CN111252761A - Purification method of graphite negative electrode material - Google Patents
Purification method of graphite negative electrode material Download PDFInfo
- Publication number
- CN111252761A CN111252761A CN202010266588.0A CN202010266588A CN111252761A CN 111252761 A CN111252761 A CN 111252761A CN 202010266588 A CN202010266588 A CN 202010266588A CN 111252761 A CN111252761 A CN 111252761A
- Authority
- CN
- China
- Prior art keywords
- powder
- crushed
- mixture
- ball mill
- purifying
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 238000000034 method Methods 0.000 title claims abstract description 33
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 31
- 239000010439 graphite Substances 0.000 title claims abstract description 31
- 238000000746 purification Methods 0.000 title claims abstract description 16
- 239000007773 negative electrode material Substances 0.000 title description 3
- 239000000843 powder Substances 0.000 claims abstract description 73
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000000463 material Substances 0.000 claims abstract description 28
- 239000002253 acid Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 21
- 238000002386 leaching Methods 0.000 claims abstract description 21
- 239000012535 impurity Substances 0.000 claims abstract description 19
- 238000007885 magnetic separation Methods 0.000 claims abstract description 17
- 230000007935 neutral effect Effects 0.000 claims abstract description 14
- 239000010406 cathode material Substances 0.000 claims abstract description 11
- 239000003513 alkali Substances 0.000 claims abstract description 9
- 230000004927 fusion Effects 0.000 claims abstract description 9
- 239000011362 coarse particle Substances 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 239000000203 mixture Substances 0.000 claims description 38
- 238000001354 calcination Methods 0.000 claims description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 238000005406 washing Methods 0.000 claims description 22
- 239000010405 anode material Substances 0.000 claims description 14
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000006148 magnetic separator Substances 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 230000005484 gravity Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000011812 mixed powder Substances 0.000 claims description 6
- 239000010419 fine particle Substances 0.000 claims description 2
- 229910044991 metal oxide Inorganic materials 0.000 abstract description 5
- 150000004706 metal oxides Chemical class 0.000 abstract description 5
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 abstract description 4
- 229910000323 aluminium silicate Inorganic materials 0.000 abstract description 4
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 abstract description 4
- 239000010453 quartz Substances 0.000 abstract description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 4
- 229910052799 carbon Inorganic materials 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 239000013014 purified material Substances 0.000 abstract description 3
- 238000004140 cleaning Methods 0.000 abstract 1
- 238000000227 grinding Methods 0.000 abstract 1
- 238000002156 mixing Methods 0.000 description 5
- 238000001556 precipitation Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910000503 Na-aluminosilicate Inorganic materials 0.000 description 3
- 239000004115 Sodium Silicate Substances 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 150000002736 metal compounds Chemical class 0.000 description 3
- 238000012216 screening Methods 0.000 description 3
- 239000000429 sodium aluminium silicate Substances 0.000 description 3
- 235000012217 sodium aluminium silicate Nutrition 0.000 description 3
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 3
- 229910052911 sodium silicate Inorganic materials 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000000498 ball milling Methods 0.000 description 2
- 239000003575 carbonaceous material Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
Landscapes
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a purification method of a graphite cathode material, which comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, alkali fusion; step six, acid leaching; crushing a graphite cathode material to be treated by a jaw crusher, feeding the crushed material into an ultrafine ball mill by a double-screw feeder after the crushed material is crushed to reasonable fineness, and crushing and grinding the material by the ultrafine ball mill; feeding the raw materials ground by the ball mill into an airflow classifier for classification; cleaning and grading the powder subjected to airflow grading by using a spiral grading machine, and drying the cleaned and graded powder by using a drying box; the invention has good purification effect and less coarse particle residue, can fully purify components such as silicate, aluminosilicate, quartz and the like in impurities and metal oxides, has high carbon purity, and ensures that the pH value of the purified material is neutral, thereby being convenient for subsequent processing.
Description
Technical Field
The invention relates to the technical field of graphite cathode material processing, in particular to a purification method of a graphite cathode material.
Background
The negative pole of the lithium ion battery is prepared by uniformly coating paste adhesive prepared by mixing a negative pole active material carbon material or non-carbon material, a binding agent and an additive on two sides of a copper foil, drying and rolling, wherein the raw material needs to be purified in the production and processing process of the graphite negative pole material, impurity components in the raw material are removed, in the purification of the graphite negative pole material in the prior art, the purification effect of the material is poor, a large amount of coarse particles remain, the components such as silicate, aluminosilicate, quartz and the like in the impurities and metal oxides cannot be fully purified, the carbon purity is not high, and the pH value of the purified material is acidic or alkaline, so that the subsequent processing is influenced, therefore, the purification method for the graphite negative pole material is necessary.
