CN108821969A - A kind of organic solvent purifying device and purification process - Google Patents
A kind of organic solvent purifying device and purification process Download PDFInfo
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- CN108821969A CN108821969A CN201810615515.0A CN201810615515A CN108821969A CN 108821969 A CN108821969 A CN 108821969A CN 201810615515 A CN201810615515 A CN 201810615515A CN 108821969 A CN108821969 A CN 108821969A
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- organic solvent
- gas
- collecting tank
- atomizing dryer
- raw material
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C68/00—Preparation of esters of carbonic or haloformic acids
- C07C68/08—Purification; Separation; Stabilisation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
- H01M10/0569—Liquid materials characterised by the solvents
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0025—Organic electrolyte
- H01M2300/0028—Organic electrolyte characterised by the solvent
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Secondary Cells (AREA)
Abstract
The invention belongs to solvent purification technical fields, more particularly to a kind of organic solvent purifying device and purification process, purification devices include raw material storage tank, atomizing dryer, gas-liquid separator, molecular sieve absorber, filter, gas circulator, first collecting tank and the second collecting tank, the atomizing dryer is connect with the raw material storage tank, the atomizing dryer, the gas-liquid separator, the molecular sieve absorber, the filter and the gas circulator are sequentially connected and form circulation loop, first collector is connect with the gas-liquid separator, second collecting tank is connect with the atomizing dryer bottom, second collecting tank is also connect with the raw material storage tank.Compared with the prior art, low energy consumption when the configuration of the present invention is simple, purifying, and is avoided that due to molecular sieve clast brings solvent into and reacts with components other in electrolyte, reduces the probability of impurity content exceeding index.
Description
Technical field
The invention belongs to solvent purification technical field more particularly to a kind of organic solvent purifying devices and purification process.
Background technique
Lithium ion battery is the green high-capacity environment-protecting battery to attract attention in recent years, is all used from battery of mobile phone to new energy
Source automobile largely uses.Electrolyte is the important component of lithium battery, its quality directly affects the optimization of battery performance
With raising.As the key core component of electrolyte, single organic solvent must be that purity is not high not less than 99.95%, moisture
It is not higher than 1ppm in 20ppm, impurity, then several solvents and high-purity lithium salts and additive, control working condition is obtained through mixed
Conjunction obtains required electrolyte.
As market competition is aggravated, profit reduces and industrialized requirement.Industry purifies single organic solvent, absolutely
It is most of to become molecular sieve or special dehydration purification material purification realization mass from original distillation procedure.But it distills
Method can only realize single special solvent purification, and the device is complicated, personnel demand is big, energy consumption and yield be not high, can accomplish
90% yield is not easy very much.It is most general that existing molecular sieve dehydration technique has become each domestic and international most manufacturers
Production method, although its production cost is low, its disadvantage is also apparent from.Molecular sieve is containing sodium, potassium, calcium, aluminium, silicon and oxygen
Compound, and contain a certain amount of combination water, or even have some special auxiliary agents, these substances, which do not enter in electrolyte, not to be influenced
Electrolyte quality, but molecular sieve surface micro mist is by constantly friction in dehydration purification process, particle is micro- less than 0.2um's
Dirt, filter are difficult thoroughly to filter out, be directly entered in lithium-ion battery electrolytes, and electrolyte contains micro hydrofluoric acid
Mixture can be reacted with above-mentioned metal oxide with hydrofluoric acid, formed metal ion, caused impurity ion content exceeded, from
And finally influence battery performance.
Summary of the invention
It is an object of the present invention to：In view of the deficiencies of the prior art, a kind of organic solvent purifying device is provided, is tied
Structure is simple, operation when low energy consumption, and be avoided that due to molecular sieve clast brings solvent into and react with components other in electrolyte,
Reduce the probability of impurity content exceeding index.
