CN113916713A - Separation and determination method of graphite impurities - Google Patents
Separation and determination method of graphite impurities Download PDFInfo
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- CN113916713A CN113916713A CN202111144321.5A CN202111144321A CN113916713A CN 113916713 A CN113916713 A CN 113916713A CN 202111144321 A CN202111144321 A CN 202111144321A CN 113916713 A CN113916713 A CN 113916713A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 185
- 239000010439 graphite Substances 0.000 title claims abstract description 161
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 161
- 239000012535 impurity Substances 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 47
- 238000000926 separation method Methods 0.000 title claims abstract description 18
- 239000002002 slurry Substances 0.000 claims abstract description 59
- 239000000126 substance Substances 0.000 claims abstract description 39
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 38
- 239000002994 raw material Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 238000004458 analytical method Methods 0.000 claims abstract description 25
- 239000002270 dispersing agent Substances 0.000 claims abstract description 25
- 239000000203 mixture Substances 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000002244 precipitate Substances 0.000 claims abstract description 19
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 238000002156 mixing Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000001914 filtration Methods 0.000 claims abstract description 10
- 229910052573 porcelain Inorganic materials 0.000 claims description 70
- 238000001354 calcination Methods 0.000 claims description 57
- 239000002956 ash Substances 0.000 claims description 41
- 235000002918 Fraxinus excelsior Nutrition 0.000 claims description 21
- 230000005484 gravity Effects 0.000 claims description 14
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 239000000178 monomer Substances 0.000 claims description 11
- 238000004140 cleaning Methods 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000691 measurement method Methods 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 6
- 238000010494 dissociation reaction Methods 0.000 claims description 4
- 230000005593 dissociations Effects 0.000 claims description 4
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 4
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 4
- 235000007715 potassium iodide Nutrition 0.000 claims description 2
- 235000019353 potassium silicate Nutrition 0.000 claims description 2
- FQENQNTWSFEDLI-UHFFFAOYSA-J sodium diphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]P([O-])(=O)OP([O-])([O-])=O FQENQNTWSFEDLI-UHFFFAOYSA-J 0.000 claims description 2
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 2
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 2
- 235000009518 sodium iodide Nutrition 0.000 claims description 2
- 229940048086 sodium pyrophosphate Drugs 0.000 claims description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 2
- 235000019818 tetrasodium diphosphate Nutrition 0.000 claims description 2
- 239000011592 zinc chloride Substances 0.000 claims description 2
- 235000005074 zinc chloride Nutrition 0.000 claims description 2
- 238000003556 assay Methods 0.000 claims 4
- 238000000746 purification Methods 0.000 abstract description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 5
- 239000011707 mineral Substances 0.000 abstract description 5
- 229910052799 carbon Inorganic materials 0.000 description 27
- 230000000052 comparative effect Effects 0.000 description 22
- 238000005188 flotation Methods 0.000 description 12
- 239000000047 product Substances 0.000 description 8
- 239000012141 concentrate Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 239000006185 dispersion Substances 0.000 description 4
- 235000010755 mineral Nutrition 0.000 description 4
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 239000007858 starting material Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 229910000861 Mg alloy Inorganic materials 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical class [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- KEAYESYHFKHZAL-UHFFFAOYSA-N Sodium Chemical class [Na] KEAYESYHFKHZAL-UHFFFAOYSA-N 0.000 description 1
- LCKIEQZJEYYRIY-UHFFFAOYSA-N Titanium ion Chemical compound [Ti+4] LCKIEQZJEYYRIY-UHFFFAOYSA-N 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- RICLFGYGYQXUFH-UHFFFAOYSA-N buspirone hydrochloride Chemical compound [H+].[Cl-].C1C(=O)N(CCCCN2CCN(CC2)C=2N=CC=CN=2)C(=O)CC21CCCC2 RICLFGYGYQXUFH-UHFFFAOYSA-N 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 229910052729 chemical element Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000010433 feldspar Substances 0.000 description 1
- 239000004088 foaming agent Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 239000003350 kerosene Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a method for separating and measuring graphite impurities. The separation and determination method of the invention comprises the following steps: 1) mixing a graphite raw material with water, and grinding to obtain slurry; 2) adding a dispersing agent into the slurry and then performing ultrasonic dispersion; 3) preparing the slurry subjected to ultrasonic dispersion into heavy liquid; 4) stirring and dispersing the heavy liquid; 5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities; 6) and (4) measuring impurity components of the upper-layer high-purity graphite to obtain the specific chemical composition and the content of the impurity components. The method for separating and determining the graphite impurities realizes convenient and efficient separation of graphite and gangue minerals, performs accurate composition and content analysis on the impurities in the separated high-purity graphite, and provides support for high-value utilization and further efficient purification of graphite, particularly the high-purity graphite.
