CN105271216B - A kind of preparation method of high purity graphite - Google Patents
A kind of preparation method of high purity graphite Download PDFInfo
- Publication number
- CN105271216B CN105271216B CN201510891382.6A CN201510891382A CN105271216B CN 105271216 B CN105271216 B CN 105271216B CN 201510891382 A CN201510891382 A CN 201510891382A CN 105271216 B CN105271216 B CN 105271216B
- Authority
- CN
- China
- Prior art keywords
- graphite
- high purity
- purity
- passed
- purifying device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Abstract
The present invention relates to a kind of preparation method of high purity graphite, this method includes step in detail below：(1) middle carbon or high-carbon graphite are taken, is passed through first paragraph graphite purifying device, 0.5~2.0h is handled under the conditions of 1000~2000 DEG C；(2) solid product that gained is handled through step (1) is passed through second segment graphite purifying device, 0.5~1.0h is handled under the conditions of 2000~3000 DEG C, produces high purity graphite.The preparation method of high purity graphite provided by the invention can reduce the requirement that high temperature method is equipped to graphite purification, industrialized production for the industrialization promotion of high temperature method, the high purity graphite of phosphorus content more than 99.99% creates conditions, it is provided simultaneously with production efficiency height, low power consumption and other advantages, beneficial to large-scale industrial production, there is extremely strong actual promotional value.
Description
Technical field
The present invention relates to graphite chemical technology field, is more particularly to a kind of preparation method of high purity graphite.
Background technology
High purity graphite is the graphite that phosphorus content reaches more than 99.9%, and production high purity graphite mainly removes stone by purifying
Impurity in ink.Graphite production needs progressively to purify, can be by graphite ore stone flour typically using floatation as the purification by mineral first step
Middle carbon (purity is 80%~93%) and high-carbon (94%~98%) are purified to after broken.And for the new energy of lithium rechargeable battery
Source material, the manufacture of graphene, nano paint, the high grade refractory of metallurgical industry, military project stabilization agent, space flight exotic material
Etc. occasion, this purity can not meet the requirement of some occasions.
The major impurity composition contained in graphite is the silicate mineral of potassium, sodium, magnesium, iron, calcium, aluminium etc., and graphite is entered
The purification of one step is exactly to take effective means to remove this partial impurities.The method of production high purity graphite generally has chemistry both at home and abroad at present
Method (hydrogen fluoride and chlorinating roasting) and high temperature method.Hydrogen fluoride is molten using the impurity in graphite and hydrofluoric acid reaction generation
Reach the purpose of purification in fluoride and the volatile matter of water, the method is big to equipment corrosion, and strong toxicity；Chlorinating roasting
It is that the impurity in graphite is converted into by volatile matter using chlorine, chlorine has strong corrosivity and toxicity, seriously pollutes environment, and
Process system is unstable, and production cost is high, limits the popularization and application of the technique to a certain extent.High temperature method mainly utilizes stone
The boiling point of ink can produce more than 99.99% ultra-pure graphite far above the boiling point of impurities silicate this characteristic, right
Equipment performance requires high, but as domestic high-temperature service prepares horizontal gradual lifting, high temperature method is developing progressively to be most latent
The high purity graphite preparation method of power.High temperature method is mainly continued by the way that middle carbon or high-carbon graphite are placed under higher technological temperature
Heating, enables the impurity in graphite fully to volatilize to reach the purpose of purification.
However, preparing high purity graphite using high temperature method, there are problems that in actual production process it is following some：First, by
Carbon or the step of high-carbon graphite one are purified to more than 99.99% purity, it is necessary to which equipment continuous firing 5 under 2600 DEG C of high temperature above is small
When more than, higher requirement, and high energy consumption are proposed to equipment；Second, purification process produces substantial amounts of impurity volatile matter, to equipment
The contamination resistance of burner hearth requires high；Third, with the progress of purification process, impurity volatile concentrations increase and difficult in heating zone
With discharge in time completely, cause graphite purification environmental degradation, the purity of graphite is difficult to further improve.
The content of the invention
The defects of it is an object of the invention to overcome prior art, there is provided a kind of method that two-step method prepares high purity graphite.
Graphite is first passed through first paragraph graphite purifying device by method provided by the invention, is grown under lower temperature conditions
Time-triggered protocol；Second segment graphite purifying device is passed through again, and short time processing is carried out under higher temperature conditions, it is high-purity so as to obtain
Graphite.The flow of the method for the invention is referred to shown in Fig. 1.
