CN113447405A - Microcrystalline graphite particle size testing method - Google Patents
Microcrystalline graphite particle size testing method Download PDFInfo
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- CN113447405A CN113447405A CN202010220833.4A CN202010220833A CN113447405A CN 113447405 A CN113447405 A CN 113447405A CN 202010220833 A CN202010220833 A CN 202010220833A CN 113447405 A CN113447405 A CN 113447405A
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- Prior art keywords
- sample
- graphite
- microcrystalline graphite
- particle size
- testing
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 36
- 239000010439 graphite Substances 0.000 title claims abstract description 36
- 239000002245 particle Substances 0.000 title claims abstract description 23
- 238000012360 testing method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000002203 pretreatment Methods 0.000 claims abstract description 10
- 238000005464 sample preparation method Methods 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000011259 mixed solution Substances 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 239000012153 distilled water Substances 0.000 claims description 6
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 5
- 239000011707 mineral Substances 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 3
- 239000002270 dispersing agent Substances 0.000 claims 1
- 230000010355 oscillation Effects 0.000 claims 1
- 239000002002 slurry Substances 0.000 claims 1
- 238000003475 lamination Methods 0.000 abstract 1
- 238000000053 physical method Methods 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 abstract 1
- 239000013078 crystal Substances 0.000 description 7
- 239000000725 suspension Substances 0.000 description 5
- 239000003599 detergent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000002425 crystallisation Methods 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000010687 lubricating oil Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000005060 rubber Substances 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 235000012211 aluminium silicate Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 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
- 239000002932 luster Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 239000010445 mica Substances 0.000 description 1
- 229910052618 mica group Inorganic materials 0.000 description 1
- 239000013081 microcrystal Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Classifications
-
- 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
- G01N15/0205—Investigating particle size or size distribution by optical means
-
- 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
- G01N1/38—Diluting, dispersing or mixing samples
Landscapes
- 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)
- Dispersion Chemistry (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a method for testing the grain size of microcrystalline graphite, which mainly comprises a sample preparation method (1), a sample pretreatment method (2) and a sample testing method (3), wherein after the sample preparation and the sample pretreatment, the grain size and the distribution of the microcrystalline graphite are tested by adopting a laser principle; the method adopts a pretreatment method, disperses the particles stacked by the microcrystalline graphite lamination by a physical method, and tests the particle size, thereby ensuring the accuracy and reliability of data.
Description
Technical Field
The present invention relates to polymer material, inorganic mineral material, industrial graphite product, lubricating oil and metallurgy, such as rubber, plastic, fiber, etc.
Background
Graphite is a natural non-metallic mineral, belongs to strategic materials, consists of carbon elements, has wide application and unique performance, and is called as black gold.
The grade of the microcrystalline graphite can reach 60-90%, and the microcrystalline graphite ore is in a lead gray and gray black structure and has a cryptocrystalline structure. The graphite has low hardness of only 1-2, has metallic luster and greasy feeling, is characterized by soil-like surface, generally has the crystal diameter of less than 1 mu m, and can only see crystal form under an electron microscope, so the graphite is also called microcrystalline graphite, soil-like graphite, graphite-like, amorphous graphite and the like.
The microcrystalline graphite is a deep metamorphic product of coal and is a compact aggregate formed by tiny natural graphite crystals; natural pure graphite is very little, and quartz, mica, kaolin, pyrite and other minerals are often contained in the natural pure graphite. The microcrystalline graphite has different crystallization degrees and different maturity of a crystal structure, has complete crystallization, has a crystal defect and a semi-graphite structure, is a mixture of cryptocrystal, microcrystal, fine crystal and scaly crystal, is an aggregate of the microcrystalline graphite, and has a stacking cassette type aggregate in an existing state.
Disclosure of Invention
The technical scheme is as follows: in order to improve the problems and test the accurate and reliable particle size and particle size distribution, the invention discloses a method for testing the particle size of microcrystalline graphite, which mainly comprises a water-based mixed solution (1), a sample preparation method (2), a sample pretreatment method (3) and a sample test method (4).