Disclosure of Invention
The present invention aims to provide a method for purifying a graphite negative electrode material to solve the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, alkali fusion; step six, acid leaching;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill;
in the second step, the raw materials ground by the ball mill are sent into an airflow classifier for classification, qualified fine particles enter a collecting device, and coarse particle powder falls down along the inner wall of the middle machine body and moves downwards;
in the third step, the powder after air flow classification is cleaned and classified by a spiral classifier through different settling speeds of solid particles in liquid by means of different specific gravities of the solid particles, and then the cleaned and classified powder is dried by a drying box;
in the fourth step, the dried powder is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
in the fifth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is stirred uniformly, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, and the mixture in the calcining furnace is washed by water and filtered until the washing is neutral;
and in the sixth step, a certain amount of hydrochloric acid solution is added into the washed mixture, the mixture is mixed and stirred for a period of time, the powder is taken out, water is added again for washing and filtering until the washing is neutral, and the treated powder is dried.
According to the technical scheme, in the first step, the raw materials are crushed and ground to 20-30 μm.
According to the technical scheme, in the second step, in the descending process of the coarse grains, secondary air is introduced for further elutriation, so that the mixed powder with the standard rises along with the secondary air again, the classification is carried out again, and the elutriated coarse grains are discharged from the material returning port along the same proportion.
According to the technical scheme, in the third step, the temperature of the drying box is 80-100 ℃.
According to the technical scheme, in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃.
According to the technical scheme, in the fifth step, the weight ratio of the powder material to the sodium hydroxide is 1: 0.4.
According to the technical scheme, in the sixth step, the acid leaching time is 150-min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
According to the technical scheme, in the sixth step, the weight ratio of the powder material to the hydrochloric acid is 1: 0.4.
Compared with the prior art, the invention has the beneficial effects that: the material is subjected to ball milling and superfine crushing by matching a jaw crusher and an superfine ball mill, the finely crushed powder is subjected to primary classification treatment by an airflow classifier, then the powder is subjected to spiral classification by a spiral classifier, magnetic separation is performed by a magnetic separator after drying and screening, magnetic impurities such as steel and iron in the powder are adsorbed, alkali fusion is performed on the powder, components such as silicate, aluminosilicate and quartz react with sodium hydroxide to generate soluble sodium silicate or acid soluble sodium aluminosilicate, then the soluble sodium silicate or acid soluble sodium aluminosilicate is removed by washing, metal oxides in the powder are converted into soluble metal compounds by acid leaching, and the soluble metal compounds are separated from the powder after filtering and washing.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a flow chart of the method of the present invention.
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, the present invention provides a technical solution:
example 1:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, alkali fusion; step six, acid leaching;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill, wherein in the first step, the raw material is crushed and ground to 20-30 mu m;
in the second step, secondary air is introduced in the descending process of coarse grains for further elutriation, so that the mixed powder with the specification rises along with the secondary air again, the coarse grains are classified again, and the elutriated coarse grains are discharged from a material return port along the same ratio;
in the third step, the powder after air flow classification is cleaned and classified by a spiral classifier through different precipitation speeds in liquid by means of different specific gravities of solid particles, and then the cleaned and classified powder is dried by a drying box, wherein the temperature of the drying box is 80-100 ℃;
in the fourth step, the dried powder is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
in the fifth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is uniformly stirred, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, the mixture in the calcining furnace is washed by water and filtered until the washing is neutral, and in the fifth step, the weight ratio of the powder to the sodium hydroxide is 1: 0.4; in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃;
adding a certain amount of hydrochloric acid solution into the washed mixture in the sixth step, mixing and stirring for a period of time, taking out the powder, adding water again, washing and filtering until the washing is neutral, and drying the treated powder, wherein in the sixth step, the weight ratio of the powder to the hydrochloric acid is 1: 0.4; in the sixth step, the acid leaching time is 120-150min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
Example 2:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, spiral grading; step three, magnetic separation; step four, alkali fusion; step five, acid leaching;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill, wherein in the first step, the raw material is crushed and ground to 20-30 mu m;