Method provided by the invention includes step in detail below：
(1) middle carbon or high-carbon graphite are taken, is passed through first paragraph graphite purifying device, is handled under the conditions of 1000~2000 DEG C
0.5~2.0h, obtain solid product；
(2) solid product that gained is handled through step (1) is passed through second segment graphite purifying device, at 2000~3000 DEG C
Under the conditions of handle 0.5~1.0h, produce high purity graphite.
Wherein, step (1) described temperature is preferably 1600~2000 DEG C；Step (2) described temperature is preferably 2600~
3000℃。
The raw material that the method for the invention uses is medium-carbon graphite or high-carbon graphite.Wherein, the purity of the medium-carbon graphite
For 80~93%, the purity of the high-carbon graphite is 94~98%.In order to realize the reasonable development of resource and make full use of, this hair
It is bright preferably using the relatively low medium-carbon graphite of purity as raw material, prepare high purity graphite.
Graphite purifying device of the present invention is non-batch formula device, can realize the continuous feed of material to be purified, carry
The continuous discharge of material after pure, does not suffer from heating, cooling process in purification process, two section apparatus control in more constant temperature respectively
In the range of degree, to realize efficient, the energy-conservation of purification process.
Knowable to being detected in process of production, after step of the present invention (1) processing, the phosphorus content in graphite is general
It is close to 99%；After step (2) processing, phosphorus content can reach more than 99.99%.
In order to promote impurity in graphite raw material quickly, fully to volatilize, the present invention preferably enters before preparation to graphite raw material
Row grinding pretreatment.Specifically, the middle carbon or high-carbon graphite are ground to particle diameter less than 500 μm by the present invention, preferably grain
200~300 μm of footpath, so as to improve purification efficiency.
In order to promote the abundant removal of impurity, the efficiency of graphite purification is further improved, the present invention is preparing high purity graphite
During be passed through halogen gas.Specifically, the present invention is continually fed into halogen gas in step (1) or/and step (2)；
It is preferred that being passed through chlorine in step (1), step (2) can lead to can be obstructed.The halogen gas is preferably fluorine gas or chlorine, further
The preferably chlorine of purity more than 99%.Because halogen gas Nature comparison is active, the present invention control chlorine flowrate be 0.5~
10m3/ h, ensure production safety on the basis of purification efficiency is improved.On this basis, the present invention simultaneously optimization processing efficiency with
And production cost, the chlorine flowrate in preferred steps (1) is 8~10m3/ h, the chlorine flowrate in step (2) is 0.5~2m3/h。
Gas flow of the present invention refers to the gas flow being passed through in every cubic metre of purifying plant inner chamber.
As a preferred embodiment of the present invention, methods described includes step in detail below：
(1) medium-carbon graphite is taken, is ground to 200~300 μm of particle diameter, is passed through first paragraph graphite purifying device, processing 0.5~
1h, obtain solid product；
The treatment conditions of the first paragraph are：1600~2000 DEG C of temperature, with 8~10m of flow velocity3/ h is continually fed into purity
More than 99% chlorine；
(2) solid product obtained by step (1) is passed through second segment graphite purifying device, handles 0.5~0.7h, produce；
The treatment conditions of the second segment are：2600~3000 DEG C of temperature, with 0.5~2m of flow velocity3/ h is continually fed into purity
More than 99% chlorine.
In the above method, the temperature needed for step (1) is relatively low, and the processing time needed for step (2) is shorter, so as to big
The big service requirement reduced to equipment；And after most impurity is removed in step (1), it can be ensured that graphite is pure in step (2)
The environment of change is more pure, beneficial to the further efficiently purification of the graphite after step (1) purification.The present invention uses above-mentioned two step
Method, it can make specific yield high purity graphite is obvious the time required to preparing to shorten, significantly improve production efficiency, and substantially reduce power consumption
And production cost.
The present invention further protects the high purity graphite being prepared in this way.The method of the invention can obtain pure
The high purity graphite of degree more than 99.99%.
In some special industrial circles, such as atomic pile, it is desirable to which impurity content is not to be exceeded in the graphite used
Tens ppm.Therefore, graphite of the purity provided by the invention more than 99.99% has high practical value.