The water-based mixed liquid (1) is a mixture of distilled water and a surfactant, and has the functions of dispersing graphite particles and eliminating charges.
The sample preparation method (2) is a vertical stirring mill with precise rotating speed, microcrystalline ore pulp with the concentration of 1-30% is prepared, the physical accumulation among microcrystalline graphite and the occurrence state of a clamping mode can be broken up through stirring, the minimum unit particles are dissociated in an aqueous mixed solution to prepare uniform suspension, and the uniform suspension is soaked for 4-48 hours for standby.
The sample pretreatment method (3) is to continuously stir the infiltrated microcrystalline graphite ore pulp for 10-60min at the rotating speed of 200-600r/h to prepare a uniform suspension sample.
According to the sample testing method (4), the reflection light intensity of the microcrystalline graphite is tested by rotating the suspension sample by 360 degrees under the laser beam, and the particle size and the distribution thereof are obtained by testing and calculating the quantity.
Has the advantages that:
according to the method, the occurrence state of microcrystalline graphite accumulation in a card room mode is eliminated through a sample preparation and pretreatment method, charges and physical stacking force are eliminated in a water-based mixed liquid mode, a uniform suspension is prepared, the particle size and distribution are tested by adopting a laser beam reflection principle, and the particle size of the occurrence state of graphite can be truly reflected.
Detailed Description
Example 1: the invention relates to a method for testing the grain size of microcrystalline graphite, which mainly comprises a water-based mixed solution (1), a sample preparation method (2), a sample pretreatment method (3) and a sample testing method (4).
The water-based mixed solution (1) is a 5% mixed solution of detergent and distilled water, and is prepared into a uniform aqueous solution at normal temperature by adopting stirring equipment; the sample preparation method (2) is that 10 percent microcrystalline graphite pulp is prepared from detergent distilled water by a precision mixer at the rotating speed of 300r/h, and is uniformly mixed, kept stand and soaked for 24 h; the sample pretreatment method (3) is that the ore pulp which is kept standing and soaked for 24 hours is continuously and uniformly mixed in a precision mixer for 30 minutes at the rotating speed of 300r/h, and is vibrated for 20 minutes by ultrasonic waves to prepare a sample; the sample testing method (4) is to load the sample into a 360 laser generator, test the reflection intensity and quantity of the light beam, and calculate the particle size and distribution by a computer.
Example 2: the water-based mixed solution (1) is 8 percent of amphoteric active agent distilled water mixed solution, and is prepared into uniform aqueous solution by adopting stirring equipment at normal temperature; the sample preparation method (2) is that a precise mixer is adopted at a rotating speed of 200r/h, 7% microcrystalline graphite pulp is prepared from detergent distilled water, and the pulp is uniformly mixed, kept stand and soaked for 48 h; the sample pretreatment method (3) is that the ore pulp which is kept standing and soaked for 48 hours is continuously and uniformly mixed in a precision mixer for 20 minutes at the rotating speed of 200r/h, and is vibrated for 10 minutes under ultrasonic wave to prepare a sample; the sample testing method (4) is to load the sample into a 360 laser generator, test the reflection intensity and quantity of the light beam, and calculate the particle size and distribution by a computer.
Through tests, the laser particle size and distribution data of the pretreated microcrystalline graphite are consistent with the particle size distribution under the electron microscope which is measured at the same time; the test cost and the reliability are greatly improved, and the grain size test level and the reliability of the microcrystalline graphite are effectively improved and promoted.
The above examples do not represent only these two ways, and the skilled person can adjust the particle size of the microcrystalline graphite according to the approximate situation and variation of the particle size to meet the test requirements of different particle size ranges and realize reliable measurement. Therefore, the method for testing the particle size of the microcrystalline graphite covers the processing industry of nonmetallic mineral materials, lubricating oil users, rubber plastic users and the like.
Claims (5)
1. A method for testing the grain size of microcrystalline graphite is characterized by comprising the following steps: the test method mainly comprises a water-based mixed solution (1), a sample preparation method (2), a sample pretreatment method (3) and a sample test method (4).