Description
Technical Field
The invention relates to the technical field of graphite purification, relates to a method for separating and determining graphite impurities, and particularly relates to a method for separating and determining high-purity graphite impurities.
Background
Graphite is a strategic mineral resource in China, not only can be applied to basic traditional industries, but also can be applied to strategic emerging industrial fields of new energy automobiles, energy storage, environmental protection and the like and high-end leading-edge fields of aerospace, national defense, electronic information, energy safety and the like, and the purity of graphite is the most main factor influencing the application field and the application value of graphite. The high-carbon graphite, especially the high-purity graphite with the fixed carbon content of more than 99.5 percent, has wider application field and higher application value, and simultaneously, the composition and the content of impurity components in the graphite are also important factors influencing the application field and the application value of the graphite. Therefore, accurate analysis of impurity components in high-carbon graphite and high-purity graphite is the key to realizing high-value utilization of graphite and further purifying graphite efficiently.
At present, the conventional purification method of graphite is mainly a flotation method. The flotation method is mainly characterized in that the fixed carbon content in the concentrate product is improved through a multi-stage ore grinding and multi-stage flotation process, the common processes include eight-grinding nine-selection, nine-grinding eleven-selection and the like, and the fixed carbon content of the concentrate product in the flotation method is about 90-95%. The conventional flotation method has the problems of complex process, long flow, high energy consumption and the like, and simultaneously has higher difficulty in purifying the earthy graphite of the product with fine graphite granularity and relatively high fixed carbon content and the flake graphite with fine graphite embedding characteristics. Even though graphite is separated from most impurities by a flotation method, the separated graphite part still has impurities although the purity is high, and the impurity analysis of the high-purity graphite part is difficult to be accurate.
At present, the analysis of the impurity components in the graphite adopts an analysis method of ash in GB/T3521-. Firstly, 0.3-2 g of dried sample is weighed and placed in a sample boat, and the sample boat is burned in a pyrolysis furnace at 900-1000 ℃ to constant weight to obtain a residue, namely ash, namely an impurity component in graphite. However, in the case of graphite having a high fixed carbon content such as high-carbon graphite and high-purity graphite, since the content of impurity components is relatively small, there is a problem that the error in the test by this method is large. In addition, the content of impurity components in the high-carbon graphite and the high-purity graphite is relatively low, and great errors exist in the analysis of specific chemical components and content of the graphite by directly adopting chemical element analysis and XRF analysis and test methods. The analytical error is greater when the graphite purity is higher.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for separating and determining graphite impurities, which realizes convenient and efficient separation of graphite and gangue minerals, accurately analyzes the components and contents of the impurities in the separated high-purity graphite, and provides a support for high-value utilization and further high-efficiency purification of graphite, particularly high-purity graphite.
In order to achieve the purpose, the invention adopts the following technical scheme:
a method for separating and measuring graphite impurities comprises the following steps:
1) mixing a graphite raw material with water, and grinding the mixture to achieve monomer dissociation of the graphite component to obtain slurry;
2) adding a dispersing agent into the slurry obtained in the step 1) and then carrying out ultrasonic dispersion;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into heavy liquid;
4) stirring and dispersing the heavy liquid, and standing to obtain an upper-layer suspended matter and a lower-layer precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) and 5) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain the specific chemical composition and content of the impurity components.
