CN1098807C - Process for preparing flake-shaped expanded graphite - Google Patents
Process for preparing flake-shaped expanded graphite Download PDFInfo
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- CN1098807C CN1098807C CN98102501A CN98102501A CN1098807C CN 1098807 C CN1098807 C CN 1098807C CN 98102501 A CN98102501 A CN 98102501A CN 98102501 A CN98102501 A CN 98102501A CN 1098807 C CN1098807 C CN 1098807C
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Abstract
The present invention is characterized in that mixed thin scale graphite (carbon content is from 85 to 96%) with the granularity of 100 to 160 meshes is put in main acid solution prepared from sulfuric acid (with the concentration of 96%) and nitric acid (with the concentration of 65%) according to the proportion of (5 to 7.5) to 1, and is uniformly stirred; after 20 to 30 minutes, potassium permanganate (with the use quantity of 6 to 7% of graphite quantity) is added and intermittently stirred for 20 to 30 minutes; ferric trichloride (with the use quantity of 5 to 6% of the graphite quantity) is added and intermittently stirred for 2 to 10 hours; the acid solution is filtered; the mixed thin scale graphite is washed with water until the pH is from 5 to 7, dried until the water is from 10 to 20%, and instantly expanded at the high temperature of 900 to 1000 DEG C. The present invention reduces the use quantity of the nitric acid by 30 to 60%, the cost and environmental pollution.
Description
The present invention relates to the preparation field of graphite material, particularly the flake-shaped expanded graphite preparation methods.
The basic skills of existing employing chemistry side's preparation expanded graphite is: with natural flake graphite (granularity is 15～80 orders) sulfuric acid (concentration 95～98%), the mix acid liquor that nitric acid (concentration 65～85%) is mixed with is made immersion treatment, after washing, drying, under 800～1000 ℃ of high temperature, make instantaneous expansion, can obtain expansion multiple and be tens to hundred times, loose density is the expanded graphite of 0.004～0.015g/ml.Chinese patent CN1032325A proposes, adopt substep to add sulfuric acid, nitric acid=2: 1), an amount of strong oxidizer potassium permanganate and intercalating agent iron trichloride nitric acid (sulfuric acid:, 50 orders are done to add sulfuric acid, nitric acid (sulfuric acid: nitric acid=1～2: 1) as secondary oxidative treatments again after once oxidation is handled with thick graphite, through washing, dry, under 900 ℃ of high temperature, expanding, can obtain the expansion multiple more than 1000 times, preparing with chemical process in the technology of expanded graphite, the sulfuric acid of use and the ratio of nitric acid are sulfuric acid: nitric acid=2～3: 1.But this method nitric acid dosage is big, cost height, harm environment.
The crystalline flake graphite granularity that is used to prepare expanded graphite is generally 50 orders with slightly, also have minority with 80 orders with thick.Chinese patent CN95103917N claim invent earlier with nitric acid, make to add after oxide treatment, the washing oxidation calcium powder with sulfuric acid again and prepare expandable method and be applicable to 200 orders with thick crystalline flake graphite, but its to use real being listed as still be that 100 orders are with thick crystalline flake graphite.Up to now, utilization still is not reported less than the research that the thin scale of 100 purposes prepares expanded graphite.
The objective of the invention is to overcome above shortcoming, working out a kind of being suitable for granularity is that 100 orders～160 purposes are mixed processing condition and the technical process that thin crystalline flake graphite prepares the high-quality expanded graphite, and this worker's condition and technical process also are suitable for using greater than 100 purpose crystalline flake graphites and prepare the high-quality expanded graphite.
The present invention places the mixing thin crystalline flake graphite (carbon content 85～96%) of granularity between 100 orders～160 orders by sulfuric acid (concentration 96%); Stir in the main acidizing fluid of nitric acid (concentration 65%)=5～7.5: 1 preparation, add potassium permanganate (consumption be quantity of graphite 6～7%) after 20～30 minutes, intermittently stir and added iron trichloride (consumption be quantity of graphite 5～6%) in 20～30 minutes, intermittently stirred 2～10 hours, filtering acid solution, water are washed to pH5～7, dry to moisture 10～20%, under 900～1000 ℃ of high temperature, carry out instantaneous expansion, can obtain to have the expanded graphite of premium properties.
