CN105823712A - Method for determining content of large flaky graphite in flaky graphite ore - Google Patents
Method for determining content of large flaky graphite in flaky graphite ore Download PDFInfo
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- CN105823712A CN105823712A CN201610129246.8A CN201610129246A CN105823712A CN 105823712 A CN105823712 A CN 105823712A CN 201610129246 A CN201610129246 A CN 201610129246A CN 105823712 A CN105823712 A CN 105823712A
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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
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- 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
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- 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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Abstract
The invention discloses a method for determining the content of large flaky graphite in a flaky graphite ore. The method comprises the following steps: crushing the ore without destroying graphite flakes through using heat cracking fragmentation to realize dissociation of graphite and gangue mineral, and dissolving the gangue mineral in a mixed acid. Finally obtained graphite has high purity, and basically keeps the original occurrence granularity of the raw ore. The method can be used for determining the content and the granularity distribution of the large graphite flakes, and can accurately reflect the granularity characteristic of graphite in the graphite raw ore, and a determination result is helpful for accurately assessing the values of the graphite ore.
Description
Technical field
The present invention relates to a kind of mineral content assay method, particularly measure the method for flaky graphite content in crystalline flake graphite ore deposit, belong to technical field of mineral processing.
Background technology
Graphite is a kind of critically important raw material of industry, is one of requisite emerging nonmetallic materials of current hi-tech development, and its application is quite varied.Industrial, different according to crystal habit, native graphite is divided into compact crystal shape graphite, crystalline flake graphite, aphanitic graphite three class.Wherein the floatability of crystalline flake graphite, lubricity, plasticity are all superior than other types graphite, and therefore its industrial value is maximum.Flaky graphite then has even more important using value.
Generally flaky graphite refers to the crystalline flake graphite of+100 mesh, compared to the ramentum graphite of-100 mesh, flaky graphite performance is more excellent, cannot synthetic, be difficult to substitute, its price is several times or even the decades of times of same grade ramentum graphite price.Thus the content of flaky graphite is to judge the important indicator that graphite ore is worth.
At present, to flaky graphite content's index in graphite ore, being all to utilize mineral mating plate, thin slice substantially to be judged by the method for rock-mineral determination, infer, according to graphite granule distribution characteristics on point, face, the particle property that graphite ore particle is overall, its result has certain deviation.Want the content of flaky graphite in Accurate Determining graphite ore, it is desirable to have a kind of Direct Determination.Directly measure flaky graphite content in Ore, the main difficulty run into is the pulverizing of Ore, Ore should be crushed to finer grain so that graphite separates with gangue mineral, measures, can not produce graphite flakes again and destroy, current existing usual manner is all difficult to solve this problem.
Graphite has high-temperature stability, and its intensity is strengthened with the raising of temperature, so through high-temperature calcination under inert gas shielding, graphite granule will not be oxidized, also will not produce the breakoff phenomenons such as fragmentation.Graphite ore is after high-temperature calcination; it is immediately placed in quickly cooling in cold water; owing in Ore, the thermal coefficient of expansion of different minerals is different; the drastically change of temperature will make to produce volumetric stress on different minerals granule faying face and cause nugget to produce a large amount of crackles; intensity is substantially reduced, and can be broken to below 3mm by hand, and graphite flakes is then owing to having good thermal shock resistance; being amenable to high temperature change and do not destroyed, this just can realize protecting the mineral under graphite flakes premise to pulverize.Sample ore after pulverizing, with Fluohydric acid. insoluble matters such as Fluohydric acid. solubilized all of silicates stone-like pulse, hydrochloric acid, nitric acid then solubilized fluorites, and has the effect promoting hydrofluoric acid dissolution silicate, and the effect of blended acid is solvable takes off whole gangue mineral；Graphite then due to its good chemical stability, will not be dissolved.Graphite ore processing method based on above-mentioned principle, the graphite granule purity finally obtained is high, and keeps original tax to deposit granularity, is used for measuring graphite big scale content and particle size distribution, can accurately reflect the particle property of graphite in graphite raw ore.