The method for separating and measuring the graphite impurities comprises the steps of fully grinding and dispersing to enable graphite components to be dissociated into monomers; then, by utilizing the density difference between the graphite component and impurity components such as quartz, feldspar, mica, calcite, kaolin and the like, dense medium sedimentation separation is carried out by preparing heavy liquid, so that the convenient and efficient separation of graphite and gangue minerals is realized, and the method is particularly suitable for earthy graphite of products with fine graphite granularity and relatively high fixed carbon content and flake graphite with fine graphite embedding characteristics; and then, the separated impurity components, particularly impurities in the high-purity graphite, are subjected to chemical component analysis, so that the quantity and quality of sample analysis are improved on the one hand, the difference of the quality of the porcelain boat and other containers before and after calcination is fully considered on the other hand, the accurate analysis of ash content in the high-purity graphite is realized through the two paths, the content of specific impurity components of the high-purity graphite is obtained through further chemical component analysis of the ash content, and a support is provided for high-value utilization and further high-efficiency purification of the graphite, particularly the high-purity graphite.
The high-purity graphite of the present invention is graphite having a fixed carbon content of not less than 99.5%.
In the step 1), the mass ratio of the graphite raw material to water is 1: 1-1: 10, for example, 1:1, 1:2, 1:3, 1:4, 1:5, 1:6, 1:7, 1:8, 1:9, 1:10, and the like.
Preferably, the fineness of the ground ore is D90 ≤ 25 μm.
In step 2), the mass of the dispersant is 2% or less of the mass of the slurry, for example, 0.1%, 0.5%, 1%, 1.5%, 1.8%, or the like of the mass of the slurry.
Preferably, the dispersant is one of water glass, sodium hexametaphosphate or sodium pyrophosphate.
Preferably, the frequency of the ultrasonic dispersion is 20-80 kHz, such as 20kHz, 30kHz, 40kHz, 50kHz, 60kHz, 70kHz, 80kHz, and the like, and the time of the ultrasonic dispersion is more than or equal to 30 min.
In the step 3), the water-soluble high-density reagent is one of zinc chloride, sodium iodide or potassium iodide.
Preferably, the specific gravity of the slurry in the heavy liquid is 2.3-2.5 g/cm3E.g. specific gravity of 2.3g/cm3、2.4g/cm3Or 2.5g/cm3And the like.
In the step 4), the stirring speed is 300-1000 r/min, such as 300r/min, 400r/min, 500r/min, 600r/min, 700r/min, 800r/min, 900r/min or 1000 r/min; the stirring time is 5-20 min, such as 5min, 6min, 7min, 8min, 9min, 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20 min.
The specific determination method of the step 6) comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 … … to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3… … to GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3… … to NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3… … to MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+……+(NQ-MQ)/GQ]/Q×100％；
wherein A: ash content of the sample;
N1、N2、N3……NQ: the quality of the porcelain boat and the residue after high-temperature calcination;
M1、M2、M3……MQ: the mass of the empty porcelain boat;
G1、G2、G3……GQ: the mass of the high purity graphite sample;
q: the number of samples;
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY(ii) a Such as SiO in ash2、Al2O3、Fe2O3、TiO2、K2O、Na2The content of O, CaO and MgO … … is BSilicon、BAluminium、BIron、BTitanium (IV)、BPotassium salt、BSodium salt、BCalcium carbonate、BMagnesium alloy……；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A
wherein C isY: the content of a chemical component Y in the high-purity graphite sample;
BY: the content of a chemical component Y in ash content of the high-purity graphite sample;
a: ash test results for the samples.
The determination method analyzes chemical components of impurities in the high-purity graphite, on one hand, improves the quantity and quality of sample analysis, on the other hand, fully considers the difference of the quality of the porcelain boat and other containers before and after calcination, realizes accurate analysis of ash content in the high-purity graphite through the two paths, and obtains the content of specific impurity components of the high-purity graphite through further chemical component analysis of the ash content. The determination method is particularly suitable for testing and analyzing the ash content and impurity content of high-carbon graphite, particularly high-purity graphite with the fixed carbon content of more than or equal to 99.5%.
In the step a), the calcining temperature is 800-1000 ℃, such as 800 ℃, 850 ℃, 900 ℃, 950 ℃ or 1000 ℃ and the like; the calcination time is 0.5-2 h, such as 0.5h, 1h, 1.5h or 2 h.
Preferably, the capacity of the porcelain boat is more than or equal to 3g, and Q is more than or equal to 7.
In the step c), the calcining temperature W is 800-1000 ℃, and the calcining time H is 0.5-2H.
