CN106966389A - A kind of method of purification of micro crystal graphite - Google Patents
A kind of method of purification of micro crystal graphite Download PDFInfo
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- CN106966389A CN106966389A CN201710294958.XA CN201710294958A CN106966389A CN 106966389 A CN106966389 A CN 106966389A CN 201710294958 A CN201710294958 A CN 201710294958A CN 106966389 A CN106966389 A CN 106966389A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a kind of method of purification of micro crystal graphite, the granularity for taking parts by weight to be 1~5 part is the natural micro crystal graphite that more than 5000, purity is 80%~90%, adds parts by weight for 3~15 parts without Ca2+、Mg2+、CL‑The pure water of foreign ion stirs into a paste, and then adds the mixed acid that parts by weight are 2~10 parts, ultrasound 20~50 minutes, 40 DEG C~100 DEG C of heating stirring reaction 4~6 hours, then by filtering, filter cake pH value is washed to neutrality, dry, obtain the native graphite that purity is more than 99.90%.The present invention combines ultrasonically treated purification micro crystal graphite using hydrofluoric acid/hydrochloric acid method, and the fixation carbon content of purifying micro crystal graphite has reached 99.97%, the economic value to improving micro crystal graphite, and expanding it has certain practical significance in the application of high-tech area.
Description
Technical field
The present invention relates to the purification technique field of micro crystal graphite, more particularly to a kind of method of purification of micro crystal graphite.
Background technology
Graphite has very important status in some special industries or high-tech area, such as a kind of raw material of industry
The industry such as atomic energy industry, auto industry, space technology, biotechnology.The graphite that these industries are used its phosphorus content must be
More than 99.9% high purity graphite, and the phosphorus content of the native graphite after general ore dressing is up to 96%, can not much meet
It is that this must be purified to native graphite using the requirement of high-purity industry.
Ash content is more, impurity hardly possible separation be restrict micro crystal graphite high-technology field apply and develop key factor it
One.In recent years, the purification research of micro crystal graphite is gradually goed deep into, mainly including floatation, alkali acid system, hydrogen fluoride and different removal of impurities
The combination of method.The effect of floatation purification micro crystal graphite is limited, and the complicated technological process of alkali acid system and huge alkali, acid are used
Amount causes purification efficiency low, and secondary pollution is serious.
A kind of Patent No. 200910112366.7, entitled purification of microcrystalline graphite product makes new technology with purifying,
Comprise the following steps：Reach that mog is to add quick lime in the graphite raw ore that -200 mesh percent of pass are more than 90% in fine grinding
Stirred with water, make the pH of the graphite ore pulp containing quick lime>9, waterglass stirring, kerosene stirring are added, pine camphor is eventually adding
Bubble is scraped in oil stirring inflation, is carried out roughing, is collected graphite rougher concentration and mine tailing；The concentrate addition waterglass stirring of roughing acquisition,
Add kerosene stirring, addition terpenic oil to stir and inflate and scrape bubble, carry out primary cleaning, collect selected concentrate；The essence of primary cleaning
The stirring of ore deposit addition waterglass, the stirring of addition kerosene, addition terpenic oil are stirred and inflated and scrape bubble, and progress recleaning collects flotation
Graphite concentrate；Above-mentioned flotation graphite concentrate adds NaOH solution to carry out batch mixing, is calcined, is washed to neutrality, with hydrochloric acid acidleach, washes,
Dewatered drying, obtains graphite and fixes the high-carbon graphite product that carbon content reaches 98.74%；The purity of this method of purification does not reach
More than 99.90%, and operating method is excessively complicated, cost is high.
