CN109867281A - A kind of preparation method of high purity graphite - Google Patents
A kind of preparation method of high purity graphite Download PDFInfo
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- CN109867281A CN109867281A CN201910282652.1A CN201910282652A CN109867281A CN 109867281 A CN109867281 A CN 109867281A CN 201910282652 A CN201910282652 A CN 201910282652A CN 109867281 A CN109867281 A CN 109867281A
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Abstract
A kind of high purity graphite material preparation method, is related to a kind of preparation method of high purity graphite, and the purpose of the present invention is to solve some problems present in existing high purity graphite material preparation process.This method is put into self-control graphite purification device, is warming up to 1000 DEG C under nitrogen protection comprising the following specific steps (1) takes raw graphite, is loaded into a certain amount of halogen mixed gas by nitrogen under the conditions of 1000-1800 DEG C and is handled 0.5-2.0h；(2) resulting solid product is continuously heating to 2300 DEG C after step (1) processing, is passed through a certain amount of gas treatment 1-2.0h under the conditions of 2000-2300 DEG C to get high purity graphite.The preparation method of high purity graphite provided by the invention can reduce requirement of the high temperature method to graphite purification temperature, industrialized production for 99.99% or more high purity graphite of phosphorus content creates conditions, it is lower to be provided simultaneously with overall cost, it is suitable for industrialized production and industrialization promotion, and the method for the present invention preparation process is simple, energy consumption is lower, environmental protection pressure is small, has good actual promotional value.
Description
Technical field
The invention belongs to graphite material purification technique fields, and in particular to a kind of preparation method of high purity graphite material.
Background technique
Graphite has the characteristics such as good conductive, thermally conductive, self-lubricating, anticorrosive, high-low temperature resistant, occupies in national economy
Critical role, after graphite material is purified, the graphite that phosphorus content reaches 99.9% or more is referred to as high purity graphite, the purity of graphite
Higher, the value of application is bigger, for example, in fuel cell, high-temperature nuclear energy reactor, semiconductor monocrystal furnace, silica fibre wire drawing
The applications such as furnace, aerospace vehicle all largely use high purity graphite products.Purification to graphite is exactly that effective means is taken to go
Except the silicate mineral of potassium, sodium, magnesium, iron, calcium, the aluminium contained in graphite etc., the method for production high purity graphite is logical both at home and abroad at present
Often have acid-base method, hydrogen fluoride, chlorinating roasting) and high temperature method.Acid-base method strong applicability, investment advantage less, at low cost,
But also there are the wrong points such as energy consumption is high, process flow length, equipment seriously corroded, contaminated wastewater are serious；Hydrogen fluoride process flow is simple,
Product grade is high, and at low cost, the method is big to equipment corrosion, and strong toxicity；Chlorinating roasting is energy saving, the high-efficient, rate of recovery
Height, but be corrosive there is also chlorine and toxicity, environment is seriously polluted, and process system is unstable, high production cost, certain
The popularization and application of the technique are limited in degree.High temperature method major advantage is to produce 99.99% or more ultra-pure graphite,
But energy consumption is high, requires equipment performance high.It can be seen that the high temperature purification of few halogen or Halogen purification and realization high performance-price ratio is stone
The developing direction of black purification technique.
Summary of the invention
It is existing in the process the invention aims to solve the problems, such as existing high purity graphite material purification, and propose
A kind of new high purity graphite material preparation method.The process of the method for the invention can refer to shown in Fig. 1.
The method that the present invention prepares high purity graphite material sequentially includes the following steps:
Step 1: taking raw graphite, is passed through intermittent graphite purifying device, under the conditions of 1000-1800 DEG C at temperature
0.5-1.0h is managed, solid product is obtained；The temperature is preferably 1600-1800 DEG C；
Step 2: will handle resulting solid product through step 1 and continue to heat up, temperature under the conditions of 1800-2300 DEG C
1~2h is handled to get high purity graphite.The temperature is preferably 2000-2300 DEG C.
