CN113559804A - Vinylene carbonate manufacturing equipment - Google Patents

Vinylene carbonate manufacturing equipment Download PDF

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Publication number
CN113559804A
CN113559804A CN202111104273.7A CN202111104273A CN113559804A CN 113559804 A CN113559804 A CN 113559804A CN 202111104273 A CN202111104273 A CN 202111104273A CN 113559804 A CN113559804 A CN 113559804A
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China
Prior art keywords
tower
communicated
triethylamine
solvent
recovery tower
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Pending
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CN202111104273.7A
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Chinese (zh)
Inventor
张风收
滕文彬
张生安
杜桂强
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Shandong Haike Xinyuan Material Technology Co Ltd
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Shandong Haike Xinyuan Material Technology Co Ltd
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Priority to CN202111104273.7A priority Critical patent/CN113559804A/en
Publication of CN113559804A publication Critical patent/CN113559804A/en
Pending legal-status Critical Current

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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/009Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18Stationary reactors having moving elements inside
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J4/00Feed or outlet devices; Feed or outlet control devices
    • B01J4/02Feed or outlet devices; Feed or outlet control devices for feeding measured, i.e. prescribed quantities of reagents
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C209/00Preparation of compounds containing amino groups bound to a carbon skeleton
    • C07C209/82Purification; Separation; Stabilisation; Use of additives
    • C07C209/86Separation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D317/00Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
    • C07D317/08Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
    • C07D317/10Heterocyclic 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
    • C07D317/32Heterocyclic 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
    • C07D317/34Oxygen atoms
    • C07D317/40Vinylene carbonate; Substituted vinylene carbonates
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00002Chemical plants
    • B01J2219/00004Scale aspects
    • B01J2219/00006Large-scale industrial plants

Abstract

The invention relates to the technical field of vinylene carbonate processing and manufacturing, and discloses vinylene carbonate manufacturing equipment, which comprises a VC synthesis reaction kettle, wherein the bottom of the VC synthesis reaction kettle is communicated with a filter press, a filter cake outlet on the filter press is communicated with a dissolver through a dryer, a filtrate outlet on the filter press is communicated with the middle part of a solvent recovery tower, the top of the solvent recovery tower is communicated with a solvent head tank, the bottom of the solvent recovery tower is communicated with the middle part of an evaporator, the bottom of a lightness-removing tower is communicated with the middle part of a refining tower, the side of the outer wall of the refining tower is communicated with a VC product tank, and the top of the refining tower and the top of the evaporator are both communicated with the middle part of the lightness-removing tower; the invention has reasonable structural design, reduces the possibility of environmental pollution caused by the unorganized diffusion of volatile peculiar smell components, reduces the possibility of blocking and damaging used equipment, and improves the recovery efficiency of triethylamine.

