CN106083049A - A kind of method preparing isotropic graphite material from sintering - Google Patents
A kind of method preparing isotropic graphite material from sintering Download PDFInfo
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Abstract
The present invention relates to a kind of method preparing isotropic graphite material from sintering, its comprise the steps: 1. by softening point at 200 330 DEG C, it is 5 30 μm that the high softening point bitumen between mesophase content ＜ 0.1%wt is crushed to particle diameter, obtains Colophonium powder；2. by above-mentioned steps 1. in the Colophonium powder for preparing mix according to the mass ratio of 1:5 1:20 with Oxygen in Liquid agent after put into liquid oxidizer and carry out oxidation processes, obtain powdery primary raw materials；3. by above-mentioned steps 2. in prepare powdery primary raw materials be shaped processing, obtain moulding material；4. by above-mentioned steps 3. in prepare moulding material under normal pressure, nonoxidizing atmosphere, be heated to 800 1000 DEG C, obtain carbonaceous product；5. by above-mentioned steps 4. in prepare carbonaceous product under normal pressure, nonoxidizing atmosphere, be heated to 2,200 2800 DEG C, obtain isotropic graphite material.Beneficial effects of the present invention: technique is simple, small investment, and product quality is more preferable.
Description
Technical field
The present invention relates to a kind of method preparing graphite material, particularly relate to one and prepare isotropic graphite material from sintering
The method of material.
Background technology
Graphite is the indispensable conductive material of national economy and the structural woods such as development metallurgy, chemical industry, electronics and nuclear industry
Material, it has the higher capacity of heat transmission, low thermal coefficient of expansion, good rupture strength, comprcssive strength and chemical stability.Stone
Ink crystal structure is a kind of mixed type crystal structure: in aspect, atom is six side's grid arrangement, and atomic distance is little, and adhesion is strong；
Spacing between aspect is relatively big, and adhesion is more weak；So its in-plane is bigger, just with the nature difference being perpendicular to in-plane
It is so-called " anisotropy ".And many special occasions propose the requirement of " isotropism " to graphite material.High anti bending strength,
The isotropic graphite material that comprcssive strength is high, thermal coefficient of expansion is low is mainly used in military project, Aero-Space, ultra high power electricity
The leading-edge fields such as pole, nuclear industry graphite.So, the preparation of isotropic graphite becomes an important research of high performance graphite
Direction.
The preparation method of Conventional graphite material mainly have two kinds: one be coke aggregate with pitch binder through kneading and compacting,
Carbonization, graphitization.Pitch binder changes into charcoal in carbonization process, and this charcoal and aggregate are the charcoals of two kinds of separate sources, and two
There is more interface between person, the performance making graphite material is not the highest, and isotropism degree is poor.Two is by having
Green coke or the mesophase pitch bead green-ball of self sintering are molded directly into type, then carbonization, graphitization.Owing to not boning
Agent, prepared graphite material median surface is few, can prepare the graphite material that intensity is big, the coefficient of expansion is low, isotropism degree is good.
In document, most non-fusible reaction is gas oxidation, is i.e. passed through air, utilizes the oxygen in air to do oxidant.
The method advantage is that non-fusible reaction is complete, non-fusible effective, and shortcoming is time-consuming long, and investment is big；Especially to low softening point
Colophonium, its non-fusible temperature and heating rate are difficult to control, non-fusible for up to tens hours, non-fusible weak effect.
Liquid phase is non-fusible just can make up this shortcoming, the non-fusible time can be reduced to dozens of minutes, and the softening point to Colophonium
Do not require.Domestic current this method yet there are no application, and external E.Vilaplana-Ortego et al. exists
“Stabilisation of low softening point petroleum pitch fibres by HNO3 ”(Carbon
41,2003,1,001 1007), in, the petroleum pitch fibre of different softening point is put in the aqueous solution of nitric acid of variable concentrations, enter
After row liquid phase is non-fusible, carry out carbonization, obtained the preferable Carbon fibe of quality, illustrate that liquid phase oxidation is feasible.