The second object of the present invention is：In view of the deficiencies of the prior art, a kind of organic solvent purifying method, energy consumption are provided
Low, refining effect is good.
To achieve the goals above, the present invention uses following technical scheme：
A kind of organic solvent purifying device, including raw material storage tank, atomizing dryer, gas-liquid separator, molecular sieve absorber,
Filter, gas circulator, the first collecting tank and the second collecting tank, the atomizing dryer are connect with the raw material storage tank, institute
Atomizing dryer, the gas-liquid separator, the molecular sieve absorber, the filter and the gas circulator is stated successively to connect
Circulation loop is connect and is formed, first collector is connect with the gas-liquid separator, second collecting tank and the atomization
The connection of drier bottom, second collecting tank are also connect with the raw material storage tank.
It further include heater as a kind of improvement of organic solvent purifying device of the present invention, the heater is set
In the atomizing dryer.
As a kind of improvement of organic solvent purifying device of the present invention, the recyclegas of the gas circulator is
Inert gas.
A kind of organic solvent purifying method, includes the following steps：
Step 1 organic solvent to be purified is added in raw material storage tank, is opened atomizing dryer, heater, gas and is followed
Ring pump and molecular sieve absorber, and heater is adjusted to assigned temperature；
Step 2, the organic solvent being atomized under atomizing dryer and heater effect are followed with what gas circulator generated
Ring gas is in contact, and concentrates at atomizing dryer bottom, is flowed in the second collecting tank via pipeline；
Step 3 is partially collected into the first collecting tank by gas-liquid separator separates by the organic solvent that gas entrainment is walked
Interior, recyclegas is filtered by molecular sieve absorber and filter, using supplying in gas circulator to atomizing dryer
It is recycled；
Step 4, the organic solvent that setting purity and moisture content are met in the second collecting tank give over to preparing lithium ion battery
Electrolyte uses, and the organic solvent for not meeting setting purity and moisture content then passes through pipeline back in raw material storage tank, then into
Row atomization drying operation, until meeting the requirements.
As a kind of improvement of organic solvent purifying method of the present invention, in step 2, organic solvent is being atomized
Nebulisation time in drier is 5~20s, and the heating temperature of heater is lower than the boiling point of organic solvent.
As a kind of improvement of organic solvent purifying method of the present invention, in step 4, purity is set as 99.95
~99.99%.
As a kind of improvement of organic solvent purifying method of the present invention, in step 4, set moisture content as
Less than 10ppm.
Compared with the prior art, the present invention at least has the advantages that：
1) present invention is by mechanism, by the material dispersion of purifying to be dried at the very thin particle as mist and heat
Air or the contact of other gases, increase moisture disengagement area, remove most of moisture in moment, accelerate the drying of material pure
Change.
2) atomization that the present invention uses does not need that solvent is directly heated to boiling point, and the processing time is 5~20 seconds,
Vacuumizing is not needed, energy consumption brought by distillation procedure is reduced while simplifying purifying process yet.
3) atomization that the present invention uses only is contacted with high purity inert gas, is avoided due to molecular sieve clast brings solvent into
It brings into electrolyte and is reacted with electrolyte, reduce the probability of impurity content exceeding index.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of organic solvent purifying device in the present invention.
Wherein：1- raw material storage tank, 2- atomizing dryer, 3- heater, 4- gas-liquid separator, 5- molecular sieve absorber, 6-
Filter, 7- gas circulator, the first collecting tank of 8-, the second collecting tank of 9-.
Specific embodiment
With reference to embodiment and Figure of description, the present invention is described in further detail, but the present invention
Embodiment be not limited to this.
Comparative example 1
This comparative example produces ethylene carbonate using vacuum distillation method, and concrete operation step is as follows：
Starting：1000kg ethylene carbonate is produced, 60 DEG C of bakings melt, squeeze into vacuum (distilling) column, open vacuum system, directly
To tower reactor, the vacuum degree of tower top to -0.1MPa；Material heating rate is controlled at 1 DEG C/min, heating agent oil temperature is set in 140 DEG C
Left and right.