The calcining temperature and calcining time of the step d) are the same as those of the step c).
In a preferred embodiment of the present invention, the method for separating and measuring graphite impurities comprises the steps of:
1) mixing a graphite raw material and water, and grinding the mixture to achieve monomer dissociation of graphite components to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1: 1-1: 10, and the fineness of the ground ore is D90 not more than 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is less than 2% of the mass of the slurry, the frequency of the ultrasonic dispersion is 20-80 kHz, and the time of the ultrasonic dispersion is more than or equal to 30 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.3-2.5 g/cm3The heavy liquid of (4);
4) stirring the heavy liquid at a stirring speed of 300-1000 r/min for 5-20 min for dispersing, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) and 5) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain the specific chemical composition and content of the impurity components.
Compared with the prior art, the invention has the beneficial effects that:
the method for separating and determining the graphite impurities realizes convenient and efficient separation of graphite and gangue minerals, performs accurate composition and content analysis on the impurities in the separated high-purity graphite, and provides support for high-value utilization and further efficient purification of graphite, particularly the high-purity graphite.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments.
Unless otherwise specified, various starting materials of the present invention are commercially available or prepared according to conventional methods in the art.
Example 1
The method for separating and measuring graphite impurities in the embodiment comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:1, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is 2% of the mass of the slurry, the ultrasonic dispersion frequency is 20kHz, and the ultrasonic dispersion time is 30 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.3g/cm3The heavy liquid of (4);
4) stirring the heavy liquid at a stirring speed of 300r/min for 20min for dispersion, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain specific chemical compositions and contents of the impurity components, wherein the specific measuring method comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
specific compositions and amounts of impurities can be obtained finally through the steps 5) and 6), and specific experimental results are shown in table 1.
Example 2
The method for separating and measuring graphite impurities in the embodiment comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:10, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is 0.5% of the mass of the slurry, the ultrasonic dispersion frequency is 30kHz, and the ultrasonic dispersion time is 25 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.5g/cm3The heavy liquid of (4);
4) stirring the heavy liquid at a stirring speed of 1000r/min for 20min for dispersion, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain specific chemical compositions and contents of the impurity components, wherein the specific measuring method comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
specific compositions and amounts of impurities can be obtained finally through the steps 5) and 6), and specific experimental results are shown in table 1. Example 3
The method for separating and measuring graphite impurities in the embodiment comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:3, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is 1% of the mass of the slurry, the ultrasonic dispersion frequency is 40kHz, and the ultrasonic dispersion time is 20 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.4g/cm3The heavy liquid of (4);
4) stirring the heavy liquid at a stirring speed of 500r/min for 15min for dispersing, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain specific chemical compositions and contents of the impurity components, wherein the specific measuring method comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
specific compositions and amounts of impurities can be obtained finally through the steps 5) and 6), and specific experimental results are shown in table 1. Example 4
The method for separating and measuring graphite impurities in the embodiment comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:5, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is 1.5% of the mass of the slurry, the ultrasonic dispersion frequency is 60kHz, and the ultrasonic dispersion time is 15 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.45g/cm3The heavy liquid of (4);
4) stirring the heavy liquid for 10min at the stirring speed of 700r/min for dispersion, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain specific chemical compositions and contents of the impurity components, wherein the specific measuring method comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper layer high purity obtained in the step 5) into each porcelain boat after calcinationG is the quality of the high-purity graphite added into each porcelain boat1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
specific compositions and amounts of impurities can be obtained finally through the steps 5) and 6), and specific experimental results are shown in table 1.
Example 5
The method for separating and measuring graphite impurities in the embodiment comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:7, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is 0.8% of the mass of the slurry, the ultrasonic dispersion frequency is 80kHz, and the ultrasonic dispersion time is 10 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.35g/cm3The heavy liquid of (4);
4) stirring the heavy liquid for 5min at the stirring speed of 900r/min for dispersion, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain specific chemical compositions and contents of the impurity components, wherein the specific measuring method comprises the following steps:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
specific compositions and amounts of impurities can be obtained finally through the steps 5) and 6), and specific experimental results are shown in table 1.
Example 6
This comparative example differs from example 1 in that the graphite starting material used in step 1) had a fixed carbon content of 95%, and was otherwise the same as example 1.