Summary of the invention
The technical problem to be solved is: provide a kind of method preparing isotropic graphite material from sintering,
Solving the method complicated process of preparation commonly preparing isotropic graphite material, the time is long, and investment is many, and the graphite material prepared
Expect second-rate problem.
The present invention solves that problem set forth above be the technical scheme is that
A kind of method preparing isotropic graphite material from sintering, its comprise the steps: 1. by softening point at 200-330
DEG C, it is 5-30 μm that the high softening point bitumen between mesophase content ＜ 0.1%wt is crushed to particle diameter, obtains Colophonium powder；2. by above-mentioned
Step 1. in the Colophonium powder for preparing mix according to the mass ratio of 1:5-1:20 with Oxygen in Liquid agent after put into liquid oxidizer and enter
Row oxidation processes, obtains powdery primary raw materials；3. by above-mentioned steps 2. in prepare powdery primary raw materials be shaped processing, obtain
Moulding material；4. by above-mentioned steps 3. in prepare moulding material under normal pressure, nonoxidizing atmosphere, be heated to 800-1000 DEG C,
To carbonaceous product；5. by above-mentioned steps 4. in prepare carbonaceous product under normal pressure, nonoxidizing atmosphere, be heated to 2200-2800
DEG C, obtain isotropic graphite material.
Described step 2. middle oxidation treatment time is 10-50min.
Described step 2. in liquid oxidizer be mass concentration be the sulfuric acid solution of the salpeter solution of 10-30%, 70-90%
Or any one in the mixed acid solution that is mixed for 1:3-2:1 in mass ratio of the sulphuric acid of the nitric acid of 10-30% and 70-90%.
Described step 2. in carry out the degree of oxidation processes for making Colophonium powder the most fully crosslinked, also have after heating
Certain softening properties, its fugitive constituent is at 10-12%wt, and described fugitive constituent plays binding agent effect in carbonization process.
3. described step is shaped processing and uses any one in compression molding, vibration moulding or isostatic pressing.
Described step 4. middle nonoxidizing atmosphere is under inert gas shielding or method isolation air buried by coke powder.
Described step 5. middle nonoxidizing atmosphere is under inert gas shielding or method isolation air buried by coke powder.
The isotropic graphite material that described method prepares, its rupture strength is 35-100MPa, and comprcssive strength is 90-
250MPa, bulk density is 1.6-1.8g/cm3, isotropism degree is 1.02-1.07.
The beneficial effects of the present invention is: 1, present invention process is simple, and the time is short, small investment.2, selected by the present invention
High softening point bitumen, macroscopically or be all isotropic on microcosmic, the isotropic graphite material prepared has
High anti bending strength, comprcssive strength are good, bulk density and the good characteristic of isotropism.3, by the isotropism stone from sintering preparation
Ink material, preparation technology is simple, owing to there is no binding agent, constant product quality, function admirable.
Detailed description of the invention
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
The high softening point bitumen that softening point is 200 DEG C is crushed to mean diameter 30 μm, with the nitric acid that mass concentration is 30% by matter
Amount mixes than for 1:5, aoxidizes 50 minutes, obtains powdery primary raw materials；By above-mentioned powdery primary raw materials through compression molding, then exist
Carry out carbonization, constant temperature 1 hour at 800 DEG C under normal pressure, inert atmosphere protection, obtain carbonaceous product；At normal pressure, inert atmosphere protection
Under carry out graphitization at 2800 DEG C, obtain isotropic graphite material；Gained isotropic graphite material rupture strength is 35MPa,
Comprcssive strength is 90MPa, and bulk density is 1.60g/cm3, isotropism degree is 1.07.
