CN208617728U - A kind of crystallization apparatus for ethylene carbonate purification purification - Google Patents

A kind of crystallization apparatus for ethylene carbonate purification purification Download PDF

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Publication number
CN208617728U
CN208617728U CN201820798660.2U CN201820798660U CN208617728U CN 208617728 U CN208617728 U CN 208617728U CN 201820798660 U CN201820798660 U CN 201820798660U CN 208617728 U CN208617728 U CN 208617728U
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China
Prior art keywords
crystallizer
purification
ethylene carbonate
embedded
external
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Expired - Fee Related
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CN201820798660.2U
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Chinese (zh)
Inventor
许兆石
李守芬
张军
陈明明
庄昊
徐东
李洋
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LIAONING GANGLONG CHEMICAL Co Ltd
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LIAONING GANGLONG CHEMICAL Co Ltd
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Abstract

The utility model discloses a kind of crystallization apparatus for ethylene carbonate purification purification, including external crystallizer and embedded crystallizer, embedded crystallizer top is equipped with cloth liquid disk, and bottom end is equipped with catch tray;Cloth liquid disk upper end is equipped with circulation fluid inlet tube, is connected with circulation pipe between circulation fluid inlet tube and circulation fluid outlet tube;Crystallizer is equipped in embedded crystallizer, and the feed end of each crystallizer is connected to the fluid hole of cloth liquid disk, the discharge end of each crystallizer is connected to the inlet opening of catch tray;Heat exchange jacket is provided with outside external crystallizer, the lower end of heat exchange jacket side is equipped with heat transferring medium inlet tube, and the upper end of the opposite other side is equipped with heat transferring medium outlet.Purifying plant structure provided by the utility model is simple, it is easy to use, the ethylene carbonate of purifying technique purification can be refined, product purity is up to 99.99% or more after purification, indices are further promoted, and fully meet the index request of lithium-ion battery electrolytes solvent application.