The raw graphite carbon content that the method for the invention uses for 85-98%, in order to realize resource reasonable development and sufficiently
It utilizes, the present invention preferably using the graphite of the lower 85-93% of carbon content as raw material, prepares high purity graphite.After to purification
Graphite detects it is found that the phosphorus content in the high purity graphite that raw graphite obtains after step process of the present invention can reach
99.99% or more.
In order to guarantee that impurity effectively adequately removes in graphite raw material, the present invention preferably grinds graphite raw material before preparation
It pre-processes and is passed through halogen gas in temperature-rise period.Grinding pretreatment refers to, will carry out before the raw graphite purification processes
Grinding, is ground to partial size less than 300 μm, preferably 150-200 μm of partial size, to improve purifying speed；Being passed through halogen gas is
Refer to that the present invention is continually fed into gas containing halogen elements, such as chlorine, fluorine gas, carbon tetrachloride, freon in purification process；
The halogen gas is carbon tetrachloride, freon and chlorine gaseous mixture under the conditions of 1000-1800 DEG C；In 1800-2300 DEG C of item
The halogen gas is preferably chlorine under part, and it is 0.2-2m that the present invention, which controls gas flow,3/h；Gas flow of the present invention is
Refer to the gas flow being passed through in every cubic metre of purifying plant inner cavity.Consider to save life simultaneously on the basis of improving purification efficiency
Cost is produced, it is 0.5-1.5m that carbon tetrachloride flow is passed through under the conditions of preferably 1000-1800 DEG C3/ h, under the conditions of 1800-2300 DEG C
The chlorine flowrate being passed through is 1-2m3/h。
The present invention have it is following the utility model has the advantages that
The present invention uses method of purification, and the energy consumption that reduction can be made to prepare specific yield high purity graphite improves production efficiency, reduces
Production cost.The method of the invention can obtain the high purity graphite of 99.99% or more purity.In some special industrial circles
In, such as semiconductor sintering or silica fibre pulling process, it is desirable that impurity content is not to be exceeded tens in the graphite heating body used
A ppm.Therefore, purity provided by the invention has high application value in 99.99% or more graphite.With prior art phase
Than the preparation method of high purity graphite provided by the invention can reduce the purification temperature of high temperature method and the heat-insulated guarantor to graphite purification furnace
Temperature requires, and creates conditions for the industrialized production of high purity graphite, has very big actual promotional value.
Detailed description of the invention
Fig. 1 is the process flow chart of high purity graphite preparation method of the present invention.
Specific embodiment
The technical solution of the present invention is not limited to the following list, further includes any between each specific embodiment
Reasonable combination.Graphite raw material in following embodiment is the graphite of phosphorus content 85-93%.
Specific embodiment 1:
High purity graphite is prepared according to the following steps:
Step 1: taking and be ground to 150-200 μm of graphite raw material of partial size, 1200 DEG C is warming up under the conditions of logical nitrogen protection, heating
Rate is 15 DEG C/min；Continuing to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture simultaneously,
1680 DEG C of heat preservation 1h, obtain solid product；Gas flow rate is 1.5m3/h；
Step 2: resulting solid product relays temperature of continuing rising in graphite purifying device and is passed through 99% chlorine simultaneously to 2300
DEG C, 2h is kept the temperature, heating rate is 2 DEG C/min, gas flow rate 2m3/h；
Through detecting, graphite phosphorus content is 99% after step 1 is handled, and phosphorus content is in graphite after step 2 is handled
99.9999%.
