CN105823712B - A kind of method for measuring flaky graphite content in crystalline flake graphite ore deposit - Google Patents
A kind of method for measuring flaky graphite content in crystalline flake graphite ore deposit Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 96
- 239000010439 graphite Substances 0.000 title claims abstract description 94
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 94
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000002253 acid Substances 0.000 claims abstract description 16
- 239000002245 particle Substances 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- 238000001816 cooling Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 6
- 229910017604 nitric acid Inorganic materials 0.000 claims description 6
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- 239000011261 inert gas Substances 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000003837 high-temperature calcination Methods 0.000 claims description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000001914 filtration Methods 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000004062 sedimentation Methods 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 15
- 239000011707 mineral Substances 0.000 abstract description 15
- 241001282153 Scopelogadus mizolepis Species 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract description 4
- 238000004090 dissolution Methods 0.000 abstract description 3
- 238000010494 dissociation reaction Methods 0.000 abstract description 2
- 230000005593 dissociations Effects 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000005259 measurement Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 5
- 239000004575 stone Substances 0.000 description 5
- 235000012239 silicon dioxide Nutrition 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 239000010453 quartz Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 229910052626 biotite Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000010433 feldspar Substances 0.000 description 2
- 239000011028 pyrite Substances 0.000 description 2
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 2
- 229910052683 pyrite Inorganic materials 0.000 description 2
- 229910052889 tremolite Inorganic materials 0.000 description 2
- 229910021532 Calcite Inorganic materials 0.000 description 1
- 206010011376 Crepitations Diseases 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- 150000001336 alkenes Chemical class 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- YGANSGVIUGARFR-UHFFFAOYSA-N dipotassium dioxosilane oxo(oxoalumanyloxy)alumane oxygen(2-) Chemical compound [O--].[K+].[K+].O=[Si]=O.O=[Al]O[Al]=O YGANSGVIUGARFR-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
- 239000002223 garnet Substances 0.000 description 1
- 239000010440 gypsum Substances 0.000 description 1
- 229910052602 gypsum Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000013011 mating Effects 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 229910052651 microcline Inorganic materials 0.000 description 1
- 229910052627 muscovite Inorganic materials 0.000 description 1
- 229910052655 plagioclase feldspar Inorganic materials 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000009738 saturating Methods 0.000 description 1
- 230000035939 shock Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume or surface-area of porous materials
- G01N15/02—Investigating particle size or size distribution
- G01N15/0272—Investigating particle size or size distribution with screening; with classification by filtering
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/286—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q involving mechanical work, e.g. chopping, disintegrating, compacting, homogenising
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
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- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
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Abstract
The invention discloses a kind of methods for measuring flaky graphite content in crystalline flake graphite ore deposit.This method is crushed using hot tearing, the powder ore in the case where not destroying graphite flakes, realize the dissociation of graphite and gangue mineral, fall gangue mineral with mixed-acid dissolution again, not only purity is high, and substantially remains in the original preservation granularity in tcrude ore for the graphite finally obtained, for measuring the big scale content of graphite and size distribution, the particle property of graphite in graphite raw ore can be accurately reflected, measurement result helps more accurately to assess the value of graphite ore.
Description
Technical field
The present invention relates to a kind of mineral content assay methods, particularly measure flaky graphite content in crystalline flake graphite ore deposit
Method belongs to technical field of mineral processing.
Background technology
Graphite is a kind of critically important raw material of industry, is the essential emerging nonmetallic materials of current hi-tech development
One of, application field is very extensive.Industrially, according to crystal habit difference, by native graphite be divided into compact crystal shape graphite,
Crystalline flake graphite, aphanitic graphite three classes.Wherein the floatability of crystalline flake graphite, lubricity, plasticity are more excellent than other types graphite
More, therefore its industrial value is maximum.And flaky graphite then has even more important application value.
Usual flaky graphite refers to the crystalline flake graphite of+100 mesh, compared to the ramentum graphite of -100 mesh, big scale stone
Performance of ink is more excellent, can not it is artificial synthesized, be difficult to substitute, price is the several times of same grade ramentum graphite price or even tens of
Times.Thus the content of flaky graphite is to judge the important indicator of graphite ore value.