Description

A kind of crystallization apparatus for ethylene carbonate purification purification
Technical field
The utility model belongs to technical field of fine, and in particular to a kind of knot for ethylene carbonate purification purification Brilliant device.
Background technique
Lithium battery electrolytes are the important source materials for making lithium battery, and ethylene carbonate is that dosage is maximum in lithium battery electrolytes Solvent, therefore, in the manufacturing process of lithium battery, to the quality requirements pole of the ethylene carbonate for lithium battery electrolytes Height, most important one are a little that all kinds of impurity contents contained in ethylene carbonate are required to lower than 10 μ g/g.In recent years, with The growth requirement of new energy resource power battery, the requirement to the purity of ethylene carbonate will be higher and higher.
At present in industrial production, the mode for generalling use rectifying removes impurity in ethylene carbonate, and mentions by rectifying After pure, the purity of ethylene carbonate can reach 99.95% or so.But there are energy consumption height, significant loss for the technique of rectification and purification Amount is big, operation large labor intensity and the problems such as unstable product quality, and therefore, pole is a kind of new for carbon it is necessary to develop The device of vinyl acetate purification purification, can be while highly purified ethylene carbonate, moreover it is possible to solve above-mentioned drawback.
Utility model content
The purpose of the utility model is to provide a kind of crystallization apparatus for ethylene carbonate purification purification, solve existing Use rectification method purification ethylene carbonate there are energy consumption height in technology, significant loss amount is big, operates large labor intensity and product The problem of unstable quality.
The utility model provides a kind of crystallization apparatus for ethylene carbonate purification purification, including external crystallizer And coaxial sleeve is set to the embedded crystallizer in the external crystallizer, the top of the external crystallizer is equipped with top End socket, bottom end are equipped with bottom head, and the top end socket is equipped with feed pipe, and the bottom head is equipped with circulation fluid and goes out liquid Pipe;
The bottom of the embedded crystallizer and the bottom head are affixed, and the top of the embedded crystallizer is equipped with cloth Liquid disk, bottom end are equipped with catch tray;The upper end of the cloth liquid disk is equipped with circulation fluid inlet tube, and the circulation fluid inlet tube is followed with described It is connected with circulation pipe between ring liquid outlet tube, is additionally provided with circulating pump on the circulation pipe;The lower end of the catch tray is equipped with discharging Pipe, the discharge nozzle are equipped with valve;
In the embedded crystallizer longitudinally be equipped with multiple crystallizers, and the feed end of each crystallizer with it is described The fluid hole of cloth liquid disk is connected to, and the discharge end of each crystallizer is connected to the inlet opening of the catch tray;
It is provided with heat exchange jacket outside the external crystallizer, the lower end of the heat exchange jacket side enters equipped with heat transferring medium The upper end of mouth pipe, the opposite other side is equipped with heat transferring medium outlet.
Preferably, the bottom end of the external crystallizer is additionally provided with 3-4 supporting leg.
Preferably, temperature sensor is equipped in the external crystallizer.
Preferably, the external crystallizer and the embedded crystallizer are cylindrical-shaped structure.
Preferably, the circulating pump is one of metering pump, turbulence pump or centrifugal pump.
Compared with prior art, the utility model has the beneficial effects that:
The utility model setting external crystallizer and embedded crystallizer are used cooperatively crystallize ethylene carbonate, In, external crystallizer can control the temperature of ethylene carbonate in external crystallizer, to accurately control embedded crystallization The temperature of ethylene carbonate in device avoids ethylene carbonate temperature change in embedded crystallizer big, to influence crystallization effect; The multiple groups crystallizer being arranged in embedded crystallizer provides attachment point for ethylene carbonate crystallization, so that nucleus is quickly formed, into And promote the formation of mass crystallization body.
Apparatus structure provided by the utility model is simple, easy to use, can refine the ethylene carbonate of purifying technique purification Ester, up to 99.99% or more, indices are further promoted product purity after purification, fully meet lithium-ion battery electrolytes The index request of solvent application.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the crystallization apparatus provided by the utility model for ethylene carbonate purification purification;
Fig. 2 is the structure of the cloth liquid disk in the crystallization apparatus provided by the utility model for ethylene carbonate purification purification Schematic diagram;
Fig. 3 is cloth liquid disk and crystallization in the crystallization apparatus provided by the utility model for ethylene carbonate purification purification The structural schematic diagram of pipe.
Description of symbols:
1- external crystallizer, the embedded crystallizer of 2-, 3- feed pipe, 4- circulation fluid outlet tube, 5- cloth liquid disk, 6- liquid collecting Disk, 7- circulation fluid inlet tube, 8- circulation pipe, 9- circulating pump, 10- discharge nozzle, 11- valve, 12- crystallizer, 13- heat exchange jacket, 14- heat transferring medium inlet tube, 15- heat transferring medium outlet, 16- supporting leg.
Specific embodiment
With reference to the accompanying drawing, specific embodiment of the present utility model is described in detail, it is to be understood that this is practical Novel protection scope is not limited by the specific implementation.
A kind of crystallization apparatus for ethylene carbonate purification purification, specifically as shown in Figure 1-3, including cylindrical-shaped structure External crystallizer 1 and coaxial sleeve are set to the embedded crystallizer 2 of the cylindrical-shaped structure in external crystallizer 1, external The top of crystallizer 1 is equipped with top end socket, and bottom end is equipped with bottom head, and top end socket is equipped with feed pipe 3, sets on bottom head There is circulation fluid outlet tube 4;