Compared with prior art, the preparation method of high purity graphite provided by the invention can reduce high temperature method and graphite purification is filled
Standby requirement, created conditions for the industrialization promotion of high temperature method, the industrialized production of the high purity graphite of phosphorus content more than 99.99%,
Production efficiency height, low power consumption and other advantages are provided simultaneously with, beneficial to large-scale industrial production, there is extremely strong actual promotional value.
Brief description of the drawings
Fig. 1 is the process chart of high purity graphite preparation method of the present invention.
Embodiment
Following examples are used to illustrate the present invention, but can not be used for limiting the scope of the present invention.
The first paragraph of use of the embodiment of the present invention and the interior chamber size of second segment graphite purifying device are
Graphite raw material in following embodiment is the medium-carbon graphite of phosphorus content 85~90%.
Embodiment 1
High purity graphite is prepared according to following steps：
(1) graphite is taken, is ground to 200~300 μm of particle diameter, is passed through first paragraph graphite purifying device, 0.5h is handled, obtains solid
Product；
The treatment conditions of the first paragraph are：2000 DEG C of temperature, with flow velocity 8m3/ h is continually fed into the chlorine of purity more than 99%
Gas；
(2) solid product obtained by step (1) is passed through second segment graphite purifying device, handles 0.5h, produce；
The treatment conditions of the second segment are：3000 DEG C of temperature, with flow velocity 1m3/ h is continually fed into the chlorine of purity more than 99%
Gas.
After testing, graphite phosphorus content is 99% after step (1) processing, and phosphorus content is in graphite after step (2) processing
99.99999%.
Embodiment 2
High purity graphite is prepared according to following steps：
(1) graphite is taken, is ground to 200~300 μm of particle diameter, is passed through first paragraph graphite purifying device, handles 1h, obtains solid production
Thing；
The treatment conditions of the first paragraph are：1600 DEG C of temperature, with flow velocity 8m3/ h is continually fed into the chlorine of purity more than 99%
Gas；
(2) solid product obtained by step (1) is passed through second segment graphite purifying device, handles 0.5h, produce；
The treatment conditions of the second segment are：2600 DEG C of temperature, with flow velocity 1m3/ h is continually fed into the chlorine of purity more than 99%
Gas.
After testing, graphite phosphorus content is 99% after step (1) processing, and phosphorus content is in graphite after step (2) processing
99.9999%.
Embodiment 3
High purity graphite is prepared according to following steps：
(1) graphite is taken, is ground to 200~300 μm of particle diameter, is passed through first paragraph graphite purifying device, handles 2h, obtains solid production
Thing；
The treatment conditions of the first paragraph are：1000 DEG C of temperature；
(2) solid product obtained by step (1) is passed through second segment graphite purifying device, handles 1h, produce；
The treatment conditions of the second segment are：2000 DEG C of temperature, with flow velocity 2m3/ h is continually fed into the chlorine of purity more than 99%
Gas.
After testing, graphite phosphorus content is 98% after step (1) processing, and phosphorus content is in graphite after step (2) processing
99.999%.
Embodiment 4
Compared with Example 1, differ only in：Nitrogen is passed through with identical flow in step (1) and (2)；Gained graphite
Purity be 99.99%, less than the 99.99999% of the gained of embodiment 1.
Embodiment 5
Compared with Example 1, differ only in：Step (1) and (2) are not passed through gas；Step (1) processing time is not
Become, step (2) could obtain the graphite of purity 99.99% after 1h.
Comparative example 1
High purity graphite is prepared according to following steps：Medium-carbon graphite is taken, 250 μm of particle diameter is ground to, is passed through graphite purifying device,
Persistently handled at 2600 DEG C using one-step method, after 8~10h, just obtain the high purity graphite of purity 99.99%, Er Qieji
Renew long processing time, the purity of graphite is also difficult to further improve.
From the comparative example, the method for the invention can significantly improve the production efficiency of purification graphite, purify graphite
Time greatly shortens, then reduces requirement of the purification graphite to equipment.
Embodiment of above is merely to illustrate the present invention, rather than limitation of the present invention.Although with reference to embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that, to technical scheme carry out it is various combination,
Modification or equivalent substitution, without departure from the spirit and scope of technical solution of the present invention, the right that all should cover in the present invention is wanted
Ask among scope.