in the second step, the pulverized and ground powder is cleaned and classified by a spiral classifier through different precipitation speeds in liquid by means of different specific gravities of solid particles, and then the cleaned and classified powder is dried by a drying box, wherein in the third step, the temperature of the drying box is 80-100 ℃;
in the third step, screening the dried powder through a vibrating screen to remove larger impurities, and then adsorbing magnetic impurities such as steel and the like in the powder by using a magnetic field generated by a magnetic separator;
in the fourth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is stirred uniformly, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, the mixture in the calcining furnace is washed by water and filtered until the washing is neutral, and in the fifth step, the weight ratio of the powder to the sodium hydroxide is 1: 0.4; in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃;
adding a certain amount of hydrochloric acid solution into the washed mixture in the fifth step, mixing and stirring for a period of time, taking out the powder, adding water again, washing and filtering until the washing is neutral, and drying the treated powder, wherein in the sixth step, the weight ratio of the powder to the hydrochloric acid is 1: 0.4; in the sixth step, the acid leaching time is 120-150min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
Example 3:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, magnetic separation; step four, alkali fusion; step five, acid leaching;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill, wherein in the first step, the raw material is crushed and ground to 20-30 mu m;
in the second step, secondary air is introduced in the descending process of coarse grains for further elutriation, so that the mixed powder with the specification rises along with the secondary air again, the coarse grains are classified again, and the elutriated coarse grains are discharged from a material return port along the same ratio;
in the third step, the powder subjected to air flow classification is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
in the fourth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is stirred uniformly, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, the mixture in the calcining furnace is washed by water and filtered until the washing is neutral, and in the fifth step, the weight ratio of the powder to the sodium hydroxide is 1: 0.4; in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃;
adding a certain amount of hydrochloric acid solution into the washed mixture in the fifth step, mixing and stirring for a period of time, taking out the powder, adding water again, washing and filtering until the washing is neutral, and drying the treated powder, wherein in the sixth step, the weight ratio of the powder to the hydrochloric acid is 1: 0.4; in the sixth step, the acid leaching time is 120-150min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
Example 4:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, acid leaching;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill, wherein in the first step, the raw material is crushed and ground to 20-30 mu m;
in the second step, secondary air is introduced in the descending process of coarse grains for further elutriation, so that the mixed powder with the specification rises along with the secondary air again, the coarse grains are classified again, and the elutriated coarse grains are discharged from a material return port along the same ratio;
in the third step, the powder after air flow classification is cleaned and classified by a spiral classifier through different precipitation speeds in liquid by means of different specific gravities of solid particles, and then the cleaned and classified powder is dried by a drying box, wherein the temperature of the drying box is 80-100 ℃;
in the fourth step, the dried powder is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
adding a certain amount of hydrochloric acid solution into the powder mixture subjected to magnetic separation in the fifth step, mixing and stirring for a period of time, taking out the powder, adding water, washing, filtering until the washing is neutral, and drying the treated powder, wherein in the sixth step, the weight ratio of the powder to the hydrochloric acid is 1: 0.4; in the sixth step, the acid leaching time is 120-150min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
Example 5:
a purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, alkali fusion;
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill, wherein in the first step, the raw material is crushed and ground to 20-30 mu m;
in the second step, secondary air is introduced in the descending process of coarse grains for further elutriation, so that the mixed powder with the specification rises along with the secondary air again, the coarse grains are classified again, and the elutriated coarse grains are discharged from a material return port along the same ratio;
in the third step, the powder after air flow classification is cleaned and classified by a spiral classifier through different precipitation speeds in liquid by means of different specific gravities of solid particles, and then the cleaned and classified powder is dried by a drying box, wherein the temperature of the drying box is 80-100 ℃;
in the fourth step, the dried powder is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
in the fifth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is uniformly stirred, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, the mixture in the calcining furnace is washed by water and filtered until the washing is neutral, and in the fifth step, the weight ratio of the powder to the sodium hydroxide is 1: 0.4; in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃.
