carbonate and chlorine are used for one-time feeding (one-time feeding means that two materials continuously enter a continuous flow reactor at a preset flow), and the ethylene carbonate can be rapidly consumed (within ten seconds) by utilizing the optimization of a temperature area and reaction pressure and the synergistic effect of different functional units and utilizing the advantage of good heat and mass transfer of the continuous flow reactor, and meanwhile, the reaction liquid is rapidly cooled, so that the generation of ethylene carbonate dichloride impurities in the whole reaction process is effectively reduced, and the reaction is accelerated by controlling the temperature and the pressure.
On the basis of conforming to the common knowledge in the field, the above preferred conditions can be arbitrarily combined to obtain the preferred examples of the invention.
The reagents and materials used in the present invention are commercially available.
The invention has the positive progress effects that:
(1) According to the preparation method of the chloroethylene carbonate, the occurrence of back mixing is reduced by utilizing a continuous flow, and the cooling unit is used, so that the amount of the byproduct chloroethylene carbonate is controlled within 5%, and the purity of the product is improved.
(2) The preparation method of chloroethylene carbonate can conveniently and accurately control the pressure of a reaction system by using continuous flow, increases the solubility of chlorine in the reaction liquid continuously by increasing the pressure of the reaction system, accelerates the reaction rate, can finish the reaction within 10-50 s, shortens the residence time further, ensures that the reaction is more fully carried out, and ensures that the conversion rate of ethylene carbonate is maintained to be more than 90%.
(3) The preparation method of chloroethylene carbonate simplifies post-treatment operation and improves the stability in a system; the generation of hot spots in the exothermic reaction is effectively avoided, and the safety of the process is greatly improved; the good heat transfer and mass transfer effects are achieved by dividing a functional single temperature zone and controlling and optimizing the temperature; the high-temperature time in the reaction process is shortened, the energy consumption is reduced, and the cost is saved; the using amount of chlorine is effectively reduced, and the environment is protected; has no amplifying effect and can be directly amplified for industrial production.
Drawings
FIG. 1 is a process flow diagram of the process for preparing chloroethylene carbonate of examples 1 to 10 and comparative examples 1 to 5 of the present application.
Reference numerals:
1-a plunger metering pump; a 2-reaction unit; 3-a cooling unit; 4-back pressure valve; 5-a gas-liquid separation device; 6, a mixed liquor inlet; 7-chlorine inlet; 8-an exhaust gas outlet; and (3) a crude 9-chloroethylene carbonate product is discharged.
Detailed Description
The invention is further illustrated by means of the following examples, which are not intended to limit the scope of the invention. The experimental methods, in which specific conditions are not noted in the following examples, were selected according to conventional methods and conditions, or according to the commercial specifications.
FIG. 1 is a process flow diagram of the process for preparing chloroethylene carbonate of examples 1 to 10 and comparative examples 1 to 5 of the present application.
Examples
The preparation methods of chloroethylene carbonate of examples 1 to 10 and comparative examples 1 to 5 are as follows:
s1: setting the temperature of a reaction unit of the continuous flow reactor;
heating ethylene carbonate to about 50 ℃ to be in a liquid state, and introducing the ethylene carbonate and a certain amount of initiator into the reaction unit 2 through a mixed solution inlet 6 by a plunger metering pump 1 to adjust the flow rate of the mixed solution;
the liquid chlorine is gasified by a gasification tank, and the chlorine is introduced into the reaction unit 2 through a chlorine inlet after being metered by a flowmeter, so as to adjust the flow rate of the chlorine and control the mole ratio of the ethylene carbonate to the chlorine;
the reaction unit is a continuous flow reactor;
the reaction pressure is regulated by a back pressure valve 4; and (3) carrying out a reaction to obtain a product A.
S2: setting the temperature of a cooling unit 3, introducing a product A into the cooling unit 3, introducing the product A into a gas-liquid separation device 5 for gas-liquid separation, obtaining a chloroethylene carbonate crude product at a chloroethylene carbonate crude product outlet 9 after the separation, and introducing waste gas generated from a waste gas outlet 8 into a tail gas treatment system; further rectifying and purifying the crude product of the chloroethylene carbonate to obtain a pure product of the chloroethylene carbonate.
Examples 1-10 and comparative examples 1-5 used the preparation methods described above, but different reaction conditions were set to give different product effects, as shown in Table 1. Table 1 shows the reaction parameters and the effects of the products of examples 1-10 and comparative examples 1-5.
TABLE 1
Effect examples
The residual amount after the reaction of the vinyl carbonate, the content of the ethylene dichloride carbonate, and the like in the crude products of the vinyl chloride carbonate of examples 1 to 10 and comparative examples 1 to 5 were detected by a detection method conventional in the art, and the purity and yield of the pure product of the vinyl chloride carbonate were obtained by calculation, and specific data are shown in table 2. Table 2 shows the results of the crude chloroethylene carbonate products of examples 1 to 10 and comparative examples 1 to 5.