At present, all it is to pass through rock-mineral determination using mineral mating plate, thin slice to flaky graphite content's index in graphite ore
Method substantially judges, according to distribution characteristics of the graphite particle on point, face infers the particle property of graphite ore particle entirety,
As a result there is certain deviation.The content of flaky graphite in Accurate Determining graphite ore is wanted, needs a kind of Direct Determination.Directly
Flaky graphite content in ore is measured, the main difficulty encountered is the crushing of ore, should ore be crushed to finer grain
In order to which graphite detaches with gangue mineral, measures, and cannot graphite flakes be generated with destruction, current existing usual manner is difficult
To solve the problems, such as this.
Graphite has high-temperature stability, and its intensity is strengthened with the raising of temperature, so being passed through under inert gas shielding
High-temperature calcination, graphite particle will not be oxidized, and will not generate the breakoff phenomenons such as fragmentation.Graphite ore is after high-temperature calcination, immediately
Quickly cooling in cold water is put into, since the coefficient of thermal expansion of different minerals in ore is different, the change dramatically of temperature will make different minerals
Volumetric stress is generated on particle faying face and nugget is caused to generate a large amount of crackles, and intensity is substantially reduced, can be broken to by hand
3mm hereinafter, and graphite flakes then due to good thermal shock resistance, being amenable to high temperature variation without being destroyed, this
It can realize that the mineral under the premise of protection graphite flakes crush.Sample ore after crushing can dissolve all silicic acid with hydrofluoric acid
Salt gangue, hydrochloric acid, nitric acid then can dissolve the hydrofluoric acid insoluble matters such as fluorite, and play the role of promoting hydrofluoric acid dissolution silicate,
Effect through mixed acid is solvable to take off whole gangue minerals；Graphite due to its good chemical stability, will not be then dissolved.Base
In the graphite ore processing method of above-mentioned principle, the graphite particle purity finally obtained is high, and keeps original preservation granularity, is used for
The big scale content of graphite and size distribution are measured, the particle property of graphite in graphite raw ore can be accurately reflected.
Invention content
The present invention provides a kind of methods for measuring flaky graphite content in crystalline flake graphite ore deposit.The method of the present invention include with
Lower step：
(1) representational graphite nugget is chosen according to sampling specification, granularity 30mm ~ 100mm is dried in an oven；
(2) in the case that graphite nugget is passed through inert gas shielding in high temperature furnace, 400 DEG C ~ 800 DEG C high-temperature calcinations 3 ~ 10
Minute；
(3) graphite nugget is taken out, is immediately placed in rapid cooling in normal-temperature water；
(4) graphite nugget after cooling is taken out, and hand-crushed to 3mm in baking oven hereinafter, dry；
(5) graphite ore is contained in polytetrafluoroethylene beaker, is added in mixed acid by liquid-solid ratio 0.5 ~ 4, is stirred at 30 ~ 70 DEG C
Resolution 1 ~ 5 hour；Standing sedimentation pours out supernatant, repeats the step 1 ~ 4 time；
(6), by sample ore filtering, cleaning, the drying after resolution, graphite powder is obtained, is sieved with standard screen, measures flaky graphite
The graphite particle sizes characteristic such as content.
The step (2) inert gas, refers to one kind in carbon dioxide or nitrogen.
The step (4) hand-crushed is referred to break into pieces with one's fingers by hand and be rolled by hand using tools such as wooden stick, iron staffs.
The step (5) mixed acid, by hydrofluoric acid：Hydrochloric acid：Nitric acid：Water=4：3：1 ratio is prepared.
The present invention is crushed using hot tearing, the powder ore in the case where not destroying graphite flakes, realizes graphite and gangue ore deposit
The dissociation of object, then fall gangue mineral with mixed-acid dissolution, not only purity is high, and substantially remains in raw ore for the graphite finally obtained
Original preservation granularity in stone for measuring the big scale content of graphite and size distribution, can accurately reflect graphite in graphite raw ore
Particle property, be of great significance for the value of accurate evaluation graphite ore.