Infinite reflux：When tower top flows back, adjusts cooling water inflow and control outlet coolant water temperature between 36~40 DEG C；
The infinite reflux time is 2 hours, stablizes the temperature gradient of full tower；The moisture content of sampling analysis refluxing opening, purity, to before the extraction of fore-running tank
Fraction.
Front-end volatiles extraction：The moisture content of sampling analysis fraction, purity, work as moisture content after foreshot extraction half an hour<It is 10ppm, pure
Degree >=99.93% can be adopted when total alcohol content is lower than 300ppm into pans.
Main distillate fraction extraction：It evaporates after tank is adopted completely or reboiler liquid level is when reaching lower limit, stop extraction.
Parking：Stop the extraction of product；Stop oil heating；When lower than 120 DEG C, heating agent oil circulating pump can be stopped；Stop
Vacuum system gives pans filling with inert gas, pressure>0.1Mpa, notification analysis personnel's sampling analysis；After reflux, stop cold
But water system.
Comparative example 2
This comparative example produces divinyl carbonate using rectifying non-pressure process, and specific operating parameter is as follows：
1) inlet amount control is at 50-80 ls/h；
2) material heating rate is at 1.5 DEG C/min；
3) control feed rate is at 50-80 ls/h；
4) bottom temperature rises to 110--120 DEG C；
5) light fraction produces 1.5-3 ls/h.
Comparative example 3
This comparative example produces methyl ethyl carbonate enester using rectifying non-pressure process, and specific operating parameter is identical as comparative example 2.
Comparative example 4
This comparative example produces ethylene carbonate using molecular sieve dehydration method of purification, and concrete operations are as follows：
1000kg ethylene carbonate is produced, 60 DEG C of bakings are melted, and liquid circulation pump, ethylene carbonate are opened in drain sump heat preservation
Ester is contacted through over-molecular sieve and is dehydrated, until moisture is less than 10ppm.
Comparative example 5
This comparative example produces diethyl carbonate using molecular sieve dehydration method of purification, and concrete operations are as follows：
1000kg diethyl carbonate is produced, liquid circulation pump is opened, ethylene carbonate is contacted through over-molecular sieve and is dehydrated, until
Moisture is less than 10ppm.
Comparative example 6
This comparative example produces methyl ethyl carbonate using molecular sieve dehydration method of purification, and concrete operations are as follows：
1000kg diethyl carbonate is produced, liquid circulation pump is opened, ethylene carbonate is contacted through over-molecular sieve and is dehydrated, until
Moisture is less than 10ppm.
Embodiment 1
As shown in Figure 1, a kind of organic solvent purifying device includes raw material storage tank 1, atomizing dryer 2, heater 3, gas-liquid
Separator 4, molecular sieve absorber 5, filter 6, gas circulator 7, the first collecting tank 8 and the second collecting tank 9, atomizing dryer
2 connect with raw material storage tank 1, and heater 3 is set to atomizing dryer 2, atomizing dryer 2, gas-liquid separator 4, molecular sieve absorber
5, filter 6 and gas circulator 7 are sequentially connected and are formed circulation loop, and the first collector 8 is connect with gas-liquid separator 4, the
Two collecting tanks 9 are connect with 2 bottom of atomizing dryer, and the second collecting tank 9 is also connect with raw material storage tank 1.The circulation of gas circulator 7
Gas is inert gas.