Comparative example 1
The comparative example adopts a conventional grinding and floating process and comprises the following steps:
1) mixing a graphite raw material (with the fixed carbon content of 85%) and water, and grinding to separate the monomers of the graphite component to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1:10, and the fineness of the ground ore is D90 which is less than or equal to 25 mu m;
2) adding the ground graphite raw material into a flotation machine for flotation, wherein the flotation concentration is 10%, the consumption of collecting agent kerosene is 100kg/t, the consumption of foaming agent No. 2 oil is 50g/t, and the flotation time is 2 min;
3) concentrating the flotation concentrate obtained in the step 2) twice to obtain a concentrate product;
4) the concentrate product is filtered and dried, and the determination of the impurity components is carried out to obtain the specific chemical composition and the content of the impurity components, and the specific determination method is the same as the step 6) in the example 1.
Comparative example 2
The comparative example is different from example 1 in that the mass ratio of the graphite raw material to water in step 1) is 2:1, and the rest is the same as example 1.
Comparative example 3
This comparative example differs from example 1 in that no dispersant was added in step 2), and the rest is the same as example 1.
Comparative example 4
This comparative example differs from example 1 in that in step 2), the dispersant was used in an amount of 5%, and the rest was the same as in example 1.
Comparative example 5
This comparative example is different from example 1 in that, in step 3), the specific gravity of the heavy liquid was 2g/cm3The rest is the same as in example 1.
Comparative example 6
This comparative example is different from example 1 in that, in step 3), the specific gravity of the heavy liquid was 3g/cm3The rest is the same as in example 1.
Comparative example 7
This comparative example differs from example 1 in that, in step 6) the specific measurement method, the number of test samples Q was 3, and the others were the same as those of example 1.
Comparative example 8
This comparative example is different from example 1 in that the specific measurement method of step 6) is the same as that of example 1 except that the empty boat is not calcined in step d).
TABLE 1
As can be seen from Table 1, the high-purity graphite concentrate can be obtained by the separation method, the fixed carbon content of the graphite raw material can be improved from 85% to 99.4-99.6%, and the ash content is 0.35-0.53%.
In example 6, the fixed carbon content of the graphite raw material used was 95%, and high purity graphite having a fixed carbon content of 99.9% was obtained, indicating that the higher the purity of the raw material, the higher the purity of the product.
In comparative example 1, the fixed carbon content of the obtained high-purity graphite is 94.7% by adopting the conventional grinding and floating process, which is far lower than that of example 1, and the effect of the method is better than that of the conventional flotation process.
In comparative examples 2, 3 and 4, too large a mass ratio of the graphite raw material to water in the ore grinding, and too much dispersant or dispersant is not added, which results in a decrease in the yield of high purity graphite and a decrease in the fixed carbon content.
In comparative example 5, the production of high purity graphite was greatly reduced due to the excessively low specific gravity of the heavy liquid.
In comparative example 6, the heavy liquid has an excessively high specific gravity, which results in a large increase in the yield of high-purity graphite and a large decrease in the fixed carbon content.
In comparative examples 7 and 8, the test analysis of the fixed carbon content and ash content is larger due to the small amount of the test analysis sample or the non-calcination of the empty porcelain boat.
The present invention is illustrated by the above-mentioned examples, but the present invention is not limited to the above-mentioned detailed process equipment and process flow, i.e. it is not meant to imply that the present invention must rely on the above-mentioned detailed process equipment and process flow to be practiced. It should be understood by those skilled in the art that any modification of the present invention, equivalent substitutions of the raw materials of the product of the present invention, addition of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (10)
1. A method for separating and measuring graphite impurities, which is characterized by comprising the following steps:
1) mixing a graphite raw material with water, and grinding the mixture to achieve monomer dissociation of the graphite component to obtain slurry;
2) adding a dispersing agent into the slurry obtained in the step 1) and then carrying out ultrasonic dispersion;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into heavy liquid;
4) stirring and dispersing the heavy liquid, and standing to obtain an upper-layer suspended matter and a lower-layer precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) and 5) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain the specific chemical composition and content of the impurity components.
2. The separation and determination method according to claim 1, wherein in the step 1), the mass ratio of the graphite raw material to water is 1:1 to 1: 10;
preferably, the fineness of the ground ore is D90 ≤ 25 μm.