Specific embodiment
Embodiment 1
Crystalline flake graphite ore deposit, graphite grade 18.76%, main gangue mineral is quartz, feldspar, muscovite, biotite, saturating brightness
Stone, the tremolite, calcite, pyrite etc..Totally 167.09 grams of 40mm ~ 100mm graphite nugget is chosen, in baking oven after 105 DEG C of drying,
It is put into high temperature furnace and 600 DEG C is heated in the case where being passed through carbon dioxide gas, after keeping the temperature 7 minutes, take out, be put into water rapidly
In, take out nugget after cooling, hand-crushed to 3mm hereinafter, in baking oven dry after be put into 1000ml polytetrafluoroethylene beakers,
Add in 400ml mixed acid（Hydrofluoric acid：Hydrochloric acid：Nitric acid=4：3：1）, it is placed in draught cupboard, is heated, stirred with magnetic force heating stirrer
It mixes 3 hours, stands 20 minutes, pour out supernatant；300ml mixed acid is added, clears up 4 hours, supernatant is poured out after standing；Again
Mixed acid 100ml is added in, after clearing up 2 hours, filters, clean together with the supernatant poured out before this, dried in baking oven, obtain stone
Black 31.97 grams of scale product is sieved 15 minutes ,+100 25.34 grams of mesh products with 100 mesh standard sieves, big scale in the graphite ore
Graphite proportion is 79.26%.The graphite products grade 99.64% finally obtained after measured.
Embodiment 2
Crystalline flake graphite ore deposit, graphite grade 12.53%, main gangue mineral is quartz, feldspar, hornblend, biotite, green mud
Stone, limonite, garnet etc..Totally 255.21 grams of 40mm ~ 100mm graphite nugget is chosen, in baking oven after 105 DEG C of drying, is put into height
650 DEG C are heated in warm stove in the case where being passed through carbon dioxide gas, after keeping the temperature 6 minutes, takes out, rapidly into the water, takes
Go out nugget after cooling, hand-crushed to 3mm in baking oven after drying hereinafter, be put into 1000ml polytetrafluoroethylene beakers, addition
600ml mixed acid（Hydrofluoric acid：Hydrochloric acid：Nitric acid=4：3：1）, it is placed in draught cupboard, it is small with the heating of magnetic force heating stirrer, stirring 4
When, 20 minutes are stood, pours out supernatant；500ml mixed acid is added, clears up 4 hours, supernatant is poured out after standing；It adds
Mixed acid 150ml after clearing up 2 hours, with the supernatant poured out before this filters, cleans, dried in baking oven, obtain graphite squama together
32.95 grams of flake products are sieved 15 minutes ,+100 22.45 grams of mesh products with 100 mesh standard sieves, flaky graphite in the graphite ore
Proportion is 68.13%.The graphite products grade 99.38% finally obtained after measured.
Embodiment 3
Crystalline flake graphite ore deposit, graphite grade 10.84%, gangue mineral be mainly quartz, microcline, plagioclase, the tremolite,
Mica, zoisite, gypsum, limonite, pyrite etc..Totally 267.72 grams of 40mm ~ 100mm graphite nugget is chosen, 105 DEG C in baking oven
After drying, it is put into high temperature furnace and 700 DEG C is heated in the case where being passed through carbon dioxide gas, heat preservation after five minutes, is taken out, fast
Speed into the water, takes out nugget after cooling, and hand-crushed to 3mm after drying in baking oven hereinafter, be put into 1000ml polytetrafluoroethyl-nes
In alkene beaker, 700ml mixed acid is added in（Hydrofluoric acid：Hydrochloric acid：Nitric acid=4：3：1）, it is placed in draught cupboard, with magnetic force heating stirring
Device heating, stirring 4 hours, stand 20 minutes, pour out supernatant；600ml mixed acid is added, clears up 4 hours, is poured out after standing
Supernatant；Mixed acid 200ml is added, after clearing up 2 hours, filters, clean together with the supernatant poured out before this, dried in baking oven
It is dry, 30.52 grams of graphite flakes product is obtained, is sieved 15 minutes with 100 mesh standard sieves ,+100 14.19 grams of mesh products, the graphite ore
Middle flaky graphite proportion is 46.49%.The graphite products grade 99.20% finally obtained after measured.