Embodiment 2
The high softening point bitumen that softening point is 235 DEG C is crushed to mean diameter 25 μm, presses quality with the sulphuric acid of mass concentration 90%
Mix than for 1:8, aoxidize 40 minutes, obtain powdery primary raw materials.By above-mentioned powdery primary raw materials through compression molding, then often
Carry out carbonization, constant temperature 1 hour at 950 DEG C under pressure, inert atmosphere protection, obtain carbonaceous product；Under normal pressure, inert atmosphere protection
Carry out graphitization at 2600 DEG C, obtain isotropic graphite material；Product rupture strength is 45MPa, and comprcssive strength is 120MPa, body
Long-pending density is 1.63g/cm3, isotropism degree is 1.05.
Embodiment 3
The high softening point bitumen that softening point is 250 DEG C is crushed to mean diameter 15 μm, with nitration mixture (nitric acid by 30% and 70%
Sulphuric acid forms for 1:3 in mass ratio) mix for 1:10 in mass ratio, aoxidize 25 minutes, obtain powdery primary raw materials.By above-mentioned powder
Shape primary raw materials, through compression molding, then carries out carbonization, constant temperature 1 hour at 900 DEG C under normal pressure, inert atmosphere protection, obtains
Carbonaceous product；Under normal pressure, inert atmosphere protection, carry out graphitization at 2400 DEG C, obtain isotropic graphite material；Gained respectively to
Same sex graphite material rupture strength is 81MPa, and comprcssive strength is 201MPa, and bulk density is 1.75g/cm3, isotropism degree is
1.03。
Embodiment 4
The high softening point bitumen that softening point is 270 DEG C is crushed to mean diameter 10 μm, presses quality with the nitric acid of mass concentration 20%
Mix than for 1:13, aoxidize 20 minutes, obtain powdery primary raw materials.By above-mentioned powdery primary raw materials through compression molding, then exist
Carry out carbonization, constant temperature 1 hour at 1000 DEG C under normal pressure, inert atmosphere protection, obtain carbonaceous product；Protect at normal pressure, inert atmosphere
Protect down and carry out graphitization at 2800 DEG C, obtain isotropic graphite material；Gained isotropic graphite material rupture strength is
100MPa, comprcssive strength is 250MPa, and bulk density is 1.8g/cm3, isotropism degree is 1.02.
Embodiment 5
The high softening point bitumen that softening point is 290 DEG C is crushed to mean diameter 10 μm, with nitration mixture (nitric acid by 20% and 80%
Sulphuric acid forms for 1:1 in mass ratio) mix for 1:16 in mass ratio, aoxidize 30 minutes, obtain powdery primary raw materials.By above-mentioned powder
Shape primary raw materials, through compression molding, then carries out carbonization, constant temperature 1 hour at 1000 DEG C under normal pressure, inert atmosphere protection, obtains
Carbonaceous product；Under normal pressure, inert atmosphere protection, carry out graphitization at 2700 DEG C, obtain isotropic graphite material；Gained respectively to
Same sex graphite material rupture strength is 95MPa, and comprcssive strength is 244MPa, and bulk density is 1.79g/cm3, isotropism degree is
1.02。
Embodiment 6
The high softening point bitumen that softening point is 300 DEG C is crushed to mean diameter 5 μm, with 70% sulphuric acid be 1:15 in mass ratio
Mixing, aoxidizes 10 minutes, obtains powdery primary raw materials.By above-mentioned powdery primary raw materials through compression molding, then in normal pressure, inertia
Carry out carbonization, constant temperature 1 hour at 1000 DEG C under atmosphere protection, obtain carbonaceous product；2200 under normal pressure, inert atmosphere protection
DEG C carry out graphitization, obtain isotropic graphite material；Gained isotropic graphite material rupture strength is 92MPa, comprcssive strength
For 232MPa, bulk density is 1.78/cm3, isotropism degree is 1.02.
