CN106882805A - A kind of micro crystal graphite purifies preparation technology - Google Patents
A kind of micro crystal graphite purifies preparation technology Download PDFInfo
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- CN106882805A CN106882805A CN201710293860.2A CN201710293860A CN106882805A CN 106882805 A CN106882805 A CN 106882805A CN 201710293860 A CN201710293860 A CN 201710293860A CN 106882805 A CN106882805 A CN 106882805A
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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
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Abstract
The invention discloses a kind of micro crystal graphite purification preparation technology, the natural micro crystal graphite that the granularity that weight portion is 40~50 parts is 200 mesh~3000 mesh, purity is 80%~90% is taken, addition weight portion is 30~42 parts without Ca2+、Mg2+、CL‑The pure water of foreign ion stirs into a paste, and is subsequently adding the strong acid that weight portion is 4~8 parts, 40 DEG C~100 DEG C of heating stirring reaction 4~6 hours, then by filtering, filter cake pH value is washed into neutrality, dries, and obtains native graphite of the purity more than 99.990%.The present invention purifies to 99.990%~99.998% high-purity natural graphite using liquid chemical method, can meet the high-tech area use requirement such as atomic energy industry, space technology, low cost, steady quality.
Description
Technical field
The present invention relates to the purification technique field of micro crystal graphite, more particularly to a kind of micro crystal graphite purification preparation technology.
Background technology
Graphite has very important status, such as a kind of raw material of industry in some special industries or high-tech area
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%, cannot much meet
It is that this must be purified to native graphite using the requirement of high-purity industry.
It is at present to improve graphite purity with high-temperature electric heat method to the method for purification that native graphite is taken, high-temperature electric heat method is to utilize
The resistance to elevated temperatures of graphite, is placed in closed high-temperature electric resistance furnace, and isolation air is heated to more than 2500 DEG C, makes the ash in graphite
Divide volatilization, so as to be fixed the high purity graphite of carbon more than 99.9%.Due to this complex process, it is necessary to build Large Electric Furnace,
Power consumption is also quite big, and needs are passed through inert gas constantly, thus with high costs.It is more especially needed, it is when graphite purity
When reaching 99.93%, the purification limit has been reached, it is impossible to make to fix carbon content continuation raising.
A kind of Patent No. 200910112366.7, entitled purification of microcrystalline graphite product makes new technology with purifying,
Comprise the following steps：Reached during mog is the graphite raw ore that -200 mesh percent of pass are more than 90% in fine grinding and add quick lime
Stirred with water, make the pH of the graphite ore pulp containing quick lime>9, waterglass stirring, kerosene stirring are added, it is eventually adding pine camphor
Bubble is scraped in oil stirring inflation, carries out roughing, collects 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
Ore deposit adds waterglass stirring, adds kerosene stirring, addition terpenic oil to stir and inflate and scrape bubble, carries out recleaning, collects flotation
Graphite concentrate；Above-mentioned flotation graphite concentrate adds the NaOH solution to carry out batch mixing, is calcined, is washed to neutrality, with hydrochloric acid acidleach, washing,
Dewatered drying, obtains graphite and fixes the high-carbon graphite product that carbon content reaches 98.74%；The purity of this method of purification is not reached
More than 99.90%, and operating method is excessively complicated, high cost.
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 (LC) grade 2-4 days in wet-treating, remove impurity, obtain final product 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 allows to change in proportion
Calculation uses diluted acid, can be separately added into, it is also possible to 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, high cost, and the time
It is long.
The content of the invention
A kind of low cost, steady quality are provided it is an object of the invention to overcome above-mentioned weak point of the prior art
Micro crystal graphite purification preparation technology.
The present invention is realized in the following way：
A kind of micro crystal graphite purifies preparation technology, it is characterised in that：Take granularity that weight portion is 40~50 parts for 200 mesh~
3000 mesh, purity are 80%~90% natural micro crystal graphite, and addition weight portion is 30~42 parts without Ca2+、Mg2+、CL-
The pure water of foreign ion stirs into a paste, and is subsequently adding the strong acid that weight portion is 4~8 parts, heats 40 DEG C~100 DEG C stirrings
Reaction 4~6 hours, then by filtering, filter cake pH value is washed to neutrality, dry, obtain purity natural more than 99.990%
Graphite.
The strong acid is the one kind in hydrochloric acid, phosphoric acid, sulfuric acid, hydrofluoric acid, nitric acid.
The beneficial effects of the present invention are：99.9%~99.998% high-purity natural is purified to using liquid chemical method
Graphite, can meet the high-tech area use requirement such as atomic energy industry, space technology, low cost, steady quality.
Specific embodiment
The specific embodiment of the invention is now described in detail in detail：
A kind of micro crystal graphite purifies preparation technology, and it is 200 mesh~3000 mesh, purity to take the granularity that weight portion is 40~50 parts
It is 80%~90% natural micro crystal graphite, addition weight portion is 30~42 parts without Ca2+、Mg2+, CL- foreign ions it is pure
Water stirs into a paste, and is subsequently adding the strong acid that weight portion is 4~8 parts, and 40 DEG C~100 DEG C stirring reactions 4~6 of heating are small
When, then by filtering, filter cake pH value is washed to neutrality, and dry, obtain native graphite of the purity more than 99.990%.