The properties of the examples are compared in the following table:
based on the above, the invention has the advantages that the jaw crusher is matched with the superfine ball mill, performing ball milling and superfine crushing on the material, performing primary grading treatment on the finely crushed powder through an airflow grader, then the powder is processed into spiral grading by a spiral grading machine, magnetic separation is carried out by a magnetic separator after drying and screening, magnetic impurities such as steel and the like in the powder are adsorbed, the powder is subjected to alkali fusion to enable components such as silicate, aluminosilicate, quartz and the like to react with sodium hydroxide to generate soluble sodium silicate or acid-soluble sodium aluminosilicate, then washing with water to remove the metal oxide, converting the metal oxide in the powder into soluble metal compound by acid leaching, filtering and washing, separating from the powder, the purification effect on the material is good, the residual coarse particles are few, the carbon purity is high, and the pH value of the purified material is neutral, so that the subsequent processing is influenced.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A purification method of a graphite anode material comprises the following steps: firstly, finely crushing materials; step two, airflow classification; step three, spiral grading; step four, magnetic separation; step five, alkali fusion; step six, acid leaching; the method is characterized in that:
in the first step, the graphite cathode material raw material to be processed is crushed by a jaw crusher, the crushed raw material is sent into an ultrafine ball mill by a double-screw feeder after being crushed to reasonable fineness, and the raw material is crushed and ground by the ultrafine ball mill;
in the second step, the raw materials ground by the ball mill are sent into an airflow classifier for classification, qualified fine particles enter a collecting device, and coarse particle powder falls down along the inner wall of the middle machine body and moves downwards;
in the third step, the powder after air flow classification is cleaned and classified by a spiral classifier through different settling speeds of solid particles in liquid by means of different specific gravities of the solid particles, and then the cleaned and classified powder is dried by a drying box;
in the fourth step, the dried powder is screened by a vibrating screen to remove larger impurities, and then magnetic impurities such as steel and the like in the powder are adsorbed by a magnetic field generated by a magnetic separator;
in the fifth step, the powder subjected to magnetic separation and sodium hydroxide are mixed according to a certain proportion, water is added to the mixture and the mixture is stirred uniformly, the mixture is placed in a calcining furnace for calcining treatment, the mixture is cooled to room temperature after the calcining treatment is finished, and the mixture in the calcining furnace is washed by water and filtered until the washing is neutral;
and in the sixth step, a certain amount of hydrochloric acid solution is added into the washed mixture, the mixture is mixed and stirred for a period of time, the powder is taken out, water is added again for washing and filtering until the washing is neutral, and the treated powder is dried.
2. The method for purifying a graphite anode material according to claim 1, wherein: in the first step, the raw materials are crushed and ground to 20-30 μm.
3. The method for purifying a graphite anode material according to claim 1, wherein: in the second step, in the descending process of the coarse grains, secondary air is introduced for further elutriation, so that the mixed powder with the standard rises along with the secondary air again, classification is carried out again, and the elutriated coarse grains are discharged from the material returning port along the same proportion.
4. The method for purifying a graphite anode material according to claim 1, wherein: in the third step, the temperature of the drying oven is 80-100 ℃.
5. The method for purifying a graphite anode material according to claim 1, wherein: in the fifth step, the calcination time is 90-120min, and the calcination temperature is 600-700 ℃.
6. The method for purifying a graphite anode material according to claim 1, wherein: in the fifth step, the weight ratio of the powder material to the sodium hydroxide is 1: 0.4.
7. The method for purifying a graphite anode material according to claim 1, wherein: in the sixth step, the acid leaching time is 120-150min, and the acid leaching temperature is 80 ℃ in a constant-temperature water bath.
8. The method for purifying a graphite anode material according to claim 1, wherein: in the sixth step, the weight ratio of the powder material to the hydrochloric acid is 1: 0.4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010266588.0A CN111252761A (en) | 2020-04-07 | 2020-04-07 | Purification method of graphite negative electrode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010266588.0A CN111252761A (en) | 2020-04-07 | 2020-04-07 | Purification method of graphite negative electrode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN111252761A true CN111252761A (en) | 2020-06-09 |
Family
ID=70942391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010266588.0A Pending CN111252761A (en) | 2020-04-07 | 2020-04-07 | Purification method of graphite negative electrode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN111252761A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112320794A (en) * | 2020-10-29 | 2021-02-05 | 中国科学院过程工程研究所 | Deep impurity removal method for waste battery cathode recycling decommissioned graphite |