Patent No. CN90109672.5, a kind of entitled method for purifying high-carbon graphite, during application (patent right) is artificial
Xi'an optical precision optical machinery research institute of the academy of sciences of state, its technical scheme is：Using by hydrochloric acid, nitric acid (or sulfuric acid) and hydrofluoric acid group
Into mixed acid agent, under normal temperature (0 DEG C -65 DEG C), the raw material of low-carbon grade 2-4 days in wet-treating, remove impurity, produce and carry
Pure high-carbon graphite, the composition and its consumption of its mixed acid agent be according to the ore body composition of graphite raw material and the composition of ash content and its
Content difference and prepare, based on every hectogram graphite raw material, the excursion of each composition usage amount of mixed acid agent is：Concentrated hydrochloric acid
15-60ml, concentrated nitric acid (or concentrated sulfuric acid) 0-30ml, hydrofluoric acid (40%) 15-60ml above-mentioned various sour agent allow to change in proportion
Calculation uses diluted acid, can be separately added into, and can also be added with mixed acid, and water (or spent acid mother liquor) can then make as supplement
Obtain solution and flood graphite raw material, somewhat excessive to be advisable, daily stirring is for several times.This operating method is excessively complicated, and cost is high, and the time
It is long.
The content of the invention
There is provided that a kind of cost is low, steady quality it is an object of the invention to overcome above-mentioned weak point of the prior art
Micro crystal graphite method of purification.
The present invention is realized in the following way：
A kind of method of purification of micro crystal graphite, it is characterised in that：The granularity for taking parts by weight to be 1~5 part is more than 5000, pure
The natural micro crystal graphite for 80%~90% is spent, parts by weight are added for 3~15 parts without Ca2+、Mg2+, CL- foreign ions
Pure water stirs into a paste, and then adds the mixed acid that parts by weight are 2~10 parts, ultrasonic 20~50 minutes, and 40 DEG C of heating~
100 DEG C of stirring reactions 4~6 hours, then by filtering, filter cake pH value is washed to neutrality, dry, obtain purity and be more than
99.90% native graphite.
Preferably, the mixed acid is by 1 by hydrofluoric acid and hydrochloric acid：1 ratio is mixed.
The beneficial effects of the present invention are：Ultrasonically treated purification micro crystal graphite is combined using hydrofluoric acid/hydrochloric acid method, purified micro-
The fixation carbon content of spar ink has reached 99.97%, the economic value to improving micro crystal graphite, expands it in high-tech area
Using with certain practical significance.
Embodiment
The specific embodiment of the invention is now described in detail：
A kind of method of purification of micro crystal graphite, the granularity for taking parts by weight to be 1~5 part be more than 5000, purity be 80%~
90% natural micro crystal graphite, adds parts by weight for 3~15 parts without Ca2+、Mg2+, CL- foreign ions pure water stirring it is equal
Even then to add the mixed acid that parts by weight are 2~10 parts into pasty state, ultrasound 20~50 minutes heats 40 DEG C~100 DEG C stirrings anti-
Answer 4~6 hours, then by filtering, filter cake pH value is washed to neutrality, dry, obtain the natural stone that purity is more than 99.90%
Ink.
Mixed acid of the present invention is by 1 by hydrofluoric acid and hydrochloric acid：1 ratio is mixed.
Embodiment 1
Take natural micro crystal graphite miberal powder 50Kg, (material purity 82%) adds pure water 150kg, stirring evenly makes it into pasty state, so
Mixed acid 100kg is added afterwards, and ultrasound 30 minutes, 60 DEG C of heating stirring reaction 5 hours, through filtering, washes filter cake pH value to neutrality,
Dry, obtain finished product 36kg, the rate of recovery 88%, product purity 99.93%.
Embodiment 2
Take natural micro crystal graphite miberal powder 50Kg, (material purity 87%) adds pure water 150kg, stirring evenly makes it into pasty state, so
Mixed acid 90kg is added afterwards, and ultrasound 40 minutes, 60 DEG C of heating stirring reaction 5 hours, through filtering, washes filter cake pH value to neutrality,
Dry, obtain finished product 39kg, the rate of recovery 89.7%, product purity 99.97%.
