CN101811694A - Method for preparing artificial graphite mesocarbon microbeads - Google Patents
Method for preparing artificial graphite mesocarbon microbeads Download PDFInfo
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- CN101811694A CN101811694A CN 201010183518 CN201010183518A CN101811694A CN 101811694 A CN101811694 A CN 101811694A CN 201010183518 CN201010183518 CN 201010183518 CN 201010183518 A CN201010183518 A CN 201010183518A CN 101811694 A CN101811694 A CN 101811694A
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Abstract
The invention relates to a method for preparing artificial graphite mesocarbon microbeads, in particular to a method for preparing a cathode material for a lithium-ion secondary battery, namely the artificial graphite mesocarbon microbeads. The technical scheme comprises steps of pretreatment of raw materials, catalysis treatment, thermal polycondensation, extraction treatment, separation and purification, and heat treatment, wherein in the extraction treatment process, the materials are directly added into an extracting agent at room temperature after the polymerization is finished, and the extracting agent accounts for 100 to 500 weight percent of the reaction materials; and in the separation and purification process, the spraying centrifugal purification is adopted, and a purifying agent accounts for 300 to 1,200 weight percent of the reaction materials. The method has the advantages that: the low temperature extracting agent is added, so the viscosity and temperature of the materials are reduced, the common centrifugal machine can be applied, and equipment cost is reduced; in the separation and purification process, extraction liquor is centrifuged first, a product is remained, the purifying agent is sprayed simultaneously, raw materials remained or the extracting agent on the surface is extracted further, and the product is purified; the method avoids the repeat purification and separation process of the materials, reduces loss, and saves time and energy; meanwhile, the extracting agent and the purifying agent are recovered to fulfill the aims of reducing cost and lightening environmental pollution.
Description
Affiliated technical field:
The present invention relates to a kind of preparation method of synthetic graphite MCMB, particularly the preparation method of anode material for lithium-ion secondary battery synthetic graphite MCMB.
Background technology:
MCMB is as the negative material of lithium-ion secondary cell, because of its particular structure characteristic, shows superior stability, charging and discharging property fast, is widely used, and especially has outstanding performance aspect power cell.At present, for the preparation method of MCMB, adopt the thermal polycondensation reaction usually, follow-up purification processes process adopts washing and separates two unit processes, realizes the separation of MCMB.This sepn process need repeat back and forth, adopts the alternately washing of different solvents simultaneously, has increased unit process like this, has increased solvent load, has prolonged the production time, the corresponding increase of energy consumption.And the organic extractant that adopts is the solvent inflammable, explosive, that toxicity is high, to producing and environment causes bigger harm.Simultaneously, repeatedly wash the loss that has not only increased material, also the MCMB surface is produced and corrode, especially strong solvent such as quinoline equal solvent can dissolve the part spheroid, form Surface Groove or cracking, charge and discharge the formation that influences surperficial SEI film in the process first at battery.
Summary of the invention:
The object of the invention provides a kind of preparation method of synthetic graphite MCMB, reduces the wastage, and saves time, and energy efficient reduces cost, and reduces environmental pollution, solves the problems referred to above that exist in the background technology.
Technical scheme of the present invention is: a kind of preparation method of synthetic graphite MCMB comprises following processing step: raw materials pretreatment, catalytic treatment, thermal polycondensation reaction, extraction treatment, separation purification, thermal treatment.
Said extraction treatment technology is: polyreaction directly adds material in the extraction agent after finishing, and the extraction agent temperature is a room temperature, and the extraction agent add-on is the 100-500wt% of reaction mass.
Said process for separating and purifying is: adopt the centrifugal purification of spray, purification dosage is the 300-1200wt% of reaction mass.
In the above-mentioned technology, extraction agent that uses and purificant are a kind of as washing oil or light oil, perhaps two kinds mixture, all recyclings of extraction agent and purificant.If extraction agent that uses and purificant are arbitrarily as the mixture of washing oil and light oil, volume each other, for example: the volume ratio of washing oil and light oil is 1:9-5:5.
Processing step more specifically: at first raw material heats, and perhaps directly purchases the liquid starting material temperature and keeps 160-300 ℃; The raw material of metering is added in the still,, prevent bumping by batch adding catalyzer; Under the heat-retaining condition, stir 1-3h, make mixing of materials even; To the reactor heating, make material generation cracking, polycondensation subsequently, generate the mesophase pitch microballoon; After reaction finishes, directly add in the extraction agent material and stirring, extraction agent is a room temperature, and main purpose is the unreacted raw material of extraction, the cooling of lowering the temperature simultaneously, and diluted material, extraction agent consumption are the 100-500wt% of raw material, preferable range is 200-300wt%.The material that extraction is finished, add in the generic centrifuge, direct centrifugation also adds purificant, spray centrifugal purification, the purificant consumption is the 300-1200wt% that adds pan feeding, and preferable range is 700-800wt%, and this process is mainly the unreacted raw material of further extraction, the while purified product, the heavy constituent raw material and the extraction agent of removal material remained on surface.Above-mentioned technology uses extraction agent and purificant to be mixtures a kind of in washing oil, the light oil or two kinds, and wants whole recyclings.Material after the purification is heat-treated, and heat treatment mode can be cryodrying, charing or greying.