Specific embodiment 2:
High purity graphite is prepared according to the following steps:
Step 1: taking and be ground to 150-200 μm of graphite raw material of partial size, 1200 DEG C is warming up under the conditions of logical nitrogen protection, heating
Rate is 15 DEG C/min；Continuing to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture simultaneously,
1680 DEG C of heat preservation 1h, obtain solid product；Gas flow rate is 1.5m3/h；
Step 2: resulting solid product relays temperature of continuing rising in graphite purifying device and is passed through 99% chlorine simultaneously to 2250
DEG C, 2h is kept the temperature, heating rate is 2 DEG C/min, gas flow rate 2m3/h；
Through detecting, graphite phosphorus content is 99% after step 1 is handled, and phosphorus content is in graphite after step 2 is handled
99.999%.
Specific embodiment 3:
High purity graphite is prepared according to the following steps:
Step 1: taking and be ground to 150-200 μm of graphite raw material of partial size, 1200 DEG C is warming up under the conditions of logical nitrogen protection, heating
Rate is 15 DEG C/min；Continuing to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture simultaneously,
1800 DEG C of heat preservation 1h, obtain solid product；Gas flow rate is 1.5m3/h；
Step 2: resulting solid product relays temperature of continuing rising in graphite purifying device and is passed through 99% chlorine simultaneously to 2100
DEG C, 2h is kept the temperature, heating rate is 2 DEG C/min, gas flow rate 2m3/h；
Through detecting, graphite phosphorus content is 99% after step 1 is handled, and phosphorus content is in graphite after step 2 is handled
99.99%.
Specific embodiment 4:
High purity graphite is prepared according to the following steps:
Step 1: taking and be ground to 200-300 μm of graphite raw material of partial size, 1200 DEG C is warming up under the conditions of logical nitrogen protection, heating
Rate is 15 DEG C/min；Continuing to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture simultaneously,
1800 DEG C of heat preservation 1h, obtain solid product；Gas flow rate is 1.5m3/h；
Step 2: resulting solid product relays temperature of continuing rising in graphite purifying device and is passed through 99% chlorine simultaneously to 2300
DEG C, 2h is kept the temperature, heating rate is 2 DEG C/min, gas flow rate 2m3/h；
Through detecting, graphite phosphorus content is 99% after step 1 is handled, and phosphorus content is in graphite after step 2 is handled
99.999%.
Claims (8)
1. a kind of high purity graphite material preparation method, which is characterized in that the carbon content of the high purity graphite is 99.99% or more.
2. a kind of preparation method of high purity graphite, which is characterized in that this method follows the steps below:
Step 1: taking raw graphite, is passed through closed graphite purifying device, under the conditions of 1000-1800 DEG C at temperature
0.5-1.0 h is managed, solid product is obtained；The temperature is preferably 1600-1800 DEG C；
Step 2: will handle resulting solid product through step 1 and continue to heat up, and temperature is protected under the conditions of 1800-2300 DEG C
1~2 h is to get high purity graphite for temperature processing, and the temperature is preferably 2000-2300 DEG C.
3. the method according to claim 2, which is characterized in that temperature described in step 1 is 1000-1800 DEG C.
4. the method according to claim 2, which is characterized in that temperature described in step 2 is 1800-2300 DEG C.
5. method described in any one according to claim 1~3, which is characterized in that the step 1 further include: raw material stone
Ink need to carry out grinding pretreatment, and the grinding pretreatment is to be ground to partial size less than 300 μm, preferably 100-200 μ of partial size
m。
6. method described in any one according to claim 1~5, which is characterized in that in step 1 or step 2) it is processed
Halogen gas is continually fed into journey.