Claims (2)
1. a kind of method of purification of micro crystal graphite, it is characterised in that：The granularity for taking parts by weight to be 1~5 part is more than 5000, purity
For 80%~90% natural micro crystal graphite, parts by weight are added for 3~15 parts without Ca2+、Mg2+、CL-The pure water of foreign ion
Stir into a paste, then add the mixed acid that parts by weight are 2~10 parts, ultrasound 20~50 minutes heats 40 DEG C~100 DEG C
Stirring reaction 4~6 hours, then by filtering, filter cake pH value is washed to neutrality, dry, obtain the day that purity is more than 99.90%
Right graphite.
2. a kind of method of purification of micro crystal graphite according to claim 1, it is characterised in that：The mixed acid is by hydrogen fluorine
Acid and hydrochloric acid press 1：1 ratio is mixed.
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107539982A (en) * | 2017-10-31 | 2018-01-05 | 湖南国盛石墨科技有限公司 | A kind of high-purity micro crystal graphite production system and its production technology |
| CN107555428A (en) * | 2017-10-31 | 2018-01-09 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite |
| CN107673347A (en) * | 2017-10-31 | 2018-02-09 | 湖南国盛石墨科技有限公司 | A kind of preparation method of spherical micro crystal graphite |
| CN107799770A (en) * | 2017-10-31 | 2018-03-13 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite for lithium cell cathode material and preparation method thereof |
| CN107895657A (en) * | 2017-12-23 | 2018-04-10 | 株洲市智汇知识产权运营服务有限责任公司 | A kind of preparation method of lithium-ion capacitor using spherical microcrystalline graphite material |
| CN107959028A (en) * | 2017-12-23 | 2018-04-24 | 株洲市智汇知识产权运营服务有限责任公司 | A kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material |
| CN108091495A (en) * | 2017-12-23 | 2018-05-29 | 林荣铨 | A kind of carbon nanotubes/application of the Lauxite carbon coating spherical shape micro crystal graphite as lithium-ion capacitor negative material |
| CN108155022A (en) * | 2017-12-23 | 2018-06-12 | 林荣铨 | Use the preparation method of the lithium-ion capacitor of carbon nanotube/Lauxite carbon coating spherical shape microcrystalline graphite material |
| CN108538608A (en) * | 2017-12-23 | 2018-09-14 | 林荣铨 | A kind of application of the spherical shape micro crystal graphite as lithium-ion capacitor negative material |
| CN109607527A (en) * | 2017-12-05 | 2019-04-12 | 湖南有色金属研究院 | A kind of purification by mineral method of low-grade micro crystal graphite |
| CN110217787A (en) * | 2019-05-27 | 2019-09-10 | 内蒙古瑞盛新能源有限公司 | A method of micro crystal graphite is purified using industrial waste acid |
| CN110745820A (en) * | 2019-12-04 | 2020-02-04 | 辽宁工程技术大学 | Purification method of smokeless coal-based microcrystalline graphite for preparing lithium ion battery negative electrode material |
| CN113149001A (en) * | 2021-03-05 | 2021-07-23 | 大同氢都驰拓新能源有限公司 | Automatic high-yield method for preparing and purifying spherical graphite |
| CN114180568A (en) * | 2021-12-22 | 2022-03-15 | 湖南宸宇富基新能源科技有限公司 | Pretreated microcrystalline graphite, negative electrode active material, and preparation and application thereof |
| CN115425225A (en) * | 2022-08-31 | 2022-12-02 | 广东凯金新能源科技股份有限公司 | Purification method of microcrystalline graphite negative electrode material for lithium ion battery |
| CN115716645A (en) * | 2022-12-09 | 2023-02-28 | 武汉理工大学 | Purification method of spherical graphite mixed acid leaching-ultrasonic water washing |
| CN116902975A (en) * | 2023-09-12 | 2023-10-20 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