The processing condition of the technology of the present invention are:
Graphite raw material: granularity 100＞N＞160 orders
Carbon content 85～96%
Sulfuric acid: nitric acid: 5～7.5: 1
Potassium permanganate: 60～70g/kg graphite
Ferrous chloride: 50～60g/kg graphite
PH value: 5～7
Expansion temperature: 900～1000 ℃
The technical process of the technology of the present invention is:
With 85～96% of carbon content, granularity 160＜N＜thin crystalline flake graphite of 100 purposes is inserted to scale the ratio of the mixing acidizing fluid of the sulfuric acid (concentration 96%) of preparation and nitric acid (concentration 65%) and is advisable to be modulated into suspension liquid) stir, add an amount of potassium permanganate after 20～30 minutes, intermittently stir and add an amount of iron trichloride after 20～30 minutes, intermittently stirred 2～10 hours, remove acid solution, water is flushed to pH5～7, dry to moisture 10～20%, under 900～1000 ℃ of high temperature, instantaneous expansion just obtains expansion multiple expanded graphite more than 200 times.
Adopt above processing condition and technical process can obtain quality expanded graphite preferably, its technical indicator compares as table one with domestic and international advanced level:
| The state of the art index | Advanced international level | International most advanced level | The present inventor | ||
| Thin scale＜100 orders | The big scale of outsourcing＞80 orders | ||||
| Loose density | 0.004～0.0052 (big scale＞80 orders) | (0.0052 big scale＞80 orders) | 0.0125 | 0.0026 | |
| Volatile matter % | 12～14 | 10.5～12.76 | 4.5～8.5 | 4.012 | |
| Sulphur content % | 2.5～3 | 2～2.65 | 0.213～0.233 | 0.211 | |
| Ash content % | One class | ＜0.1 | ＜0.1 | ||
| Two classes | ＜3 | ＜3 | 2.06～2.47 | 0.897 | |
| Three classes | ＜6％ | ||||
Table 1, expanded graphite the key technical indexes are relatively
By as can be known last, adopt its inspection density of invented technology condition and technical process system expanded graphite (with equal granulometric facies ratio), volatile matter, sulphur content content all to be better than internal and international advanced level, ash oontent meets the second standard requirement.
The present invention has the following advantages:
1. the graphite raw material granularity of Shi Yonging is mixed thin crystalline flake graphite in 100 orders～160 purposes, and this method still has good effect for the crystalline flake graphite of granularity more than 100 orders.
2. in main acidizing fluid, the ratio of sulfuric acid and nitric acid is 5-.5: 1, nitric acid reduced 30%-60% than traditional method, and the harm of nitrosonitric acid to environment has not only reduced cost but also reduced.
3. in oxidising process, substep adds sulfuric acid, nitric acid, potassium permanganate, iron trichloride, finishes once that oxidation need not add sulfuric acid and nitric acid carries out secondary oxidation.
Be described in further detail below in conjunction with embodiment:
Embodiment 1
Thin crystalline flake graphite, granularity is 100 orders-160 an order mixing raw material, carbon content 85-96%, sulfuric acid: nitric acid=7.5: 1, potassium permanganate 64g/kg graphite, iron trichloride 60g/kg graphite, the pH value is 5,950 ℃ of expansion temperatures.The expanded graphite technical indicator that obtains is: 200 times of expansion multiples, loose density 0.0125g/ml, ash content 2.47%, sulphur content 0.213%, volatile matter 8.47%.
Embodiment 2
Thin crystalline flake graphite, granularity is 100 orders-160 an order mixing raw material, carbon content 85-96%, sulfuric acid: nitric acid=5: 1, potassium permanganate 64g/kg graphite, iron trichloride 60g/kg graphite, 950 ℃ of expansion temperatures.The expanded graphite technical indicator that obtains is: 195 times of expansion multiples, loose density 0.0125g/ml, ash content 2.06%, sulphur content 0.233%, volatile matter 5.01%.
Embodiment 3
Flaky graphite, granularity is greater than 80 orders, sulfuric acid: nitric acid=7.5: 1, potassium permanganate, iron trichloride, expansion temperature are with embodiment one, and the pH value is 5, and the expanded graphite technical indicator of acquisition is: expansion multiple＞900 times, loose density 0.0026g/ml, ash content 0.897%, sulphur content 0.211%, volatile matter 4.0%.