The bottom of embedded crystallizer 2 and bottom head are affixed, and the top of embedded crystallizer 2 is equipped with cloth liquid disk 5, bottom end Equipped with catch tray 6;The upper end of cloth liquid disk 5 is equipped with circulation fluid inlet tube 7, connects between circulation fluid inlet tube 7 and circulation fluid outlet tube 4 It is connected to circulation pipe 8, circulating pump 9 is additionally provided on circulation pipe 8, circulating pump 9 is one of metering pump, turbulence pump or centrifugal pump;Collection The lower end of liquid disk 6 is equipped with discharge nozzle 10, and discharge nozzle 10 is equipped with valve 11;
In embedded crystallizer 2 longitudinally be equipped with multiple crystallizers 12, and the feed end of each crystallizer 12 with cloth liquid disk 5 Fluid hole connection, the discharge end of each crystallizer 12 is connected to the inlet opening of catch tray 6, and cloth liquid disk 5 and catch tray 6 Structure is identical;
Heat exchange jacket 13 is provided with outside external crystallizer 1, the lower end of 13 side of heat exchange jacket is equipped with heat transferring medium entrance The upper end of pipe 14, the opposite other side is equipped with heat transferring medium outlet 15.
The application method of the utility model is as follows: under a certain pressure, by the ethylene carbonate of a certain amount of purification to be refined Ester liquid is added in external crystallizer 1 through feed pipe 3, is then sent ethylene carbonate by cloth liquid disk 5 using circulating pump 9 Enter in the crystallizer 12 in embedded crystallizer 2, and makes ethylene carbonate in crystallizer 12 in a manner of liquid film under stream;In carbonic acid During vinyl acetate enters crystallizer 12, the temperature in external crystallizer 1 is gradually reduced, ethylene carbonate is made to enter crystallization After pipe 12, crystallizing layer is formed in the inner wall of crystallizer 12, and when the temperature in external crystallizer 1 is down to 32-34 DEG C, stop Only cool down, is simultaneously stopped to crystallizer 12 and feeds, 0.5-2h is then kept the temperature, after heat preservation, by uncrystallized ethylene carbonate Then and the ethylene carbonate after rectifying column purifies mother liquor is collected by catch tray 6, is then discharged and is collected from discharge nozzle 10, Mixing enters in external crystallizer 1 to lower batch and continues to crystallize;After uncrystallized ethylene carbonate mother liquor drains, gradually rise Temperature in high external crystallizer 1 makes the crystallizing layer generated in crystallizer 12 melting, when temperature liter in external crystallizer 1 When to 34-36 DEG C, stop heating, and keep the temperature 0.5-2h, heat preservation finishes, and by molten liquid discharge, collects and is greater than to get to purity 99.99% ethylene carbonate;Meanwhile after ethylene carbonate molten liquid of the purity greater than 99.99% drains, continue to increase outer The temperature in formula crystallizer 1 is set, melts remaining crystallizing layer in crystallizer 12 all, the crystalline solid of fusing is from 10 row of discharge nozzle Out, that is, the purifying of ethylene carbonate is completed.
In the utility model, 13 internal circulation flow of heat exchange jacket heating agent or refrigerant, by heating agent or refrigerant control it is external The temperature of ethylene carbonate in formula crystallizer 1, since the volume of external crystallizer 1 is big, even if by carbon in external crystallizer 1 The temperature of vinyl acetate is adjusted to 32-34 DEG C, and ethylene carbonate and impurity are also difficult to crystallize wherein, that is, allows to crystallize, also need System temperature is down to crystallization time that is very low, while also needing to grow very much.In addition, even if ethylene carbonate and impurity are complete Portion crystallizes, and in external crystallizer 1 so big volume space, also has no idea carbonic acid through the method for fractional melting Vinyl acetate and impurity separate.
Multiple crystallizers 12 are longitudinally equipped in embedded crystallizer 2, the ethylene carbonate in external crystallizer 1 is from cloth liquid Disk 5 enters crystallizer 12, and the feed end of each crystallizer 12 is connected to the fluid hole of cloth liquid disk 5, i.e., all carbonic acid second Enester enters in crystallizer 12, since crystallizer 12 is slim-lined construction, when temperature is down to ethylene carbonate and impurity crystallization temperature When spending, it is easy to the tube wall attachment crystallization in crystallizer 12, meanwhile, after tube wall adheres to crystalline solid, as crystal seed, it is easy to promote It crystallizes more raw materials near crystal seed, to quickly form crystallizing layer, completes crystallization.The surplus material not crystallized then from Discharge nozzle 10 is discharged and collects, and then mixes with ethylene carbonate to be crystallized, enters in external crystallizer 1 to lower batch and continues Crystallization.
Within the temperature range of 32-34 DEG C, ethylene carbonate and impurity are in crystalline state, but due to the carbonic acid of crystal state Vinyl acetate is i.e. fusible in 34-36 DEG C, and impurity needs higher temperature that could melt, this just for both separation provide Condition.When operation, the temperature in external crystallizer 1 is risen to 34-36 DEG C first, to make embedded crystallizer 2 Interior temperature is also stabilized in 34-36 DEG C, at this point, ethylene carbonate all melts, is discharged and collects from discharge nozzle 10.It is remaining Not melting is impurity, continues to increase temperature, melts the impurity of lenticular and collects, that is, completes a purification process, then Aforesaid operations are repeated, the purification of ethylene carbonate is continued.
It should be noted that the bottom end of external crystallizer 1 is additionally provided with 3-4 supporting leg 16, for supporting whole device, make Its firm work.
Temperature sensor is equipped in external crystallizer 1, temperature sensor can detecte the temperature in external crystallizer 1 Degree makes it meet technique requirement to accurately control the temperature in embedded crystallizer 2.
In the utility model, disclosed above is only specific embodiment of the utility model, and still, the utility model is implemented Example is not limited to this, and the changes that any person skilled in the art can think of should all fall into the protection scope of the utility model.