7. the method according to claim 6, which is characterized in that the intake of the gas is 0.5~2 m3/h。
8. the method according to claim 6, which is characterized in that with 0.5~1.5 m of flow in step 13/ h is passed through
Halogen gaseous mixture, in step 2 with 1~2 m of flow3/ h is passed through the chlorine of 99% or more purity.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255553A (en) * | 2019-07-17 | 2019-09-20 | 钢研晟华科技股份有限公司 | A kind of method that high-temperature vacuum prepares high purity graphite |
| CN111137884A (en) * | 2020-01-10 | 2020-05-12 | 北京化工大学 | Method for purifying graphite through chloridizing roasting |
| CN111186834A (en) * | 2020-01-09 | 2020-05-22 | 成都理工大学 | Method for preparing high-purity graphite by adopting natural crystalline graphite |
| CN111362263A (en) * | 2020-04-07 | 2020-07-03 | 佛山瑞之进智汇科技有限公司 | Preparation method of high-purity graphite material |
| CN111792641A (en) * | 2020-07-20 | 2020-10-20 | 哈尔滨理工大学 | Graphite purification method |
| CN113603085A (en) * | 2021-03-19 | 2021-11-05 | 哈尔滨理工大学 | Method for efficiently purifying graphite |
| CN113735110A (en) * | 2021-11-08 | 2021-12-03 | 山西烁科晶体有限公司 | Purification method of semiconductor-grade graphite powder |
| CN115403407A (en) * | 2022-07-18 | 2022-11-29 | 株洲弗拉德科技有限公司 | Preparation method of high-purity graphite felt |
| WO2023019361A1 (en) * | 2021-08-18 | 2023-02-23 | Kingston Process Metallurgy Inc. | Process for purifying and producing a high purity particulate graphite material for use in lithium-ion batteries |
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| US3416895A (en) * | 1966-10-12 | 1968-12-17 | Ultra Carbon Corp | Method of purifying graphite |
| CN105271216A (en) * | 2015-12-07 | 2016-01-27 | 湖南顶立科技有限公司 | Preparation method of high-purity graphite |
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| CN108147406A (en) * | 2017-11-30 | 2018-06-12 | 巨化集团技术中心 | A kind of method for purifying Delanium |
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| FR1135459A (en) * | 1955-08-03 | 1957-04-29 | Union Carbide & Carbon Corp | Carbon purification |
| US3416895A (en) * | 1966-10-12 | 1968-12-17 | Ultra Carbon Corp | Method of purifying graphite |
| CN105271216A (en) * | 2015-12-07 | 2016-01-27 | 湖南顶立科技有限公司 | Preparation method of high-purity graphite |
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| CN108147406A (en) * | 2017-11-30 | 2018-06-12 | 巨化集团技术中心 | A kind of method for purifying Delanium |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110255553A (en) * | 2019-07-17 | 2019-09-20 | 钢研晟华科技股份有限公司 | A kind of method that high-temperature vacuum prepares high purity graphite |
| CN111186834A (en) * | 2020-01-09 | 2020-05-22 | 成都理工大学 | Method for preparing high-purity graphite by adopting natural crystalline graphite |
| CN111137884A (en) * | 2020-01-10 | 2020-05-12 | 北京化工大学 | Method for purifying graphite through chloridizing roasting |
| CN111362263A (en) * | 2020-04-07 | 2020-07-03 | 佛山瑞之进智汇科技有限公司 | Preparation method of high-purity graphite material |
| CN111792641A (en) * | 2020-07-20 | 2020-10-20 | 哈尔滨理工大学 | Graphite purification method |
| CN113603085A (en) * | 2021-03-19 | 2021-11-05 | 哈尔滨理工大学 | Method for efficiently purifying graphite |
| WO2023019361A1 (en) * | 2021-08-18 | 2023-02-23 | Kingston Process Metallurgy Inc. | Process for purifying and producing a high purity particulate graphite material for use in lithium-ion batteries |
| CN113735110A (en) * | 2021-11-08 | 2021-12-03 | 山西烁科晶体有限公司 | Purification method of semiconductor-grade graphite powder |
| CN113735110B (en) * | 2021-11-08 | 2022-05-13 | 山西烁科晶体有限公司 | Purification method of semiconductor-grade graphite powder |
| CN115403407A (en) * | 2022-07-18 | 2022-11-29 | 株洲弗拉德科技有限公司 | Preparation method of high-purity graphite felt |
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