Summary of the invention
The invention provides and a kind of measure the method for flaky graphite content in crystalline flake graphite ore deposit.The inventive method comprises the following steps:
(1) choose representational graphite nugget, granularity 30mm ~ 100mm according to sampling specification, dry in an oven；
(2) in the case of 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) take out graphite nugget, be immediately placed in normal-temperature water and cool down rapidly；
(4) take out the graphite nugget after cooling, hand-crushed to below 3mm, baking oven is dried；
(5) during graphite ore is contained in polytetrafluoroethylene beaker, adding mixed acid by liquid-solid ratio 0.5 ~ 4, at 30 ~ 70 DEG C, stirring clears up 1 ~ 5 hour；Standing sedimentation, pours out supernatant, repeats this step 1 ~ 4 time；
(6) the sample ore after clearing up filters, cleans, dries, and obtains graphite powder, sieves with standard screen, measures the graphite particle size characteristics such as flaky graphite content.
The most described noble gas of step, refers to the one in carbon dioxide or nitrogen.
The most described hand-crushed of step, refers to manual breaking into pieces with one's fingers, and utilizes the instrument such as wooden stick, iron staff to roll by hand.
The most described mixed acid of step, by Fluohydric acid.: hydrochloric acid: nitric acid: the proportions of water=4:3:1.
The present invention utilizes hot tearing to crush, powder ore in the case of not destroying graphite flakes, realize dissociating of graphite and gangue mineral, gangue mineral is fallen again with mixed-acid dissolution, the graphite finally obtained not only purity is high, and granularity is deposited in the original tax substantially remained in tcrude ore, is used for measuring graphite big scale content and particle size distribution, can accurately reflect the particle property of graphite in graphite raw ore, the value for accurate evaluation graphite ore is significant.
Detailed description of the invention
Embodiment 1
Crystalline flake graphite ore deposit, graphite grade 18.76%, main gangue mineral is quartz, Anhydrite, white mica, biotite, diopside, the tremolite, calcite, pyrite etc..Choose 40mm ~ 100mm graphite nugget totally 167.09 grams, in baking oven after 105 DEG C of drying, put into and high temperature furnace is heated in the case of being passed through carbon dioxide 600 DEG C, after being incubated 7 minutes, take out, put into rapidly in water, take out the nugget after cooling, hand-crushed, to below 3mm, is put in 1000ml polytetrafluoroethylene beaker after drying in baking oven, adds 400ml mixed acid (Fluohydric acid.: hydrochloric acid: nitric acid=4:3:1), it is placed in fume hood, with the heating of magnetic force heating stirrer, stirring 3 hours, stand 20 minutes, pour out supernatant；Add 300ml mixed acid, clear up 4 hours, after standing, pour out supernatant；Add mixed acid 100ml, after clearing up 2 hours, filter in the lump with the supernatant poured out before this, clean, baking oven is dried, obtains graphite flakes product 31.97 grams, sieve 15 minutes with 100 mesh standard sieves, + 100 mesh products 25.34 grams, in this graphite ore, flaky graphite proportion is 79.26%.The final graphite products grade 99.64% obtained after measured.
Embodiment 2
Crystalline flake graphite ore deposit, graphite grade 12.53%, main gangue mineral is quartz, Anhydrite, hornblend, biotite, chlorite, limonite, garnet etc..Choose 40mm ~ 100mm graphite nugget totally 255.21 grams, in baking oven after 105 DEG C of drying, put into and high temperature furnace is heated in the case of being passed through carbon dioxide 650 DEG C, after being incubated 6 minutes, take out, put into rapidly in water, take out the nugget after cooling, hand-crushed, to below 3mm, is put in 1000ml polytetrafluoroethylene beaker after drying in baking oven, adds 600ml mixed acid (Fluohydric acid.: hydrochloric acid: nitric acid=4:3:1), it is placed in fume hood, with the heating of magnetic force heating stirrer, stirring 4 hours, stand 20 minutes, pour out supernatant；Add 500ml mixed acid, clear up 4 hours, after standing, pour out supernatant；Add mixed acid 150ml, after clearing up 2 hours, filter in the lump with the supernatant poured out before this, clean, baking oven is dried, obtains graphite flakes product 32.95 grams, sieve 15 minutes with 100 mesh standard sieves, + 100 mesh products 22.45 grams, in this graphite ore, flaky graphite proportion is 68.13%.The final graphite products grade 99.38% obtained after measured.