Strong acid of the present invention is one kind or its several mixing in hydrochloric acid, phosphoric acid, sulfuric acid, hydrofluoric acid, nitric acid.
It is that, using acid and the impurity reaction water-soluble ion of generation, dissolving removes graphite that the present invention adds the purpose of strong acid
In impurity component；The particle size range of the native graphite that this technique is directly used is big, in 3000 mesh between 200 mesh and former
Material carbon range is wide, and 80% to 99%, therefore be less than more than 98% from the oxidant of high concentration its concentration range
98% reaction is incomplete；Temperature during due to acidolysis directly influences the speed of acidolysis reaction, thus the control of its reaction temperature exists
40 DEG C~100 DEG C, less than 40 DEG C, reaction is incomplete, higher than 100 DEG C, to accelerating reaction speed DeGrain, causes energy wave
Take.The acidolysis reaction time, general control was at 4~6 hours.
It is with being crossed by ion exchange resin treatment without Ca during present invention washing2+、Mg2+, the foreign ion such as CL-
Pure water removes the soluble impurity produced after acidolysis reaction, and filter cake must be washed till neutrality, to ensure to remove through acidolysis reaction
The soluble impurity of generation.
Present invention process is simple, not strict to ingredient requirement, it is adaptable to process granularity in 3000 mesh to 200 mesh, purity
80%~90% all size raw material, and do not need special installation and material, you can a step purifies to 99.990~
9.998% high-purity natural graphite, can meet the high-tech area use requirement such as atomic energy industry, space technology, low cost,
Steady quality.
Embodiment 1
Natural micro crystal graphite miberal powder 400Kg (material purity 85%) is taken, water is added (with by ion exchange resin treatment mistake
Without Ca2+、Mg2+, the foreign ion such as CL- pure water) 300kg, stirring evenly makes it into pasty state, is subsequently adding hydrochloric acid 80kg, heating
60 DEG C of stirring reactions 5 hours, through filtering, reclaim chemical reagent 23.5kg, consume 56.5kg, and filter cake pH value is washed to neutrality, does
It is dry, obtain finished product 336kg, the rate of recovery 84%, product purity 99.995%.
Embodiment 2
Crystallite ball graphite 500kg is taken, the mesh of granularity 800 (phosphorus content 96%) adds water (using by ion exchange resin
It is treated without Ca2+、Mg2+, the foreign ion such as CL- pure water) 420kg, stirring evenly makes it into pasty state, be subsequently adding sulfuric acid and
40kg, 60 DEG C of heating stirring reaction 5 hours, by washing and filtering, reclaims chemical reagent 5.8kg, consumes 34.2kg, filter cake pH value
Neutrality is washed to, product purity 99.992% is dried to obtain, product 477.5kg, the rate of recovery 95.5% is obtained.
Claims (2)
1. a kind of micro crystal graphite purifies preparation technology, it is characterised in that：Take granularity that weight portion is 40~50 parts for 200 mesh~
3000 mesh, purity are 80%~90% natural micro crystal graphite, and addition weight portion is 30~42 parts without Ca2+、Mg2+、CL-It is miscellaneous
The pure water of matter ion stirs into a paste, and is subsequently adding the strong acid that weight portion is 4~8 parts, 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 natural stone of the purity more than 99.990%
Ink.
2. a kind of micro crystal graphite according to claim 1 purifies preparation technology, it is characterised in that：The strong acid be hydrochloric acid,
One kind in phosphoric acid, sulfuric acid, hydrofluoric acid, nitric acid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN114180569A (en) * | 2021-12-21 | 2022-03-15 | 中国科学技术大学 | Purification method of mixed-phase graphite |
| CN114212788A (en) * | 2021-11-25 | 2022-03-22 | 贝特瑞新材料集团股份有限公司 | Graphite purification process and graphite |
| 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 |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102602908A (en) * | 2012-04-09 | 2012-07-25 | 上海尚饮思生化医药有限公司 | Purification method of battery-grade graphite fluoride |
| CN104211048A (en) * | 2013-06-05 | 2014-12-17 | 中国科学院上海有机化学研究所 | Preparation method of fluorinated graphene |
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| CN102602908A (en) * | 2012-04-09 | 2012-07-25 | 上海尚饮思生化医药有限公司 | Purification method of battery-grade graphite fluoride |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| CN114212788A (en) * | 2021-11-25 | 2022-03-22 | 贝特瑞新材料集团股份有限公司 | Graphite purification process and graphite |
| WO2023093321A1 (en) * | 2021-11-25 | 2023-06-01 | 贝特瑞新材料集团股份有限公司 | Graphite purification process and graphite |
| TWI839950B (en) * | 2021-11-25 | 2024-04-21 | 大陸商貝特瑞新材料集團股份有限公司 | Graphite purification process and graphite obtained therefrom |
| CN114180569A (en) * | 2021-12-21 | 2022-03-15 | 中国科学技术大学 | Purification method of mixed-phase graphite |
| 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 |
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