2. The method as claimed in claim 1, wherein the water-based mixed solution (1) is a mixed solution of distilled water containing 0.1-15% of a graphite dispersing agent.
3. The method as claimed in claim 1, wherein the sample preparation method (2) is to fully stir and disperse the water-based mixed solution in the stirring device at a rotation speed of 600r/h and a concentration of 1% -30% of ore pulp for 10-60min at a rotation speed of 100-.
4. The method as claimed in claim 1, wherein the sample pretreatment method (3) comprises fully stirring and dispersing the soaked mineral slurry in a stirring device at a rotation speed of 200-600r/h for 10-60min, and continuing to use ultrasonic oscillation for 3-20 min.
5. The method according to claim 1, wherein in the sample testing method (4), the laser beam is used for testing the intensity of the scattered light of the microcrystalline graphite in 360 degrees, so as to obtain the number of particles with different particle sizes and obtain the particle sizes and the distribution thereof.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010220833.4A CN113447405A (en) | 2020-03-26 | 2020-03-26 | Microcrystalline graphite particle size testing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010220833.4A CN113447405A (en) | 2020-03-26 | 2020-03-26 | Microcrystalline graphite particle size testing method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113447405A true CN113447405A (en) | 2021-09-28 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010220833.4A Pending CN113447405A (en) | 2020-03-26 | 2020-03-26 | Microcrystalline graphite particle size testing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113447405A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09215276A (en) * | 1996-01-31 | 1997-08-15 | Nippon Carbon Co Ltd | Rotating apparatus graphite brush for motor vehicle |
| CN103983548A (en) * | 2014-05-30 | 2014-08-13 | 浙江天能电池(江苏)有限公司 | Method for testing particle size of acetylene black for lead storage battery |
| CN104843680A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for batch preparation of graphene from microcrystalline graphite |
| CN105060281A (en) * | 2015-07-22 | 2015-11-18 | 深圳市贝特瑞新能源材料股份有限公司 | Nano-graphite slurry preparation method |
| CN106940284A (en) * | 2017-05-24 | 2017-07-11 | 张建平 | A kind of dispersability of titanium dioxide detection method |
| 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 |
| CN110895234A (en) * | 2018-12-29 | 2020-03-20 | 江苏天奈科技股份有限公司 | Detection method of graphene composite slurry |
-
2020
- 2020-03-26 CN CN202010220833.4A patent/CN113447405A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09215276A (en) * | 1996-01-31 | 1997-08-15 | Nippon Carbon Co Ltd | Rotating apparatus graphite brush for motor vehicle |
| CN103983548A (en) * | 2014-05-30 | 2014-08-13 | 浙江天能电池(江苏)有限公司 | Method for testing particle size of acetylene black for lead storage battery |
| CN104843680A (en) * | 2015-04-03 | 2015-08-19 | 北京理工大学 | Method for batch preparation of graphene from microcrystalline graphite |
| CN105060281A (en) * | 2015-07-22 | 2015-11-18 | 深圳市贝特瑞新能源材料股份有限公司 | Nano-graphite slurry preparation method |
| CN106940284A (en) * | 2017-05-24 | 2017-07-11 | 张建平 | A kind of dispersability of titanium dioxide detection method |
| 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 |
| CN110895234A (en) * | 2018-12-29 | 2020-03-20 | 江苏天奈科技股份有限公司 | Detection method of graphene composite slurry |
Non-Patent Citations (3)
| Title |
|---|
| 段佳琪 等: "超声-混酸法提纯微晶石墨", 《非金属矿》 * |
| 王承二 等: "乳化煤油粒度对隐晶质石墨浮选效果的影响", 《非金属矿》 * |
| 金明国: "基于高剪切选择性絮凝调浆的隐晶质石墨浮选研究", 《中国优秀博硕士学位论文全文数据库(硕士)工程科技Ⅰ辑》 * |
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| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20210928 |
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