Embodiment 3
Crystalline flake graphite ore deposit, graphite grade 10.84%, gangue mineral predominantly quartz, microcline, plagioclase, the tremolite, Muscovitum, zoisite, Gypsum Fibrosum, limonite, pyrite etc..Choose 40mm ~ 100mm graphite nugget totally 267.72 grams, in baking oven after 105 DEG C of drying, put into and high temperature furnace is heated in the case of being passed through carbon dioxide 700 DEG C, after being incubated 5 minutes, take out, put into rapidly in water, take out the nugget after cooling, hand-crushed, to below 3mm, is put in 1000ml polytetrafluoroethylene beaker after drying in baking oven, adds 700ml mixed acid (Fluohydric acid.: hydrochloric acid: nitric acid=4:3:1), it is placed in fume hood, with the heating of magnetic force heating stirrer, stirring 4 hours, stand 20 minutes, pour out supernatant；Add 600ml mixed acid, clear up 4 hours, after standing, pour out supernatant；Add mixed acid 200ml, after clearing up 2 hours, filter in the lump with the supernatant poured out before this, clean, baking oven is dried, obtains graphite flakes product 30.52 grams, sieve 15 minutes with 100 mesh standard sieves, + 100 mesh products 14.19 grams, in this graphite ore, flaky graphite proportion is 46.49%.The final graphite products grade 99.20% obtained after measured.
Claims (4)
1. measuring a method for flaky graphite content in crystalline flake graphite ore deposit, the method comprises the following steps:
(1) choose representational graphite nugget, granularity 30mm ~ 100mm according to sampling specification, dry in an oven；
(2) in the case of 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) take out graphite nugget, be immediately placed in normal-temperature water and cool down rapidly；
(4) take out the graphite nugget after cooling, hand-crushed to below 3mm, baking oven is dried；
(5) during graphite ore is contained in polytetrafluoroethylene beaker, adding mixed acid by liquid-solid ratio 0.5 ~ 4, at 30 ~ 70 DEG C, stirring clears up 1 ~ 5 hour；Standing sedimentation, pours out supernatant, repeats this step 1 ~ 4 time；
(6) the sample ore after clearing up filters, cleans, dries, and obtains graphite powder, sieves with standard screen, measures the graphite particle size characteristics such as flaky graphite content.
The most according to claim 1, method, it is a feature of the present invention that: the most described noble gas of step, refers to the one in carbon dioxide or nitrogen.
The most according to claim 1, method, it is a feature of the present invention that: the most described hand-crushed of step, refers to manual breaking into pieces with one's fingers, and utilizes the instrument such as wooden stick, iron staff to roll by hand.
The most according to claim 1, method, it is a feature of the present invention that: the most described mixed acid of step, by Fluohydric acid.: hydrochloric acid: the proportions of nitric acid=4:3:1.
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| CN201610129246.8A CN105823712B (en) | 2016-03-08 | 2016-03-08 | A kind of method for measuring flaky graphite content in crystalline flake graphite ore deposit |
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| CN201610129246.8A CN105823712B (en) | 2016-03-08 | 2016-03-08 | A kind of method for measuring flaky graphite content in crystalline flake graphite ore deposit |
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| CN105823712B CN105823712B (en) | 2018-06-26 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107462452A (en) * | 2017-09-25 | 2017-12-12 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of method for determining crystalline flake graphite ore deposit particle size distribution characteristics |
| 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 |
| CN114634179A (en) * | 2022-03-25 | 2022-06-17 | 矿冶科技集团有限公司 | Pretreatment equipment and method before grinding of graphite ore |
Citations (5)
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| 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
Patent Citations (5)
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|---|---|---|---|---|
| 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 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN107462452A (en) * | 2017-09-25 | 2017-12-12 | 苏州中材非金属矿工业设计研究院有限公司 | A kind of method for determining crystalline flake graphite ore deposit particle size distribution characteristics |
| 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 |
| CN114634179A (en) * | 2022-03-25 | 2022-06-17 | 矿冶科技集团有限公司 | Pretreatment equipment and method before grinding of graphite ore |
| 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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| CN105823712B (en) | 2018-06-26 |
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