CN1616347A - High purity graphite purfying process - Google Patents
High purity graphite purfying process Download PDFInfo
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- CN1616347A CN1616347A CN 200410087882 CN200410087882A CN1616347A CN 1616347 A CN1616347 A CN 1616347A CN 200410087882 CN200410087882 CN 200410087882 CN 200410087882 A CN200410087882 A CN 200410087882A CN 1616347 A CN1616347 A CN 1616347A
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Abstract
The technological process of purifying graphite includes soaking reaction between microcrystalline graphite material with carbon content over 80 % and the hydrofluoric acid and sulfuric acid solution in reactor under the heating with water vapor at 70-90 deg.c for 7-9 hr; separating graphite from the solution to obtain acid-containing graphite; water washing to pH 5.5-6.5, deposition, pressure filtering and stoving to obtain microcrystalline graphite of carbon content over 99 %. The material composition includes microcrystalline graphite 30-35 wt%, hydrofluoric acid solution 20-30 wt% and sulfuric acid solution 35-45 wt%, where the hydrofluoric acid solution has concentration of 40 % and density of 1.13, and the sulfuric acid solution has concentration of 98 % and density of 1.84. The purified graphite of carbon content over 99 %, water content less than 0.5 % and ash content less than 1 % has expanded application range, and may be used especially in producing graphite milk for color TV.
Description
One, technical field:
The present invention discloses a kind of graphite purfying process, and particularly a kind of is the purifying technique that raw material extracts high purity graphite with the micro crystal graphite.
Two, background technology:
Graphite is a kind of important nonmetallic mineral material, high-carbon, high-purity, ultra-fine be the basic prerequisite that graphite material is used widely in high-tech sector.Micro crystal graphite is that the method for purification of raw material comprises: (1) is the molten alkaline process of auxiliary material with solid members solid NaOH; (2) with liquid NaOH be the normal pressure method of purification of auxiliary material; (3) with HF-HCL system method of purification; (4) with HF-chloroazotic acid system method of purification.The carbon content of the method for these several purifications between 92-97.5%, do not reach the requirement of 99% purity, thereby range of application is restricted usually.
Three, summary of the invention:
Purpose of the present invention is exactly the low defective of purification degree that exists at prior art, and a kind of high purity graphite purfying process is provided.
Technical scheme comprises the steps: that (1) is raw material with carbon content greater than 80% Graphite Powder 99, adds in the reactor with hydrofluoric acid and sulphuric acid soln, and water vapour is warmed to 70-90 ℃, stirs, floods reaction 7-9 hour simultaneously, simultaneously combustion gas; (2) with whizzer reacted acid solution is separated with graphite, the acid solution after the separation is recycled; (3) acidiferous graphite is washed, and reaches pH value at 5.5-6.5; (4) carry out settlement separately, acid solution after the separation is recycled; (5) with pressure filter separation solution and solution discharged once more, obtain Graphite Cake; (6) Graphite Cake is dried the back and pulverize, make high purity finished product Graphite Powder 99.The weight proportion of graphite and hydrofluoric acid, sulphuric acid soln is respectively: 30-35%, 20-30%, 35%-45%, described hydrofluoric acid are concentration 40%, density 1.13, and sulfuric acid is concentration 98%, density 1.84.Comprise also in the above-mentioned technology that Graphite Powder 99 sets up several feed reservoir separately, interconnect between each feed reservoir, hydrofluoric acid and sulfuric acid are provided with an amount acid tank, mixed acid solution can directly enter reactor, also can enter in the feed reservoir of Graphite Powder 99, through centrifugation and settlement separate after recovery solution directly enter in the feed reservoir of Graphite Powder 99 and use, the waste gas that produces in the technology and the waste liquid of discharge carry out environmental protection treatment respectively.
Purifying technique of the present invention can be purified to the micro crystal graphite of carbon content 80% carbon content and be not less than 99%, moisture content is not more than 0.5%, the ash content of coal is not more than 1% high purity graphite, promote the technology content and the range of application of micro crystal graphite greatly, particularly can use this products production colour TV aquadag product.
Four, description of drawings:
Accompanying drawing is the process flow sheet of one embodiment of the present invention.
Five, embodiment:
With reference to accompanying drawing, (1) the microlite ink powder with 1280 kilograms carbon content 80% adds in three interconnective successively feed reservoir, in the sulphuric acid soln amount acid tank with the hydrofluoric acid solution of 960 kilograms of concentration 40%, density 1.13 and 1680 kilograms of concentration 98%, density 1.84, add reactor, with 80 ℃ steam reactor is heated to 80 ℃, stir, flood reaction 8 hours simultaneously, get rid of gas and carry out environmental protection treatment.(2) will react back solution with whizzer and separate, recycle in the acid solution amount of returning to acid tank after the separation or the feed reservoir with graphite.(3) wash through disperseing the pond that acidiferous Graphite Cake is disperseed to deliver to water wash column, pH value is controlled at 6.(4) put into settling bowl and precipitate, the acid solution after the separation returns in the feed reservoir to be recycled.(5) with pressure filter once more separation solution and solution discharged after carry out recycling as the washing water in the step (3) after the environmental protection treatment, and obtain Graphite Cake; (6) Graphite Cake put into dryer dry after, enter pulverizer and pulverize, make high purity finished product Graphite Powder 99, measure at last, pack.