Effect of the present invention: compare with conventional thermal polycondensation method production MCMB, difference of the present invention be extraction treatment with separate purification process.Extraction treatment of the present invention has solved a use high temperature centrifugal separation technique difficult problem, adopts the mode of low-temperature extraction agent adding, has reduced the viscosity and the temperature of material, makes generic centrifuge be used, and reduces equipment cost.Extraction agent is with most of unreacted raw material abstraction in the material, for next step purification provides condition simultaneously.It is earlier centrifugal with extraction liquid to separate purification process, stays product, sprays purificant simultaneously, and remaining raw material in surface or extraction agent are further extracted purified product.This process has been avoided material purification, separation, and the process of Ti Chuning has reduced loss repeatedly, has saved time, energy consumption.Simultaneously extraction agent and purificant are reclaimed, reach and reduce cost, reduce the purpose of environmental pollution.
Embodiment:
The invention will be further described by the following examples.
In an embodiment, after the material that uses the inventive method to produce carried out cryodrying, the fugitive constituent of test material characterized washing effect.The material refining effect can be with after the material greying, and the test material specific surface area characterizes.
The fugitive constituent testing method adopts thermal weight loss to measure:
1, the weighing weight of material is g
1, add and put into the intensification of retort furnace internal heating in the crucible.
2,950 ℃ of lasting 10min of insulation, cooling back weighing weight of material g
2
3, fugitive constituent %=
The test of BET nitrogen adsorption method is adopted in the specific surface area test, and equipment adopts the Kang Ta NOVE1000e of company type to test:
1, takes by weighing the 1g material and add in the test tube, put into degassing station, the degassing.
2, room temperature degassing 0.5h, 100 ℃ of degassing 2h, 300 ℃ of degassing 3h keep the degassing to be cooled to room temperature.
3, after the test tube weighing that the degassing is finished, put into nitrogen absorption station and measure.
4, by the equipment requirements test, provide test data.
It below is specific embodiment.
The used reactor of embodiment is the magnetic force driving reactor, and is withstand voltage less than 15MPa, volume 6m
3
Embodiment one:
250 ℃ pitch 3t are added in the reactor, in stirring, insulating process, add catalyzer 30Kg, divide 5 addings.Be warmed up to 420 ℃, keep the 8h polymerization.The polymer material of reaction terminating is directly added in the extraction agent light oil of room temperature, and light oil consumption 6t stirs 3h, puts into the whizzer centrifugation, adds the light oil spray simultaneously and purifies light oil consumption 9t.Purify after the above-mentioned solvent recuperation and utilize again.Material carries out cryodrying after the last centrifugation, the test fugitive constituent.To test material specific surface area after the material graphitization processing.
Embodiment two:
250 ℃ pitch 3t are added in the reactor, in stirring, insulating process, add catalyzer 30Kg, divide 5 addings.Be warmed up to 420 ℃, keep the 8h polymerization.The polymer material of reaction terminating is directly added in the extraction agent washing oil of room temperature, and washing oil consumption 9t stirs 3h, puts into the whizzer centrifugation, adds the washing oil spray simultaneously and purifies washing oil consumption 24t.Purify after the above-mentioned solvent recuperation and utilize again.Material carries out cryodrying after the last centrifugation, the test fugitive constituent.To test material specific surface area after the material graphitization processing.
Embodiment three:
250 ℃ pitch 3t are added in the reactor, in stirring, insulating process, add catalyzer 30Kg, divide 5 addings.Be warmed up to 420 ℃, keep the 8h polymerization.The polymer material of reaction terminating is directly added in the extraction agent washing oil of room temperature, and washing oil consumption 6t stirs 3h, puts into the whizzer centrifugation, adds the light oil spray simultaneously and purifies light oil consumption 30t.Purify after the above-mentioned solvent recuperation and utilize again.Material carries out cryodrying after the last centrifugation, the test fugitive constituent.To test material specific surface area after the material graphitization processing.
Embodiment four:
250 ℃ pitch 3t are added in the reactor, in stirring, insulating process, add catalyzer 30Kg, divide 5 addings.Be warmed up to 420 ℃, keep the 8h polymerization.The polymer material of reaction terminating is directly added in the extraction agent washing oil of room temperature, and washing oil consumption 6t stirs 3h, puts into the whizzer centrifugation, adds mixing oil (washing oil 30% light oil 70%) spray simultaneously and purifies mixing oil consumption 24t.Purify after the above-mentioned solvent recuperation and utilize again.Material carries out cryodrying after the last centrifugation, the test fugitive constituent.To test material specific surface area after the material graphitization processing.