Claims (5)

1. a kind of crystallization apparatus for ethylene carbonate purification purification, which is characterized in that including external crystallizer (1) and Coaxial sleeve is set to the embedded crystallizer (2) in the external crystallizer (1), and the top of the external crystallizer (1) is set There is top end socket, bottom end is equipped with bottom head, and the top end socket is equipped with feed pipe (3), and the bottom head is equipped with and follows Ring liquid outlet tube (4);
The bottom of the embedded crystallizer (2) and the bottom head are affixed, and the top of the embedded crystallizer (2) is equipped with Cloth liquid disk (5), bottom end are equipped with catch tray (6);The upper end of the cloth liquid disk (5) is equipped with circulation fluid inlet tube (7), the circulation fluid It is connected between inlet tube (7) and the circulation fluid outlet tube (4) circulation pipe (8), is additionally provided with circulating pump on the circulation pipe (8) (9);The lower end of the catch tray (6) is equipped with discharge nozzle (10), and the discharge nozzle (10) is equipped with valve (11);
Multiple crystallizers (12) longitudinally are equipped in the embedded crystallizer (2), and the feed end of each crystallizer (12) Be connected to the fluid hole of the cloth liquid disk (5), the discharge end of each crystallizer (12) with the catch tray (6) into Fluid apertures connection;
It is provided with heat exchange jacket (13) outside the external crystallizer (1), the lower end of heat exchange jacket (13) side, which is equipped with, to be changed The upper end of thermal medium inlet tube (14), the opposite other side is equipped with heat transferring medium outlet (15).
2. the crystallization apparatus according to claim 1 for ethylene carbonate purification purification, which is characterized in that described external The bottom end of formula crystallizer (1) is additionally provided with 3-4 supporting leg (16).
3. the crystallization apparatus according to claim 1 for ethylene carbonate purification purification, which is characterized in that described external Temperature sensor is equipped in formula crystallizer (1).
4. the crystallization apparatus according to claim 1 for ethylene carbonate purification purification, which is characterized in that described is outer Setting formula crystallizer (1) and the embedded crystallizer (2) is cylindrical-shaped structure.
5. the crystallization apparatus according to claim 1 for ethylene carbonate purification purification, which is characterized in that the circulation Pumping (9) is one of metering pump, turbulence pump or centrifugal pump.
CN201820798660.2U 2018-05-25 2018-05-25 A kind of crystallization apparatus for ethylene carbonate purification purification Expired - Fee Related CN208617728U (en)

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Application Number Priority Date Filing Date Title
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Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201820798660.2U CN208617728U (en) 2018-05-25 2018-05-25 A kind of crystallization apparatus for ethylene carbonate purification purification

Publications (1)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108440489A (en) * 2018-05-25 2018-08-24 辽宁港隆化工有限公司 A kind of crystallization apparatus and purification process for the refined purification of ethylene carbonate

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108440489A (en) * 2018-05-25 2018-08-24 辽宁港隆化工有限公司 A kind of crystallization apparatus and purification process for the refined purification of ethylene carbonate

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Granted publication date: 20190319