| CN115924907A (en) * | 2022-12-21 | 2023-04-07 | 江苏金亚隆科技有限公司 | Physical purification process of graphite raw material |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090136849A1 (en) * | 2005-05-27 | 2009-05-28 | Btr New Energy Materials Inc. | Composite carbon material of negative electrode in lithuim ion battery and its preparation method |
| CN105197920A (en) * | 2015-10-20 | 2015-12-30 | 辽宁工程技术大学 | Microcrystal graphite separation and purification method |
| CN107522197A (en) * | 2017-09-15 | 2017-12-29 | 福建翔丰华新能源材料有限公司 | The method of the preparation high-purity of economy, the micro crystal graphite of high graphitization degree |
| CN107601494A (en) * | 2017-09-05 | 2018-01-19 | 河南易成新能源股份有限公司 | A kind of graphite cathode material purification process |
| CN207418306U (en) * | 2017-10-31 | 2018-05-29 | 湖南国盛石墨科技有限公司 | A kind of spheroidization micro crystal graphite production system |
| CN110600737A (en) * | 2019-09-30 | 2019-12-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite negative electrode material |
-
2020
- 2020-04-07 CN CN202010266588.0A patent/CN111252761A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090136849A1 (en) * | 2005-05-27 | 2009-05-28 | Btr New Energy Materials Inc. | Composite carbon material of negative electrode in lithuim ion battery and its preparation method |
| CN105197920A (en) * | 2015-10-20 | 2015-12-30 | 辽宁工程技术大学 | Microcrystal graphite separation and purification method |
| CN107601494A (en) * | 2017-09-05 | 2018-01-19 | 河南易成新能源股份有限公司 | A kind of graphite cathode material purification process |
| CN107522197A (en) * | 2017-09-15 | 2017-12-29 | 福建翔丰华新能源材料有限公司 | The method of the preparation high-purity of economy, the micro crystal graphite of high graphitization degree |
| CN207418306U (en) * | 2017-10-31 | 2018-05-29 | 湖南国盛石墨科技有限公司 | A kind of spheroidization micro crystal graphite production system |
| CN110600737A (en) * | 2019-09-30 | 2019-12-20 | 广东凯金新能源科技股份有限公司 | Preparation method of graphite negative electrode material |
Non-Patent Citations (2)
| Title |
|---|
| 谭旭升等: "碱酸法纯化石墨试验研究", 《中国矿业》 * |
| 郑水林: "非金属矿粉体加工技术现状与发展", 《中国非金属矿工业导刊》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112320794A (en) * | 2020-10-29 | 2021-02-05 | 中国科学院过程工程研究所 | Deep impurity removal method for waste battery cathode recycling decommissioned graphite |
| CN115924907A (en) * | 2022-12-21 | 2023-04-07 | 江苏金亚隆科技有限公司 | Physical purification process of graphite raw material |
| CN115924907B (en) * | 2022-12-21 | 2023-07-14 | 江苏金亚隆科技有限公司 | Physical purification process of graphite raw material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JPH10152354A (en) | Method for treating manganese slag | |
| CN106587116A (en) | Method for extracting lithium carbonate and aluminum hydroxide through lepidolite and fly ash | |
| CN113999970B (en) | Method for extracting lithium from lithium porcelain stone mineral by roasting through mixed sulfate process | |
| CN111151370A (en) | Production method of high-quality ultra-pure fine iron powder | |
| CN111252761A (en) | Purification method of graphite negative electrode material | |
| KR101054832B1 (en) | Manufacturing method of zinc oxide powder recycled zinc-containing waste acid | |
| CN104150489B (en) | Quartz mine method of purification and gained quartz products | |
| CN105256130A (en) | Method for recycling chloride process titanium dioxide chlorination furnace blown-out materials containing fine-grain rutile | |
| CN113998680A (en) | Method for preparing lithium iron phosphate anode material by taking high-iron Bayer process red mud as iron source | |
| CN101148268A (en) | Method for separating and extracting calcium tungstate and tin slag by utilizing tungsten-containing tin furnace residue or tungsten-tin middlings | |
| KR101186170B1 (en) | The method of withdrawing zinc oxide from waste powder of steel making | |
| CN110600737B (en) | Preparation method of graphite negative electrode material | |
| CN1284259C (en) | Method for preparing manganese-zinc ferrite granules and mixed carbonate by using waste dry batteries | |
| CN100586617C (en) | Method for recycling and preparing ultra-fine zinc dust from zinc dust containing material | |
| EP0632514B1 (en) | Process for recycling used-up dry cells, and ferrite production process | |
| CN110606675B (en) | Vanadium-titanium slag superfine powder admixture and preparation method thereof | |
| CN114405659A (en) | Process method for producing ceramic material based on granite machine-made sand tailings | |
| CN107557590A (en) | Zinc dross recoverying and utilizing method | |
| CN105290410A (en) | Method for preparing and reducing iron powder through steelmaking sludge | |
| CN110369119A (en) | Comprehensive recovery process for iron, carbon and zinc in steel mill dust waste | |
| CN107127046A (en) | A kind of rutile chats comprehensive utilization process | |
| CN114835132B (en) | High-efficiency energy-saving process for processing coal-series kaolin by dry and wet method | |
| KR100857725B1 (en) | Purification method for limestone | |
| KR20210042099A (en) | Manufacturing method of purified lithium compound and manufacturing method of lithium transition metal composite oxide | |
| CN115572159A (en) | Method for preparing manganese-zinc ferrite material from copper-manganese waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20200609 |
|
| RJ01 | Rejection of invention patent application after publication |