Claims (1)
1. process for preparing flake-shaped expanded graphite, it is characterized in that: with granularity between 100 orders-160 order, carbon content is at the thin crystalline flake graphite of mixing of 85-96%, place acidizing fluid to stir, acidizing fluid proportioning: the sulfuric acid of concentration 96%: the nitric acid=5-7.5 of concentration 65%: 1, adding consumption after 20-30 minute is the potassium permanganate of quantity of graphite 6-7%, intermittently stir that to add consumption after 30-30 minute be the iron trichloride of quantity of graphite 5-6%, intermittently stir filtering acid solution after 2-10 hour, water washes to pH5-7, dry to moisture 10-20%, under 900-1000 ℃ of high temperature, carry out instantaneous expansion, can obtain expanded graphite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98102501A CN1098807C (en) | 1998-06-17 | 1998-06-17 | Process for preparing flake-shaped expanded graphite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN98102501A CN1098807C (en) | 1998-06-17 | 1998-06-17 | Process for preparing flake-shaped expanded graphite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1239071A CN1239071A (en) | 1999-12-22 |
| CN1098807C true CN1098807C (en) | 2003-01-15 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN98102501A Expired - Fee Related CN1098807C (en) | 1998-06-17 | 1998-06-17 | Process for preparing flake-shaped expanded graphite |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3691836B1 (en) * | 2004-08-27 | 2005-09-07 | 東洋炭素株式会社 | Expanded graphite sheet |
| CN100400416C (en) * | 2006-07-11 | 2008-07-09 | 河北农业大学 | Process for preparing expandable graphite with high reference expansion temperature |
| CN102320596A (en) * | 2011-07-13 | 2012-01-18 | 武汉理工大学 | Preparation method of fine-flake expanded graphite |
| CN102408108A (en) * | 2011-07-27 | 2012-04-11 | 攀枝花学院 | Expanding method of fine flake graphite and preparation method of expanded graphite board |
| CN102491310A (en) * | 2011-11-18 | 2012-06-13 | 武汉理工大学 | Preparation method of finely squamose sulfur-free expandable graphite |
| CN103578678A (en) * | 2013-11-20 | 2014-02-12 | 南京工程学院 | Magnetic iron-based graphite intercalation compound and preparation method thereof |
| CN105419559B (en) * | 2015-11-25 | 2018-10-19 | 浙江华彩新材料有限公司 | A kind of antifouling and antibiosis electronic component fluorescent powder coating and preparation method thereof |
| CN105419558B (en) * | 2015-11-25 | 2019-02-01 | 浙江华彩新材料有限公司 | A kind of antibacterial electronic component fluorescent powder coating and preparation method thereof |
| CN106185881A (en) * | 2016-06-07 | 2016-12-07 | 黑龙江省宝泉岭农垦帝源矿业有限公司 | A kind of method that in utilization, low-carbon (LC) Fine particle processing prepares sulphur-free expanded graphite |
| CN106185882A (en) * | 2016-06-07 | 2016-12-07 | 黑龙江省宝泉岭农垦帝源矿业有限公司 | A kind of method that in utilization, low-carbon (LC) Fine particle processing prepares low-sulphur expanded graphite |
| CN109437950A (en) * | 2018-11-23 | 2019-03-08 | 大同新成新材料股份有限公司 | A kind of manufacturing process of graphite-seal ring |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032325A (en) * | 1987-09-03 | 1989-04-12 | 清华大学 | The manufacture method of high magnification expansible crystalline flake graphite |
| CN1153743A (en) * | 1996-10-18 | 1997-07-09 | 宋克敏 | Prodn process of no-sulphur expansion graphite |
-
1998
- 1998-06-17 CN CN98102501A patent/CN1098807C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1032325A (en) * | 1987-09-03 | 1989-04-12 | 清华大学 | The manufacture method of high magnification expansible crystalline flake graphite |
| CN1153743A (en) * | 1996-10-18 | 1997-07-09 | 宋克敏 | Prodn process of no-sulphur expansion graphite |
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|---|---|
| CN1239071A (en) | 1999-12-22 |
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