TABLE 2
The embodiments 1-10 of the invention adopt the preparation method of chloroethylene carbonate, the residual amount of the ethylene carbonate after the reaction is more than 90%, namely the conversion rate of the ethylene carbonate is more than 90%; the process conditions of comparative examples 1 and 4, in which the residual amount of ethylene carbonate was more than 10%, resulted in waste of raw materials. The content of the dichloro ethylene carbonate impurity in the crude product prepared by the method can be controlled within 5.0%, so that the purity of the crude product is improved. In the subsequent gas-liquid separation, the chloroethylene carbonate crude product is further rectified and purified to obtain a final product, the product yield can reach more than 93 percent, and the product purity can reach more than 99 percent.
Claims (10)
1. A process for the preparation of chloroethylene carbonate, characterized in that the process for the preparation of chloroethylene carbonate is a continuous flow process comprising the steps of:
s1: introducing ethylene carbonate and an initiator into the reaction unit, and then introducing chlorine to react to obtain a product A; wherein, the liquid crystal display device comprises a liquid crystal display device,
the temperature of the reaction unit is 80-140 ℃;
the molar ratio of the ethylene carbonate to the chlorine is 1: (1.2-2.0);
the pressure of the reaction is 4-18 bar;
the residence time of the reaction is 5 s-60 s;
s2: introducing the product A into a cooling unit, and then performing gas-liquid separation to obtain a chloroethylene carbonate crude product; wherein the temperature of the cooling unit is 50-70 ℃.
2. The method for producing chloroethylene carbonate according to claim 1, wherein in S1, the temperature of the reaction unit is 80 to 120 ℃;
and/or the initiator is one or more of azodiisobutyronitrile, azodiisoheptonitrile, azoi Ding Qingji formamide, benzoyl peroxide and benzoyl peroxide tert-butyl ester;
and/or, the initiator accounts for 0.05-0.5% of the total weight of the ethylene carbonate.
3. The method for producing chloroethylene carbonate according to claim 2, wherein in S1, the temperature of the reaction unit is 100 to 120 ℃;
and/or the initiator is azodiisobutyronitrile or benzoyl peroxide;
and/or the initiator comprises 0.05 to 0.3%, preferably 0.08 to 0.12% of the total weight of the ethylene carbonate.
4. The method for preparing chloroethylene carbonate according to claim 1, wherein in S1, the ethylene carbonate and an initiator are introduced into the reaction unit through a constant flow pump;
and/or the ethylene carbonate and the initiator are introduced in a continuous flow stable way;
and/or introducing the chlorine gas into the reaction unit through a flow meter;
and/or the pressure of the reaction is regulated by a back pressure valve.
5. The method for producing chloroethylene carbonate according to claim 1, wherein in S1, the molar ratio of the ethylene carbonate to the chlorine gas is 1: (1.2-1.8);
and/or the pressure of the reaction is 4-15 bar;
and/or the residence time of the reaction is 10 to 50s.
6. The method for producing chloroethylene carbonate according to claim 5, wherein in S1, the molar ratio of the ethylene carbonate to the chlorine gas is 1: (1.4-1.6);
and/or the pressure of the reaction is 5-10 bar;
and/or the residence time of the reaction is 20-30 s.
7. The method for producing chloroethylene carbonate according to claim 1, wherein in S1, the reaction unit comprises a plurality of reactor modules;
when the reactor modules are more than two, the reactor modules form a reactor module group by being connected in series or in parallel;
wherein the reactor module or the reactor module group is provided with a plurality of material inlets and a plurality of material outlets;
wherein the reactor module or the reactor module group is provided with a plurality of temperature areas.
8. The process for the preparation of chloroethylene carbonate according to claim 7, wherein in S1 the reactor module comprises a number of continuous flow reactors, preferably one or more of microreactors, tubular reactors, cascade mixers and static mixers;
when the number of the reactors is more than two, the reactors are mutually connected in series;
wherein the continuous flow reactor is provided with a plurality of temperature areas;
wherein the tubular reactor is one or more of a single tube, a plurality of tubes connected in parallel, a hollow tube and a filling tube.
9. The process for preparing chloroethylene carbonate according to claim 1, wherein in S2, the temperature of the cooling unit is 50 to 60 ℃, preferably 50 to 55 ℃.
10. The method for preparing chloroethylene carbonate according to claim 1, wherein in S2, the step of treating tail gas is further included after the gas-liquid separation;
and/or rectifying the crude product of the chloroethylene carbonate to obtain a pure product of the chloroethylene carbonate.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210199593 | 2022-03-02 | ||
| CN2022101995933 | 2022-03-02 |
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| Publication Number | Publication Date |
|---|---|
| CN116462655A true CN116462655A (en) | 2023-07-21 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202310189025.XA Pending CN116462655A (en) | 2022-03-02 | 2023-03-01 | Process for preparing chloroethylene carbonate |
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| CN (1) | CN116462655A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117263901A (en) * | 2023-11-21 | 2023-12-22 | 山东海化集团有限公司 | Method for continuously producing vinylene carbonate |
-
2023
- 2023-03-01 CN CN202310189025.XA patent/CN116462655A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117263901A (en) * | 2023-11-21 | 2023-12-22 | 山东海化集团有限公司 | Method for continuously producing vinylene carbonate |
| CN117263901B (en) * | 2023-11-21 | 2024-04-05 | 山东海化集团有限公司 | Method for continuously producing vinylene carbonate |
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