Claims (4)
1. a kind of method for measuring flaky graphite content in crystalline flake graphite ore deposit, this method include the following steps：
(1) representational graphite nugget is chosen according to sampling specification, granularity 30mm ~ 100mm is dried in an oven；
(2) in the case that graphite nugget is passed through inert gas shielding in high temperature furnace, 400 DEG C ~ 800 DEG C high-temperature calcinations 3 ~ 10 minutes；
(3) graphite nugget is taken out, is immediately placed in rapid cooling in normal-temperature water；
(4) graphite nugget after cooling is taken out, and hand-crushed to 3mm in baking oven hereinafter, dry；
(5) graphite ore is contained in polytetrafluoroethylene beaker, and mixed acid is added in by liquid-solid ratio 0.5 ~ 4, the stirring resolution 1 at 30 ~ 70 DEG C
~ 5 hours；Standing sedimentation pours out supernatant, repeats the step 1 ~ 4 time；
(6), by sample ore filtering, cleaning, the drying after resolution, graphite powder is obtained, is sieved with standard screen, measures flaky graphite content
Wait graphite particle sizes characteristic.
2. method according to claim 1, the present invention is characterized in that：The step (2) inert gas, refers to carbon dioxide
Or one kind in nitrogen.
3. method according to claim 1, the present invention is characterized in that：The step (4) hand-crushed refers to break into pieces with one's fingers by hand,
And it is rolled by hand using tools such as wooden stick, iron staffs.
4. method according to claim 1, the present invention is characterized in that：The step (5) mixed acid, by hydrofluoric acid：Hydrochloric acid：
Nitric acid=4：3：1 ratio is prepared.
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| CN106404482A (en) * | 2016-08-31 | 2017-02-15 | 大工（青岛）新能源材料技术研究院有限公司 | Pretreatment method for detection of silicon and aluminum contents in ceramics |
| CN107462452B (en) * | 2017-09-25 | 2020-07-07 | 苏州中材非金属矿工业设计研究院有限公司 | Method for measuring particle size distribution characteristics of flake graphite ore |
| CN108680412A (en) * | 2018-06-04 | 2018-10-19 | 中钢集团新型材料（浙江）有限公司 | A kind of sample preparation methods and test method for calcined coke coefficient of thermal expansion |
| CN114634179B (en) * | 2022-03-25 | 2024-04-12 | 矿冶科技集团有限公司 | Pretreatment equipment and method for graphite ore before grinding |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0350110A (en) * | 1989-07-19 | 1991-03-04 | Kansai Coke & Chem Co Ltd | Method for highly purifying graphite |
| CN1331048A (en) * | 2000-06-30 | 2002-01-16 | 郭东章 | Process for purifying natural 3R-type graphite ore |
| FR2831881B1 (en) * | 2001-11-02 | 2004-01-16 | Hubert Lauvray | PROCESS FOR THE PURIFICATION OF METALLURGICAL SILICON BY INDUCTIVE PLASMA COUPLED TO DIRECTIONAL SOLIDIFICATION AND DIRECT OBTAINING OF SOLAR QUALITY SILICON |
| CN1557704A (en) * | 2004-01-21 | 2004-12-29 | 敏 岳 | Method for purifying natural crystalline flake graphite of high purity |
| CN105271187A (en) * | 2015-09-10 | 2016-01-27 | 连云港江利达矿产品有限公司 | Graphite electrode production process |
-
2016
- 2016-03-08 CN CN201610129246.8A patent/CN105823712B/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0350110A (en) * | 1989-07-19 | 1991-03-04 | Kansai Coke & Chem Co Ltd | Method for highly purifying graphite |
| CN1331048A (en) * | 2000-06-30 | 2002-01-16 | 郭东章 | Process for purifying natural 3R-type graphite ore |
| FR2831881B1 (en) * | 2001-11-02 | 2004-01-16 | Hubert Lauvray | PROCESS FOR THE PURIFICATION OF METALLURGICAL SILICON BY INDUCTIVE PLASMA COUPLED TO DIRECTIONAL SOLIDIFICATION AND DIRECT OBTAINING OF SOLAR QUALITY SILICON |
| CN1557704A (en) * | 2004-01-21 | 2004-12-29 | 敏 岳 | Method for purifying natural crystalline flake graphite of high purity |
| CN105271187A (en) * | 2015-09-10 | 2016-01-27 | 连云港江利达矿产品有限公司 | Graphite electrode production process |
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