Claims (1)
1. a kind of preparation method of high purity graphite, it is characterised in that comprise the following steps：
(1) medium-carbon graphite is taken, is ground to 200~300 μm of particle diameter, is passed through first paragraph graphite purifying device, handles 0.5~1h；
The treatment conditions of the first paragraph are：1600~2000 DEG C of temperature, with 8~10m of flow velocity3/ h be continually fed into purity 99% with
On chlorine；
(2) solid product obtained by step (1) is passed through second segment graphite purifying device, handles 0.5~0.7h, produce；
The treatment conditions of the second segment are：2600~3000 DEG C of temperature, with 0.5~2m of flow velocity3/ h be continually fed into purity 99% with
On chlorine；
The graphite purifying device is non-batch formula device, can realize material to be purified continuous feed, purification after material company
It is continuous to discharge, heating, cooling process is not suffered from purification process, two section apparatus are controlled in the range of stationary temperature respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510891382.6A CN105271216B (en) | 2015-12-07 | 2015-12-07 | A kind of preparation method of high purity graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510891382.6A CN105271216B (en) | 2015-12-07 | 2015-12-07 | A kind of preparation method of high purity graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105271216A CN105271216A (en) | 2016-01-27 |
| CN105271216B true CN105271216B (en) | 2018-01-02 |
Family
ID=55141157
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510891382.6A Active CN105271216B (en) | 2015-12-07 | 2015-12-07 | A kind of preparation method of high purity graphite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105271216B (en) |
Families Citing this family (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106219526B (en) * | 2016-07-19 | 2018-11-27 | 福建翔丰华新能源材料有限公司 | A kind of method of purification of micro crystal graphite |
| CN106348288B (en) * | 2016-08-18 | 2019-04-23 | 中南钻石有限公司 | A kind of purification process technique of compound probability diamond graphite stem |
| CN108516544A (en) * | 2018-06-01 | 2018-09-11 | 中钢集团新型材料（浙江）有限公司 | It is electrolysed HF and KHF2Generate the method and system of fluorine gas purification graphite |
| CN108516543A (en) * | 2018-06-01 | 2018-09-11 | 中钢集团新型材料（浙江）有限公司 | Potassium hexafluoromanganate and the antimony pentafluoride method that heat production fluorine gas purifies graphite altogether |
| CN109867281A (en) * | 2019-04-10 | 2019-06-11 | 哈尔滨理工大学 | A kind of preparation method of high purity graphite |
| CN110482542A (en) * | 2019-04-10 | 2019-11-22 | 哈尔滨理工大学 | A kind of preparation method of high purity graphite heater |
| CN111017922B (en) * | 2020-01-09 | 2022-04-12 | 成都理工大学 | Activation method of natural crystalline graphite fine powder for preparing high-purity graphite |
| CN111792641A (en) * | 2020-07-20 | 2020-10-20 | 哈尔滨理工大学 | Graphite purification method |
| CN112411173A (en) * | 2020-11-18 | 2021-02-26 | 湖南顶立科技有限公司 | Preparation method of high-purity carbon fiber hard felt |
| CN114990689B (en) * | 2022-04-28 | 2024-03-22 | 中电化合物半导体有限公司 | Synthesis method and application of silicon carbide powder |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5505929A (en) * | 1986-09-22 | 1996-04-09 | Toyo Tanso Co., Ltd. | Method for manufacturing high purity graphite material and manufacturing apparatus for use thereof |
| CN101357761A (en) * | 2008-09-09 | 2009-02-04 | 河南天利碳素材料有限公司 | High pure graphitic profile and preparation technique thereof |
| CN102745681A (en) * | 2012-07-19 | 2012-10-24 | 武汉工程大学 | Method and device for purifying graphite |
| CN102923699A (en) * | 2012-11-26 | 2013-02-13 | 鹤岗市赛欧新材料有限责任公司 | Continuous pyrographite purifying device |
| CN104386670A (en) * | 2014-04-23 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Isostatic-pressure high-purity graphite material and preparation method thereof |
-
2015
- 2015-12-07 CN CN201510891382.6A patent/CN105271216B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5505929A (en) * | 1986-09-22 | 1996-04-09 | Toyo Tanso Co., Ltd. | Method for manufacturing high purity graphite material and manufacturing apparatus for use thereof |
| CN101357761A (en) * | 2008-09-09 | 2009-02-04 | 河南天利碳素材料有限公司 | High pure graphitic profile and preparation technique thereof |