This purifying technology is in time cleared up the fluorochemical that chemical reaction produces in the purification process, and the fluoro-gas that produces when clearing up is constantly escaped, and has guaranteed that reaction channel is unblocked, and the chemical reaction that graphite is purified can carry out thoroughly.Adopt this technology, can be that 80% micro crystal graphite is purified to carbon content is not less than 99%, ash is not more than 1%, moisture is not more than 0.5% high-carbon graphite with carbon containing, make tens of times of micro crystal graphite raw ore increments, can create remarkable economic efficiency and social benefit.
Claims (3)
1, a kind of high purity graphite purfying process, it is characterized in that this technology comprises the steps: that (1) is raw material with carbon content greater than 80% Graphite Powder 99, add in the reactor with hydrofluoric acid and sulphuric acid soln, water vapour is warmed to 70-90 ℃, stir, flood reaction 7-9 hour simultaneously, simultaneously combustion gas; (2) with whizzer reacted acid solution is separated with graphite, the acid solution after the separation is recycled; (3) acidiferous graphite is washed, and reaches pH value at 5.5-6.5; (4) carry out settlement separately, acid solution after the separation is recycled; (5) with pressure filter separation solution and solution discharged once more, obtain Graphite Cake; (6) Graphite Cake is dried the back and pulverize, make high purity finished product Graphite Powder 99.
2, high purity graphite purfying process according to claim 1, the weight proportion that it is characterized in that graphite and hydrofluoric acid, sulphuric acid soln is respectively: 30-35%, 20-30%, 35%-45%, described hydrofluoric acid is concentration 40%, density 1.13, and sulfuric acid is concentration 98%, density 1.84.
3, high purity graphite purfying process according to claim 1, it is characterized in that Graphite Powder 99 sets up several feed reservoir separately, interconnect between each feed reservoir, hydrofluoric acid and sulfuric acid are provided with an amount acid tank, mixed acid solution can directly enter reactor, also can enter in the feed reservoir of Graphite Powder 99, through centrifugation and settlement separate after recovery solution directly enter in the feed reservoir of Graphite Powder 99 and use, the waste gas that produces in the technology and the waste liquid of discharge carry out environmental protection treatment respectively.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100878826A CN100371244C (en) | 2004-07-28 | 2004-10-25 | High purity graphite purfying process |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410035472 | 2004-07-28 | ||
| CN200410035472.7 | 2004-07-28 | ||
| CNB2004100878826A CN100371244C (en) | 2004-07-28 | 2004-10-25 | High purity graphite purfying process |
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| Publication Number | Publication Date |
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| CN1616347A true CN1616347A (en) | 2005-05-18 |
| CN100371244C CN100371244C (en) | 2008-02-27 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2004100878826A Expired - Fee Related CN100371244C (en) | 2004-07-28 | 2004-10-25 | High purity graphite purfying process |
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| CN (1) | CN100371244C (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101983917A (en) * | 2010-11-02 | 2011-03-09 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | Preparation method of high purity graphite |
| CN101367517B (en) * | 2008-09-24 | 2011-08-10 | 青岛恒胜石墨有限公司 | Method for preparing high pure graphite with steam heating |
| CN103373723A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | High-purity crystalline graphite purifying process |
| CN108203092A (en) * | 2018-02-06 | 2018-06-26 | 青岛晶莹石墨有限公司 | Graphite powder impurity removal process and sewage treatment process |
| CN113233454A (en) * | 2021-06-24 | 2021-08-10 | 黑龙江普莱德新材料科技有限公司 | Method for producing high-purity graphite by using recovered acid |
| CN113716559A (en) * | 2021-09-03 | 2021-11-30 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Strong acid method scale graphite purification process and device |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0621020B2 (en) * | 1987-11-28 | 1994-03-23 | 東北大学長 | Method for producing highly oriented sheet-shaped graphite using layered compounds |
| CN1020089C (en) * | 1990-11-30 | 1993-03-17 | 中国科学院西安光学精密机械研究所 | Graphite purification method |
| CN1062834C (en) * | 1998-08-31 | 2001-03-07 | 四川轻化工学院 | Method for producing flexible graphite material with medium-carbon natural scaly graphite powder |
| CA2374132A1 (en) * | 2002-03-01 | 2003-09-01 | Hydro Quebec | Procedure for the surface purification of graphite containing impurities by means of a diluted aqueous solution of nh4f and h2so4 |
-
2004
- 2004-10-25 CN CNB2004100878826A patent/CN100371244C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101367517B (en) * | 2008-09-24 | 2011-08-10 | 青岛恒胜石墨有限公司 | Method for preparing high pure graphite with steam heating |
| CN101983917A (en) * | 2010-11-02 | 2011-03-09 | 黑龙江省牡丹江农垦奥宇石墨深加工有限公司 | Preparation method of high purity graphite |
| CN103373723A (en) * | 2012-04-17 | 2013-10-30 | 夏华松 | High-purity crystalline graphite purifying process |
| CN108203092A (en) * | 2018-02-06 | 2018-06-26 | 青岛晶莹石墨有限公司 | Graphite powder impurity removal process and sewage treatment process |
| CN113233454A (en) * | 2021-06-24 | 2021-08-10 | 黑龙江普莱德新材料科技有限公司 | Method for producing high-purity graphite by using recovered acid |
| CN113716559A (en) * | 2021-09-03 | 2021-11-30 | 黑龙江省宝泉岭农垦溢祥石墨有限公司 | Strong acid method scale graphite purification process and device |
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| Publication number | Publication date |
|---|---|
| CN100371244C (en) | 2008-02-27 |
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