The present embodiment purifies ethylene carbonate using the above organic solvent purifying device, and specific step is as follows：
1) 1000kg ethylene carbonate to be purified, melt in 60 DEG C of bakings, be added in raw material storage tank 1, and 60 DEG C of guarantors
Temperature opens atomizing dryer 2, heater 3, gas circulator 7 and molecular sieve absorber 5, and adjusts heater 3 to specified temperature
Degree；
2) ethylene carbonate being atomized in the case where atomizing dryer 2 and heater 3 act on is followed with what gas circulator 7 generated
Ring gas is in contact, and concentrates at 2 bottom of atomizing dryer, is flowed in the second collecting tank 9 via pipeline；
3) it is partially separated and collected by gas-liquid separator 4 into the first collecting tank 8, is followed by the organic solvent that gas entrainment is walked
Ring gas is filtered by molecular sieve absorber 5 and filter 6, using supplying to follow in gas circulator 7 to atomizing dryer 2
Ring uses；
4) organic solvent for meeting setting purity and moisture content in the second collecting tank 9 gives over to preparation lithium ion battery electrolysis
Liquid uses, and the organic solvent for not meeting setting purity and moisture content then passes through pipeline back in raw material storage tank 1, then carries out mist
Change drying process, until meeting the requirements.
Embodiment 2
Unlike the first embodiment：The present embodiment uses organic solvent purifying device purifying diethyl carbonate, operating process
In do not need to heat, temperature is room temperature.
Remaining is with embodiment 1, and which is not described herein again.
Embodiment 3
Unlike the first embodiment：The present embodiment purifies methyl ethyl carbonate, operating process using organic solvent purifying device
In do not need to heat, temperature is room temperature.
Remaining is with embodiment 1, and which is not described herein again.
The organic solvent of comparative example 1~6 and Examples 1 to 3 after purification is detected respectively, testing result such as 1 institute of table
Show.
1 organic solvent testing result of table
With comparative example 1~3 for A group, comparative example 4~6 is B group, and Examples 1 to 3 is C group, three kinds of organic solvents in every group
Mass ratio be 1:1:1,124kg lithium hexafluoro phosphate is added and makes one ton of electrolyte, then tests electrolyte index.And it is each
It takes 1kg electrolyte to be placed in 60 DEG C of baking ovens to toast, sees the time used when coloration changes to 30hazen, test result is shown in Table 2.
2 electrolyte test result of table
| Content | Moisture/ppm | Acidity/ppm | Start color | Coloring Time/H | Sodium ion/ppm | Calcium ion/ppm |
| The electrolyte of A group solvent configuration | 5 | 15 | It is colorless and transparent | 12 | / | / |
| The electrolyte that B group solvent is prepared | 5 | 16 | It is colorless and transparent | 3 | 5 | 4 |
| The electrolyte that C group solvent is prepared | 5 | 15 | It is colorless and transparent | 12 | / | / |
It can be seen that by the above testing result：It is all good with the organic solvent indices that distillating method produces, but need
The a large amount of energy consumptions of high temperature are wanted, while yield is relatively high.It also can satisfy requirement with the solvent index that molecular sieve contact method purifies,
But comparison methyl ethyl carbonate purification process, the purity of methyl ethyl carbonate do not rise anti-drop, analysis the reason is that methyl ethyl carbonate with
Cause to decompose generation because itself is unstable in molecular sieve contact process.Using organic scavenging device (atomization purification of the invention
Method) solvent that is obtained close to the way of distillation of obtained solvent its indices of purifying, although the time is than molecular sieve contact method
Between it is slightly long, but it can satisfy production needs.
In addition, the electrolyte that several methods of purification are prepared is compared, the electrolyte index that wherein way of distillation and atomization obtain
It is close, by 60 DEG C of baking ovens accelerate metamorphic processes see also close to.It is the electrolyte that molecular sieve contact method obtains, sodium instead
Content is 5ppm, calcium content 4ppm, and toasting 3 hours there have been coloration is more than 30hazen situation, which increase electrolyte plus
The use hidden danger of battery after entering to battery.