3. The separation and measurement method according to claim 1 or 2, wherein in step 2), the mass of the dispersant is 2% or less of the mass of the slurry;
preferably, the dispersant is one of water glass, sodium hexametaphosphate or sodium pyrophosphate;
preferably, the frequency of ultrasonic dispersion is 20-80 kHz, and the time of ultrasonic dispersion is more than or equal to 30 min.
4. A separation and assay method according to one of claims 1 to 3, wherein, in the step 3), the water-soluble high-density reagent is one of zinc chloride, sodium iodide or potassium iodide;
preferably, in said heavy liquidThe specific gravity of the slurry is 2.3-2.5 g/cm3。
5. A separation and measurement method according to any one of claims 1 to 4, wherein in the step 4), the stirring speed is 300 to 1000r/min, and the stirring time is 5 to 20 min.
6. A separation and assay method according to any one of claims 1 to 5, wherein the specific assay method of step 6) is:
a) taking Q porcelain boats, numbering 1, 2, 3 to Q, and calcining at high temperature;
b) adding the upper-layer high-purity graphite obtained in the step 5) into each calcined porcelain boat, and sequentially marking the mass of the high-purity graphite added into each porcelain boat as G1、G2、G3To GQ；
c) Calcining the porcelain boat to constant weight under the high-temperature condition that the calcining temperature is W, recording the accumulated calcining time as H, and recording the mass of the cooled porcelain boat and the residue as N in sequence1、N2、N3To NQ；
d) Cleaning the residues in the porcelain boat, calcining the empty porcelain boat for H time under the high-temperature condition of the calcining temperature W, taking out and cooling the empty porcelain boat, and recording the mass of the empty porcelain boat as M in sequence1、M2、M3To MQ；
e) Ash results for the samples were obtained by the following formula:
A＝[(N1-M1)/G1+(N2-M2)/G2+(N3-M3)/G3+(NQ-MQ)/GQ]/Q×100％；
f) fully and uniformly mixing the obtained Q ashes, and then carrying out chemical component analysis to obtain specific chemical components and content of the ashes, wherein the content of the chemical component Y in the ashes is recorded as BY；
g) The specific content of impurity components in the graphite is obtained by the following formula:
CY＝BY*A。
7. the separation and measurement method according to claim 6, wherein in the step a), the calcination temperature is 800 to 1000 ℃, and the calcination time is 0.5 to 2 hours;
preferably, the capacity of the porcelain boat is more than or equal to 3g, and Q is more than or equal to 7.
8. A separation and measurement method according to claim 6 or 7, wherein in the step c), the calcination temperature W is 800 to 1000 ℃, and the calcination time H is 0.5 to 2 hours.
9. The separation and measurement method according to claim 8, wherein the calcination temperature and calcination time of step d) and step c) are the same.
10. A separation and assay method according to one of claims 1 to 9, characterized in that it comprises the following steps:
1) mixing a graphite raw material and water, and grinding the mixture to achieve monomer dissociation of graphite components to obtain slurry, wherein the mass ratio of the graphite raw material to the water is 1: 1-1: 10, and the fineness of the ground ore is D90 not more than 25 mu m;
2) adding a dispersing agent into the slurry obtained in the step 1), and then performing ultrasonic dispersion, wherein the mass of the dispersing agent is less than 2% of the mass of the slurry, the frequency of the ultrasonic dispersion is 20-80 kHz, and the time of the ultrasonic dispersion is more than or equal to 30 min;
3) adding a water-soluble high-density reagent into the slurry subjected to ultrasonic dispersion in the step 2), and preparing the slurry into slurry with the specific gravity of 2.3-2.5 g/cm3The heavy liquid of (4);
4) stirring the heavy liquid at a stirring speed of 300-1000 r/min for 5-20 min for dispersing, and standing to obtain an upper suspension and a lower precipitate;
5) separating, filtering and drying the upper-layer suspended matter and the lower-layer precipitate to obtain upper-layer high-purity graphite and lower-layer impurities, and calculating the percentage content of the impurities;
6) and 5) measuring impurity components of the upper-layer high-purity graphite obtained in the step 5) to obtain the specific chemical composition and content of the impurity components.
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