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Cited By (20)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107555428A (en) * | 2017-10-31 | 2018-01-09 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite secondary pickling method of purification and its high-purity micro crystal graphite |
| CN107673347A (en) * | 2017-10-31 | 2018-02-09 | 湖南国盛石墨科技有限公司 | A kind of preparation method of spherical micro crystal graphite |
| CN107799770A (en) * | 2017-10-31 | 2018-03-13 | 湖南国盛石墨科技有限公司 | A kind of micro crystal graphite for lithium cell cathode material and preparation method thereof |
| CN107539982A (en) * | 2017-10-31 | 2018-01-05 | 湖南国盛石墨科技有限公司 | A kind of high-purity micro crystal graphite production system and its production technology |
| CN109607527A (en) * | 2017-12-05 | 2019-04-12 | 湖南有色金属研究院 | A kind of purification by mineral method of low-grade micro crystal graphite |
| CN109607527B (en) * | 2017-12-05 | 2022-01-28 | 湖南有色金属研究院 | Beneficiation and purification method of low-grade microcrystalline graphite |
| CN108155022B (en) * | 2017-12-23 | 2020-04-03 | 林荣铨 | Preparation method of lithium ion capacitor using microcrystalline graphite material |
| CN107895657A (en) * | 2017-12-23 | 2018-04-10 | 株洲市智汇知识产权运营服务有限责任公司 | A kind of preparation method of lithium-ion capacitor using spherical microcrystalline graphite material |
| CN107959028A (en) * | 2017-12-23 | 2018-04-24 | 株洲市智汇知识产权运营服务有限责任公司 | A kind of carbon nanotubes/application of the spherical micro crystal graphite of Lauxite carbon coating as lithium ion battery negative material |
| CN108091495A (en) * | 2017-12-23 | 2018-05-29 | 林荣铨 | A kind of carbon nanotubes/application of the Lauxite carbon coating spherical shape micro crystal graphite as lithium-ion capacitor negative material |
| CN108155022A (en) * | 2017-12-23 | 2018-06-12 | 林荣铨 | Use the preparation method of the lithium-ion capacitor of carbon nanotube/Lauxite carbon coating spherical shape microcrystalline graphite material |
| CN108538608A (en) * | 2017-12-23 | 2018-09-14 | 林荣铨 | A kind of application of the spherical shape micro crystal graphite as lithium-ion capacitor negative material |
| CN110217787A (en) * | 2019-05-27 | 2019-09-10 | 内蒙古瑞盛新能源有限公司 | A method of micro crystal graphite is purified using industrial waste acid |
| CN110745820A (en) * | 2019-12-04 | 2020-02-04 | 辽宁工程技术大学 | Purification method of smokeless coal-based microcrystalline graphite for preparing lithium ion battery negative electrode material |
| CN113149001A (en) * | 2021-03-05 | 2021-07-23 | 大同氢都驰拓新能源有限公司 | Automatic high-yield method for preparing and purifying spherical graphite |
| CN114180568A (en) * | 2021-12-22 | 2022-03-15 | 湖南宸宇富基新能源科技有限公司 | Pretreated microcrystalline graphite, negative electrode active material, and preparation and application thereof |
| CN115425225A (en) * | 2022-08-31 | 2022-12-02 | 广东凯金新能源科技股份有限公司 | Purification method of microcrystalline graphite negative electrode material for lithium ion battery |
| CN115716645A (en) * | 2022-12-09 | 2023-02-28 | 武汉理工大学 | Purification method of spherical graphite mixed acid leaching-ultrasonic water washing |
| CN116902975A (en) * | 2023-09-12 | 2023-10-20 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
| CN116902975B (en) * | 2023-09-12 | 2024-03-12 | 深圳市贝特瑞新能源技术研究院有限公司 | Self-assembled microcrystalline graphite anode material and preparation method and application thereof |
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Application publication date: 20170721 |