In conclusion being a kind of preferred side using organic scavenging device of the invention and purification process (atomization method of purification)
It is high to purify obtained organic solvent quality for method, and low energy consumption in purification process, and speed of production is moderate.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to above-mentioned specific embodiment, all those skilled in the art exist
Made any conspicuous improvement, replacement or modification all belong to the scope of protection of the present invention on the basis of the present invention.This
Outside, although using some specific terms in this specification, these terms are merely for convenience of description, not to the present invention
Constitute any restrictions.
Claims (7)
1. a kind of organic solvent purifying device, it is characterised in that：Including raw material storage tank, atomizing dryer, gas-liquid separator, molecule
Absorber, filter, gas circulator, the first collecting tank and the second collecting tank are sieved, the atomizing dryer and the raw material store up
Tank connection, the atomizing dryer, the gas-liquid separator, the molecular sieve absorber, the filter and the gas follow
Ring pump is sequentially connected and is formed circulation loop, and first collector is connect with the gas-liquid separator, second collecting tank
It is connect with the atomizing dryer bottom, second collecting tank is also connect with the raw material storage tank.
2. organic solvent purifying device according to claim 1, it is characterised in that：It further include heater, the heater
Set on the atomizing dryer.
3. organic solvent purifying device according to claim 1, it is characterised in that：The recyclegas of the gas circulator
For inert gas.
4. a kind of organic solvent purifying method, which is characterized in that include the following steps：
Step 1 organic solvent to be purified is added in raw material storage tank, opens atomizing dryer, heater, gas circulator
With molecular sieve absorber, and heater is adjusted to assigned temperature；
Step 2, the circulating air that the organic solvent and gas circulator being atomized under atomizing dryer and heater effect generate
Body is in contact, and concentrates at atomizing dryer bottom, is flowed in the second collecting tank via pipeline；
Step 3 is partially collected into the first collecting tank by gas-liquid separator separates by the organic solvent that gas entrainment is walked, is followed
Ring gas is filtered by molecular sieve absorber and filter, is made using in gas circulator to atomizing dryer for circulation
With；
Step 4, the organic solvent that setting purity and moisture content are met in the second collecting tank, which gives over to, prepares lithium ion battery electrolysis
Liquid uses, and the organic solvent for not meeting setting purity and moisture content then passes through pipeline back in raw material storage tank, then carries out mist
Change drying process, until meeting the requirements.
5. organic solvent purifying method according to claim 4, it is characterised in that：In step 2, organic solvent is in mist
Changing the nebulisation time in drier is 5~20s, and the heating temperature of heater is lower than the boiling point of organic solvent.
6. organic solvent purifying method according to claim 4, it is characterised in that：In step 4, set purity as
99.95~99.99%.
7. organic solvent purifying method according to claim 4, it is characterised in that：In step 4, moisture content is set
For less than 10ppm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810615515.0A CN108821969A (en) | 2018-06-14 | 2018-06-14 | A kind of organic solvent purifying device and purification process |
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| CN201810615515.0A CN108821969A (en) | 2018-06-14 | 2018-06-14 | A kind of organic solvent purifying device and purification process |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101685880A (en) * | 2008-09-25 | 2010-03-31 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of electrolyte of low-temperature lithium ion battery |
| CN102079741A (en) * | 2010-12-21 | 2011-06-01 | 东莞市杉杉电池材料有限公司 | Novel dewatering and purifying method of ethylene carbonate (EC) |
-
2018
- 2018-06-14 CN CN201810615515.0A patent/CN108821969A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101685880A (en) * | 2008-09-25 | 2010-03-31 | 张家港市国泰华荣化工新材料有限公司 | Preparation method of electrolyte of low-temperature lithium ion battery |
| CN102079741A (en) * | 2010-12-21 | 2011-06-01 | 东莞市杉杉电池材料有限公司 | Novel dewatering and purifying method of ethylene carbonate (EC) |
Non-Patent Citations (1)
| Title |
|---|
| 杨宗发主编: "《药物制剂设备》", 31 August 2014 * |
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Application publication date: 20181116 |