In order to contrast the present invention and background technology, below the comparative example adopt background technology.
The comparative example:
250 ℃ pitch 3t are added in the reactor, in stirring, insulating process, add catalyzer 30Kg, divide 5 addings.Be warmed up to 420 ℃, keep the 8h polymerization.The polymer material of reaction terminating is added cooling in the purificant light oil (9t), mix; Carry out centrifugation then; Separate the material that finishes and add in the container interior adding purificant light oil (9t), purify; Carry out centrifugation after finishing; And then repeat said process twice.Material carries out cryodrying after the last centrifugation, the test fugitive constituent.To test material specific surface area after the material graphitization processing.
The various embodiments described above data are as follows:
By the data contrast of the present invention and background technology embodiment, can reach a conclusion:
The mode that the present invention adopts the low-temperature extraction agent to add uses generic centrifuge to separate, and spray is purified then, has avoided the background technology material to purify, separate the process of purifying repeatedly.Reducing loss, equipment cost, saving time, energy consumption, reducing under the prerequisite of environmental pollution, the product performance that product of producing and background technology are produced are suitable.
Claims (5)
1. the preparation method of a synthetic graphite MCMB is characterized in that comprising following processing step: raw materials pretreatment, catalytic treatment, thermal polycondensation reaction, extraction treatment, separation purification, thermal treatment.
2. according to the preparation method of the described synthetic graphite MCMB of claim 2, it is characterized in that said extraction treatment technology is: after polyreaction finishes, material is directly added in the extraction agent, and the extraction agent temperature is a room temperature, and the extraction agent add-on is the 100-500wt% of reaction mass.
3. according to the preparation method of the described synthetic graphite MCMB of claim 1, it is characterized in that said process for separating and purifying is: adopt the centrifugal purification of spray, purification dosage is the 300-1200wt% of reaction mass.
4. according to the preparation method of claim 2 or 3 described synthetic graphite MCMB, it is characterized in that a kind of as washing oil or light oil of the extraction agent that uses and purificant, perhaps two kinds mixture.
5. according to the preparation method of the described synthetic graphite MCMB of claim 4, it is characterized in that the extraction agent that uses and purificant mixture as washing oil or light oil, washing oil and light oil volume ratio are 1:9-5:5.
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| CN 201010183518 CN101811694A (en) | 2010-05-27 | 2010-05-27 | Method for preparing artificial graphite mesocarbon microbeads |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022494A (en) * | 2012-12-21 | 2013-04-03 | 济宁碳素集团有限公司 | Preparation method of synthetic graphite and application thereof |
| CN111807360A (en) * | 2020-07-28 | 2020-10-23 | 韶山润泽新能源科技有限公司 | Purification treatment system and process for natural graphite negative electrode powder |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272453A (en) * | 2000-05-26 | 2000-11-08 | 冶金工业部鞍山热能研究院 | Preparation method of mesophase carbon microsphere |
| JP2005050819A (en) * | 2004-08-04 | 2005-02-24 | Osaka Gas Co Ltd | Meso carbon micro beads |
| CN101081698A (en) * | 2006-09-15 | 2007-12-05 | 天津大学 | Preparation method of active meson-phase charcoal micro-balloon with high-ratio surface area and high mesoporosity |
-
2010
- 2010-05-27 CN CN 201010183518 patent/CN101811694A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1272453A (en) * | 2000-05-26 | 2000-11-08 | 冶金工业部鞍山热能研究院 | Preparation method of mesophase carbon microsphere |
| JP2005050819A (en) * | 2004-08-04 | 2005-02-24 | Osaka Gas Co Ltd | Meso carbon micro beads |
| CN101081698A (en) * | 2006-09-15 | 2007-12-05 | 天津大学 | Preparation method of active meson-phase charcoal micro-balloon with high-ratio surface area and high mesoporosity |
Non-Patent Citations (2)
| Title |
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| 《功能材料》 20090930 李凤娟等 炭化温度对中间相炭微球结构的影响 第1519-1521页 1-5 第40卷, 第9期 2 * |
| 《材料导报》 20080531 胡伟等 中间相炭微球热处理用作锂离子电池负极材料 第19-21页 1-5 第22卷, 第5期 2 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103022494A (en) * | 2012-12-21 | 2013-04-03 | 济宁碳素集团有限公司 | Preparation method of synthetic graphite and application thereof |
| CN103022494B (en) * | 2012-12-21 | 2013-11-06 | 济宁碳素集团有限公司 | Preparation method of synthetic graphite and application thereof |
| CN111807360A (en) * | 2020-07-28 | 2020-10-23 | 韶山润泽新能源科技有限公司 | Purification treatment system and process for natural graphite negative electrode powder |
| CN111807360B (en) * | 2020-07-28 | 2021-03-19 | 韶山润泽新能源科技有限公司 | Purification treatment system and process for natural graphite negative electrode powder |
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Application publication date: 20100825 |