Description

Vinylene carbonate manufacturing equipment
Technical Field
The invention relates to the technical field of vinylene carbonate processing and manufacturing, in particular to vinylene carbonate manufacturing equipment.
Background
The electrolyte additive is one of four key components of the lithium battery and one of main components of the electrolyte, can obviously improve the performance of the battery, provides special functions for the lithium battery under different application environments, and benefits from the rapid growth of the lithium battery to further promote the rapid growth of the industry demand of the lithium battery additive.
Vinylene carbonate, also known as 1, 3-dioxol-2-one and ethylene carbonate, VC for short, is colorless transparent liquid, is a key variety in numerous products of lithium battery additives, and is the most suitable variety for improving the safety and stability of lithium batteries. The addition of a proper amount of vinylene carbonate into the battery can obviously improve SEI film forming characteristics, prevent air expansion, improve the cycle performance of the battery, improve the low-temperature performance of electrolyte, and improve the capacity, platform, cycle and other performances of the lithium battery.
The problems existing in the prior art are as follows:
firstly, in the prior art, a plate-frame filter is adopted to carry out solid-liquid separation on a crude product after reaction, in the actual operation process, as the plate-frame filter is not a closed device, the smell of a filter cake is high, and particularly, after the temperature is higher than 20 ℃, volatile peculiar smell components can be diffused around without tissues, so that the environmental pollution is caused;
secondly, in the triethylamine recovery process in the prior art, the recovery efficiency is low;
in the prior art, the solvent is directly fed into a rectifying device after being recovered, but polymers such as partial polyacetylene, poly (ethylene carbonate) and the like can be generated in the reaction process and are viscous, and the reboiler is easily blocked by direct rectification after the solvent is recovered.
Therefore, a vinylene carbonate manufacturing device is provided.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provide a vinylene carbonate manufacturing device, which can reduce the possibility of environmental pollution caused by the unorganized diffusion of volatile odor components, reduce the possibility of blockage and damage to used equipment and improve the recovery efficiency of triethylamine.
In order to achieve the technical purpose and achieve the technical effect, the invention is realized by the following technical scheme:
a manufacturing device of vinylene carbonate comprises a VC synthesis reaction kettle, a chlorinated ethylene carbonate head tank, a solvent head tank, a triethylamine head tank, a filter press, a dryer, a condenser, a dissolver, a triethylamine recovery tower, a solvent recovery tower, an evaporator, a lightness-removing tower and a refining tower, wherein the triethylamine head tank, the solvent head tank and the chlorinated ethylene carbonate head tank are respectively arranged on one side above the VC synthesis reaction kettle, the bottom of the VC synthesis reaction kettle is communicated with the filter press, a filter cake outlet on the filter press is communicated with the dissolver through the dryer, a filtrate outlet on the filter press is communicated with the middle part of the solvent recovery tower, the tower top of the solvent recovery tower is communicated with the solvent head tank, the bottom of the solvent recovery tower is communicated with the middle part of the evaporator, the bottom of the lightness-removing tower is communicated with the middle part of the refining tower, and the side of the outer wall of the refining tower is communicated with a VC product tank, the top of the refining tower and the top of the evaporator are both communicated with the middle part of the light component removal tower, an oil layer outlet on the dissolver is communicated with the middle part of the triethylamine recovery tower, and the top of the triethylamine recovery tower is communicated with the triethylamine head tank.
Preferably, a condenser is arranged on the other side above the VC synthesis reaction kettle, and the outlet of the condenser is communicated with the activated carbon fiber adsorption system.
Based on the technical characteristics, the organic volatile matters in the VC synthesis reaction kettle are convenient to condense and recover, the emission of organic matters is reduced, and the utilization rate of raw materials is improved.
Preferably, an air suction cover is arranged above the filter press, and an outlet of the air suction cover is communicated with the activated carbon fiber adsorption system.
Based on the technical characteristics, the volatile components are absorbed by the air suction hood and then absorbed by the activated carbon fiber absorption system, so that the unorganized emission of the volatile components is reduced.
Preferably, the evaporator is one of a rising film evaporator, a falling film evaporator and a scraper evaporator.
Based on the technical characteristics, the evaporator is convenient to use.
Preferably, the triethylamine recovery tower, the solvent recovery tower, the light component removal tower and the refining tower are all packed towers with tower plates, the number of the tower plates in the triethylamine recovery tower and the light component removal tower is 20-25, the number of the tower plates in the solvent recovery tower is 15-25, and the number of the tower plates in the refining tower is 30-40.
Preferably, the dryer is one of a convection dryer, a conduction dryer, a radiant dryer, a dielectric dryer.
Based on the technical characteristics, the dryer is convenient to use.
Compared with the prior art, the invention has the following beneficial effects:
the invention has reasonable structural design, and one specific application of the embodiment is as follows: firstly, the method comprises the following steps: the reaction materials in the VC synthesis kettle are subjected to solid-liquid separation by the filter press through the cooperation of the filter press and the dryer, the separated filtrate enters the solvent recovery tower, and the separated solid filter cake is dried by the dryer and then is sent into the dissolver, so that the possibility of environmental pollution caused by the unorganized diffusion of volatile peculiar smell components is reduced;
and secondly, the possibility of blocking and damaging used equipment is reduced by matching the solvent recovery tower, the evaporator, the lightness-removing tower and the refining tower, and the recovery efficiency of triethylamine is improved by matching the dissolver and the triethylamine recovery tower.
Of course, it is not necessary for any product in which the invention is practiced to achieve all of the above-described advantages at the same time.
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 will be briefly introduced below, and it is obvious that the drawings in the following description 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 structural diagram of a use state of the present invention;
in the drawings, the components represented by the respective reference numerals are listed below:
the method comprises the following steps of 1-VC synthesis reaction kettle, 2-chloroethylene carbonate head tank, 3-solvent head tank, 4-triethylamine head tank, 5-filter press, 6-dryer, 7-condenser, 8-dissolver, 9-triethylamine recovery tower, 10-solvent recovery tower, 11-evaporator, 12-lightness removing tower and 13-refining tower.
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, a manufacturing device of vinylene carbonate comprises a VC synthesis reaction kettle 1, a vinyl chloride carbonate head tank 2, a solvent head tank 3, a triethylamine head tank 4, a filter press 5, a dryer 6, a condenser 7, a dissolver 8, a triethylamine recovery tower 9, a solvent recovery tower 10, an evaporator 11, a lightness-removing tower 12 and a refining tower 13, wherein the triethylamine head tank 4, the solvent head tank 3 and the vinyl chloride carbonate head tank 2 are respectively arranged on one side above the VC synthesis reaction kettle 1, the condenser 7 is arranged on the other side above the VC synthesis reaction kettle 1, an outlet of the condenser 7 is communicated with an activated carbon fiber adsorption system, so that organic volatile matters in the VC synthesis reaction kettle 1 can be conveniently condensed and recovered, the emission of organic matters is reduced, the utilization rate of raw materials is improved, the bottom of the VC synthesis reaction kettle 1 is communicated with the filter press 5, an air suction hood is arranged above the filter press 5, and the outlet of the air suction hood is communicated with an activated carbon fiber adsorption system, volatile components are absorbed by the air suction hood and then absorbed by the activated carbon fiber adsorption system (the activated carbon fiber adsorption system adopts the prior art and is not shown in the figure), the unorganized emission of the volatile components is reduced, the outlet of a filter cake on the filter press 5 is communicated with a dissolver 8 through a dryer 6, the dryer 6 is one of a convection dryer, a conduction dryer, a radiation dryer and a dielectric dryer, the use of the dryer 6 is convenient, the filtrate outlet on the filter press 5 is communicated with the middle part of a solvent recovery tower 10, the tower top of the solvent recovery tower 10 is communicated with a solvent head tank 3, the bottom of the solvent recovery tower 10 is communicated with the middle part of an evaporator 11, the bottom of a lightness removing tower 12 is communicated with the middle part of a refining tower 13, the side of the outer wall of the refining tower 13 is communicated with a VC product tank, the top of the refining tower 13 and the top of the evaporator 11 are both communicated with the middle of the light component removal tower 12, the evaporator 11 is one of a rising film evaporator, a falling film evaporator and a scraper evaporator, the evaporator 11 is convenient to use, an oil layer outlet on the dissolver 8 is communicated with the middle of the triethylamine recovery tower 9, the top of the triethylamine recovery tower 9 is communicated with the triethylamine head tank 4, the triethylamine recovery tower 9, the solvent recovery tower 10, the light component removal tower 12 and the refining tower 13 are all packed towers with tower plates, the number of the tower plates in the triethylamine recovery tower 9 and the light component removal tower 12 is 20-25, the number of the tower plates in the solvent recovery tower 10 is 15-25, and the number of the tower plates in the refining tower 13 is 30-40.
One specific application of this embodiment is: the invention has reasonable structural design, firstly, a certain amount of triethylamine, dimethyl carbonate and chloroethylene carbonate are respectively added into a corresponding triethylamine head tank 4, a solvent head tank 3 and a chloroethylene carbonate head tank 2 by a pump, then the dimethyl carbonate and the chloroethylene carbonate are measured and put into a VC synthesis reaction kettle 1, a heating system is started after uniform stirring, the VC synthesis kettle 1 is heated to 60-80 ℃ by heat-conducting oil, then the triethylamine is dripped into the VC synthesis reaction kettle 1, the reaction is continued for 2h after the triethylamine is dripped, after the reaction is finished, the synthesis reaction kettle 1 is cooled to normal temperature, the materials are discharged into a filter press 5 from the bottom of the synthesis reaction kettle 1, solid-liquid separation is carried out by the filter press 5, volatilized organic matters are condensed and then flow back into the synthesis reaction kettle 1 by a condenser 7 arranged above the synthesis reaction kettle 1, the residual non-condensable gas enters an activated carbon fiber adsorption system;
the filtrate separated by the filter press 5 enters a solvent recovery tower 10, the vacuum degree is controlled to be 10Kpa, the temperature of the top of the tower is 45 ℃, the temperature of the bottom of the tower is 60 ℃, the excessive dimethyl carbonate in the filtrate is convenient to recover, the dimethyl carbonate returns to a solvent head tank 3, vinylene carbonate with the purity of more than 80 percent obtained at the bottom of the tower enters an evaporator 11, vinylene carbonate with the purity of more than 90 percent obtained at the top of the evaporator 11 enters a light component removal tower 12, the vacuum degree of the light component removal tower 12 is controlled to be 5Kpa, the temperature of the top of the tower is 80 ℃, the temperature of the bottom of the tower is 110 ℃, light component separation is carried out, the vinylene carbonate with the purity of more than 99 percent obtained at the bottom of the tower enters a refining tower 13, the vacuum degree of the refining tower 13 is controlled to be 5Kpa, the temperature of the top of the tower is 80 ℃, the temperature of the bottom of the tower is 110 ℃, the VC product tank is used for extracting high-purity vinylene carbonate with the purity of more than 99.99 percent from the side of the outer wall of the VC product tank, so that the possibility of blockage and damage to used equipment is greatly reduced;
filter cakes separated by the filter press 5 are dried by a dryer 6 and then enter a dissolver 8, so that the possibility of environmental pollution caused by the unorganized diffusion of volatile peculiar smell components is reduced, then a certain amount of potassium hydroxide is added after water is added into the dissolver 8 for dissolving, triethylamine hydrochloride is neutralized into triethylamine, the triethylamine and the water-insoluble characteristic is utilized for standing and layering, the upper oil phase is a mixture of triethylamine, ethylene carbonate, polyvinyl carbonate and the like, the lower layer is a sodium chloride aqueous solution, and the sodium chloride aqueous solution enters a sodium chloride refining system to obtain a byproduct sodium chloride;
the mixture of triethylamine, ethylene carbonate, polyethylene carbonate and the like on the upper layer enters a triethylamine recovery tower 9, triethylamine is recovered and sent to a triethylamine head tank 4, and the triethylamine recovery efficiency is more than 90 percent, so that the triethylamine recovery efficiency is greatly improved.
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 (6)

