CN110482542A - A kind of preparation method of high purity graphite heater - Google Patents
A kind of preparation method of high purity graphite heater Download PDFInfo
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- CN110482542A CN110482542A CN201910282676.7A CN201910282676A CN110482542A CN 110482542 A CN110482542 A CN 110482542A CN 201910282676 A CN201910282676 A CN 201910282676A CN 110482542 A CN110482542 A CN 110482542A
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- graphite
- high purity
- purity graphite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
Abstract
A kind of preparation method of high purity graphite heater, is related to a kind of preparation method of high purity graphite heater, and the purpose of the present invention is to solve some problems present in existing high purity graphite heating production procedure.This method is heated up, halogen mixed gas processing 2-5h is passed through under the conditions of 1200-1800 DEG C under nitrogen protection comprising the following specific steps (1) graphite raw material is put into self-control graphite purification device through cold isostatic compaction；(2) resulting solid product continues to heat up after step (1) processing, is passed through gas treatment 3-6h under the conditions of 2100-2300 DEG C to get high purity graphite heater.Preparation method 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 heater of phosphorus content creates conditions, overall cost is lower simultaneously, and environmental protection treatment 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 heater.
Background technique
Graphite has the characteristics such as good conductive, thermally conductive, self-lubricating, anticorrosive, high-low temperature resistant, is widely used as high temperature
Heater, due to containing the silicate mineral impurity of some potassium, sodium, magnesium, iron, calcium, aluminium etc. in graphite, due to impurity presence and
It is unable to satisfy the requirement of certain occasions, is such as used as the graphite heating body of semiconductor monocrystal furnace or fibre drawing furnace.It needs thus pair
Graphite carries out purification removal partial impurities, so that its phosphorus content is reached 99.9% or more, this kind of graphite is known as high purity graphite.To mesh
The method of preceding domestic and international production high purity graphite usually has chemical method (acid-base method, hydrogen fluoride and chlorinating roasting) and high temperature method.
Acid-base method strong applicability, investment advantage less, at low cost, but also have that energy consumption is high, process flow length, equipment seriously corroded, gives up
Water pollution seriously waits wrong point；Hydrogen fluoride process flow is simple, and product grade is high, and at low cost, the method is big to equipment corrosion, and
And strong toxicity；Chlorinating roasting is energy saving, high-efficient, the rate of recovery is high, but is corrosive there is also chlorine and toxicity, seriously pollutes ring
Border, and process system is unstable, high production cost, limits the popularization and application of the technique to a certain extent.High temperature method is main
Advantage is to be able to produce 99.99% or more ultra-pure graphite, but energy consumption is high, is required equipment performance high.It can be seen that few halogen
Or Halogen purifies and realizes that the high temperature purification of high performance-price ratio is the developing direction of graphite purification technology.
Summary of the invention
It is some present in existing high purity graphite heater purification process the invention aims to solve the problems, such as, and propose
A kind of new high purity graphite generates heat preparation.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 heater sequentially includes the following steps:
Step 1: taking raw graphite, is passed through intermittent graphite purifying device, under the conditions of 1200-1800 DEG C at temperature
2-5h 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
3~6h is handled to get high purity graphite.The temperature is preferably 2100-2300 DEG C.
The raw graphite carbon content that the method for the invention uses for 90-98%, in order to realize resource reasonable development and sufficiently
It utilizes, the present invention preferably using the graphite of the relatively low 94-96% of carbon content as raw material, prepares high purity graphite heater.
By being detected to the graphite after purification it is found that the high purity graphite that raw graphite obtains after step process of the present invention is sent out
Phosphorus content in hot body 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
Pretreatment, cold isostatic compaction are simultaneously passed through halogen gas in temperature-rise period.Grinding pretreatment refers to, the raw graphite is mentioned
It is ground before pure processing, is ground to partial size less than 300 μm, preferably 150-200 μm of partial size, to improve purifying speed；It is cold
Isostatic pressing, which refers to, forms heater green body, briquetting pressure 50-100MPa using cold isostatic press；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 1200-1800 DEG C；In 1800-2300 DEG C of item
The halogen gas is preferably chlorine under part, and it is 1-4m that the present invention, which controls gas flow,3/h；Gas flow of the present invention refers to
The gas flow being passed through in every cubic metre of purifying plant inner cavity.Consider to save production simultaneously on the basis of improving purification efficiency
Cost, it is 1-3m that halogen mixed gas flow is passed through under the conditions of preferably 1200-1800 DEG C3/ h is passed through under the conditions of 1800-2300 DEG C
Chlorine flowrate be 2-4m3/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 later period environmental protection pressure is small, creates condition for the industrialized production of high purity graphite calandria, actually pushes away with very big
Wide value.