| CN102745681A (en) * | 2012-07-19 | 2012-10-24 | 武汉工程大学 | Method and device for purifying graphite |
| CN102923699A (en) * | 2012-11-26 | 2013-02-13 | 鹤岗市赛欧新材料有限责任公司 | Continuous pyrographite purifying device |
| CN104386670A (en) * | 2014-04-23 | 2015-03-04 | 天津锦美碳材科技发展有限公司 | Isostatic-pressure high-purity graphite material and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| 攀枝花细鳞片石墨制备高纯石墨的几种方法比较;赖奇等;《攀枝花学院学报》;20070630;第24卷(第3期);第10-14页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105271216A (en) | 2016-01-27 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105271216B (en) | A kind of preparation method of high purity graphite | |
| CN101665253B (en) | Polysilicon purification method and crucible and purification device used for polysilicon purification | |
| CN105347337B (en) | A kind of method of use freon high temperature purification native graphite | |
| CN109867281A (en) | A kind of preparation method of high purity graphite | |
| CN105460923B (en) | A kind of continuous preparation method of high-purity fluorographite | |
| RU2451635C2 (en) | Method of producing highly pure elementary silicon | |
| CN108069422A (en) | A kind of method of graphite purification | |
| CN101362600A (en) | Method for removing boron from polysilicon by wet metallargy | |
| CN113651341A (en) | Method for synthesizing lithium hexafluorophosphate solution by using fluorine-containing waste residues | |
| CN103882245A (en) | Magnesium refining method and titanium sponge preparation method | |
| CN105347338B (en) | A kind of method of use light metal halogen high temperature purification native graphite | |
| CN102275904A (en) | Method of preparing high-purity graphite by using chemical liquid-phase method | |
| CN100575843C (en) | Polycrystalline silicon reducing furnace water-cooling double glass viewing mirror | |
| CN104016334A (en) | Purification method for graphite | |
| CN108675293A (en) | A kind of graphite high temperature purification device | |
| CN203768482U (en) | Novel vacuum electron beam smelting furnace | |
| WO2009005412A2 (en) | Method for producing polycrystalline silicon | |
| CN111362263A (en) | Preparation method of high-purity graphite material | |
| CN102795629B (en) | Method for purification of dichlorosilane from dry method recovered material | |
| CN101775650A (en) | Preparation method of solar polycrystalline silicon cast ingot and device thereof | |
| CN108793170B (en) | Industrial silicon acid pickling process after ventilation, slagging, smelting and pretreatment | |
| CN103072995A (en) | Method for removing phosphorus in polycrystalline silicon | |
| CN105948002A (en) | Production process for recovering waste acid for preparing nitrosyl sulfuric acid | |
| JP2015137183A (en) | Method of producing lithium sulfide | |
| CN102862989A (en) | Pretreatment method for purifying polycrystalline silicon by metallurgic method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 410118 Hunan Dingli Technology Co., Ltd., east of Lantian North Road, north of liangtang East Road and west of Shuangtang Road, Xingsha industrial base, Changsha Economic and Technological Development Zone, Changsha City, Hunan Province Patentee after: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. Address before: 410118 Hunan province Changsha Muyun town Muyun Industrial Park Patentee before: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. |
|
| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 410199 No. 1271, liangtang East Road, Xingsha industrial base (Changlong Street), Changsha area, China (Hunan) pilot Free Trade Zone, Changsha, Hunan Province Patentee after: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. Address before: 410118 Hunan Dingli Technology Co., Ltd., east of Lantian North Road, north of liangtang East Road and west of Shuangtang Road, Xingsha industrial base, Changsha Economic and Technological Development Zone, Changsha City, Hunan Province Patentee before: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 410199 No. 1271, liangtang East Road, Xingsha industrial base (Changlong Street), Changsha area, China (Hunan) pilot Free Trade Zone, Changsha, Hunan Province Patentee after: Hunan Dingli Technology Co.,Ltd. Address before: 410199 No. 1271, liangtang East Road, Xingsha industrial base (Changlong Street), Changsha area, China (Hunan) pilot Free Trade Zone, Changsha, Hunan Province Patentee before: ADVANCED CORPORATION FOR MATERIALS & EQUIPMENTS Co.,Ltd. |