1. The utility model provides a preparation of vinylene carbonate is equipped, includes VC synthetic reation kettle (1), chlorinated ethylene carbonate elevated tank (2), solvent elevated tank (3), triethylamine elevated tank (4), pressure filter (5), desicator (6), condenser (7), dissolvent (8), triethylamine recovery tower (9), solvent recovery tower (10), evaporimeter (11), lightness-removing column (12) and refined tower (13), its characterized in that: a triethylamine elevated tank (4), a solvent elevated tank (3) and a chloroethylene carbonate elevated tank (2) are respectively arranged on one side above the VC synthesis reaction kettle (1), the bottom of the VC synthesis reaction kettle (1) is communicated with a filter press (5), a filter cake outlet on the filter press (5) is communicated with a dissolver (8) through a dryer (6), a filtrate outlet on the filter press (5) is communicated with the middle part of a solvent recovery tower (10), the top of the solvent recovery tower (10) is communicated with the solvent elevated tank (3), the bottom of the solvent recovery tower (10) is communicated with the middle part of an evaporator (11), the bottom of a lightness-removing tower (12) is communicated with the middle part of the refining tower (13), the outer wall side of the refining tower (13) is communicated with a VC product tank, the top of the refining tower (13) and the top of the evaporator (11) are both communicated with the middle part of the lightness-removing tower (12), an oil layer outlet on the dissolver (8) is communicated with the middle part of the triethylamine recovery tower (9), and the tower top of the triethylamine recovery tower (9) is communicated with the triethylamine head tank (4).
2. The vinylene carbonate manufacturing equipment according to claim 1, wherein: a condenser (7) is arranged on the other side above the VC synthesis reaction kettle (1), and the outlet of the condenser (7) is communicated with an activated carbon fiber adsorption system.
3. The vinylene carbonate manufacturing equipment according to claim 1, wherein: an air suction cover is arranged above the filter press (5), and the outlet of the air suction cover is communicated with the activated carbon fiber adsorption system.
4. The vinylene carbonate manufacturing equipment according to claim 1, wherein: the evaporator (11) is one of a rising film evaporator, a falling film evaporator and a scraper evaporator.
5. The vinylene carbonate manufacturing equipment according to claim 1, wherein: the triethylamine recovery tower (9), the solvent recovery tower (10), the light component removal tower (12) and the refining tower (13) are all packed towers with tower plates, the number of the tower plates in the triethylamine recovery tower (9) and the light component removal tower (12) is 20-25, the number of the tower plates in the solvent recovery tower (10) is 15-25, and the number of the tower plates in the refining tower (13) is 30-40.
6. The vinylene carbonate manufacturing equipment according to claim 1, wherein: the dryer (6) is one of a convection dryer, a conduction dryer, a radiation dryer and a dielectric dryer.
CN202111104273.7A 2021-09-22 2021-09-22 Vinylene carbonate manufacturing equipment Pending CN113559804A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114315786A (en) * 2021-12-20 2022-04-12 上海晋瑄智能设备制造有限公司 Process method for solid-liquid separation and recovery of vinylene carbonate reaction liquid

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Application publication date: 20211029