Detailed description of the invention
Fig. 1 is the process flow chart that high purity graphite of the present invention heats preparation.
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 calandria 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；Continue to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture, In 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；Continue to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture, In 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；Continue to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture, In 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；Continue to heat up at 1200-1800 DEG C, heating rate is 5 DEG C/min and is passed through halogen gaseous mixture, In 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 (9)
1. a kind of preparation method of high purity graphite heater, which is characterized in that the carbon content of the high purity graphite heater exists
99.99% or more.
2. a kind of preparation method of high purity graphite heater, which is characterized in that this method follows the steps below:
Step 1: taking raw graphite, is passed through closed graphite purifying device, temperature under the conditions of 1200-1800 DEG C
2-5 h are handled, 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
For isothermal holding 3-6 h to get high purity graphite, the temperature is preferably 2100-2300 DEG C.
3. the method according to claim 2, which is characterized in that temperature described in step 1 is 1200-1800 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
Graphite need to carry out grinding pretreatment, and the grinding pretreatment is to be ground to partial size less than 300 μm, preferably partial size 100-200
μm。
6. method described in any one according to claim 1~3, which is characterized in that the step 1 further include: pre- place
For raw graphite after reason through cold isostatic compaction, briquetting pressure is 75-100 MPa. in 50-100 MPa, preferably pressure.
7. method described in any one according to claim 1~6, which is characterized in that in step 1 or step 2) processing
It is continually fed into halogen gas in the process.
8. the method according to claim 6, which is characterized in that the intake of the gas is 1~4 m 3/h。
9. the method according to claim 6, which is characterized in that with 1~3 m of flow in step 1 3/ h is passed through
Halogen gaseous mixture, in step 2 with 2~4 m of flow3/ h is passed through the chlorine of 99% or more purity.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN113603085A (en) * | 2021-03-19 | 2021-11-05 | 哈尔滨理工大学 | Method for efficiently purifying graphite |
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| CN101920957A (en) * | 2010-08-17 | 2010-12-22 | 北京矿冶研究总院 | Preparation method of high-purity 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 |
| CN105460923A (en) * | 2015-12-25 | 2016-04-06 | 山东重山光电材料股份有限公司 | Continuous preparing method of high purity carbon monofluoride |
| CN108069422A (en) * | 2017-12-25 | 2018-05-25 | 凯盛石墨碳材料有限公司 | A kind of method of graphite purification |
| CN108147406A (en) * | 2017-11-30 | 2018-06-12 | 巨化集团技术中心 | A kind of method for purifying Delanium |
| CN109292769A (en) * | 2018-11-23 | 2019-02-01 | 湖南顶立科技有限公司 | A kind of high purity graphite powder and preparation method thereof |
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2019
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Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101920957A (en) * | 2010-08-17 | 2010-12-22 | 北京矿冶研究总院 | Preparation method of high-purity 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 |
| CN105460923A (en) * | 2015-12-25 | 2016-04-06 | 山东重山光电材料股份有限公司 | Continuous preparing method of high purity carbon monofluoride |
| CN108147406A (en) * | 2017-11-30 | 2018-06-12 | 巨化集团技术中心 | A kind of method for purifying Delanium |
| CN108069422A (en) * | 2017-12-25 | 2018-05-25 | 凯盛石墨碳材料有限公司 | A kind of method of graphite purification |
| CN109292769A (en) * | 2018-11-23 | 2019-02-01 | 湖南顶立科技有限公司 | A kind of high purity graphite powder and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN113603085A (en) * | 2021-03-19 | 2021-11-05 | 哈尔滨理工大学 | Method for efficiently purifying graphite |
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