Embodiment 7
The high softening point bitumen that softening point is 315 DEG C is crushed to mean diameter 10 μm, with nitration mixture (nitric acid by 10% and 90%
Sulphuric acid forms for 2:1 in mass ratio) mix for 1:18 in mass ratio, aoxidize 20 minutes, obtain powdery primary raw materials.By above-mentioned powder
Shape primary raw materials, through compression molding, then carries out carbonization, constant temperature 1 hour at 900 DEG C under normal pressure, inert atmosphere protection, obtains
Carbonaceous product；Under normal pressure, inert atmosphere protection, carry out graphitization at 2500 DEG C, obtain isotropic graphite material；Gained respectively to
Same sex graphite material rupture strength is 89MPa, and comprcssive strength is 216MPa, and bulk density is 1.77g/cm3, isotropism degree is
1.03。
Embodiment 8
The high softening point bitumen that softening point is 330 DEG C is crushed to mean diameter 25 μm, with 10% nitric acid be 1:20 in mass ratio
Mixing, aoxidizes 40 minutes, obtains powdery primary raw materials.By above-mentioned powdery primary raw materials through compression molding, then in normal pressure, inertia
Carry out carbonization, constant temperature 1 hour at 800 DEG C under atmosphere protection, obtain carbonaceous product；2600 under normal pressure, inert atmosphere protection
DEG C carry out graphitization, obtain isotropic graphite material；Gained isotropic graphite material rupture strength is 69MPa, comprcssive strength
For 165MPa, bulk density is 1.69g/cm3, isotropism degree is 1.06.
Each embodiment material property parameter is as shown in the table:
| Embodiment | Rupture strength (MPa) | Comprcssive strength (MPa) | Bulk density (g/cm<sup>3</sup>) | Isotropism degree |
| Embodiment 1 | 35 | 90 | 1.60 | 1.07 |
| Embodiment 2 | 45 | 120 | 1.63 | 1.05 |
| Embodiment 3 | 81 | 201 | 1.75 | 1.03 |
| Embodiment 4 | 100 | 250 | 1.8 | 1.02 |
| Embodiment 5 | 95 | 244 | 1.79 | 1.02 |
| Embodiment 6 | 92 | 232 | 1.78 | 1.02 |
| Embodiment 7 | 89 | 216 | 1.77 | 1.03 |
| Embodiment 8 | 69 | 165 | 1.69 | 1.06 |
The specific embodiment of the present invention is not construed as limiting the invention, the analog structure of every employing present invention and change, all
Within the scope of the present invention.
Claims (8)
1. the method preparing isotropic graphite material from sintering, it is characterised in that: it comprises the steps: 1. will soften
Point is at 200-330 DEG C, and it is 5-30 μm that the high softening point bitumen between mesophase content ＜ 0.1%wt is crushed to particle diameter, obtains asphalt powder
Material；2. by above-mentioned steps 1. in prepare Colophonium powder mix according to the mass ratio of 1:5-1:20 with Oxygen in Liquid agent after put into liquid
Body oxidant carries out oxidation processes, obtains powdery primary raw materials；3. by above-mentioned steps 2. in prepare powdery primary raw materials become
Type is processed, and obtains moulding material；4. by above-mentioned steps 3. in prepare moulding material be heated under normal pressure, nonoxidizing atmosphere
800-1000 DEG C, obtain carbonaceous product；5. by above-mentioned steps 4. in prepare carbonaceous product heat under normal pressure, nonoxidizing atmosphere
To 2200-2800 DEG C, obtain isotropic graphite material.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
Step 2. middle oxidation treatment time is 10-50min.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
Step 2. in liquid oxidizer be mass concentration be the salpeter solution of 10-30%, the sulfuric acid solution of 70-90% or the nitric acid of 10-30%
Any one in the mixed acid solution being mixed for 1:3-2:1 in mass ratio with the sulphuric acid of 70-90%.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
Step 2. in carry out the degree of oxidation processes for making Colophonium powder the most fully crosslinked, also there is certain softening special after heating
Property, its fugitive constituent is at 10-12%wt, and described fugitive constituent plays binding agent effect in carbonization process.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
3. step is shaped processing and uses any one in compression molding, vibration moulding or isostatic pressing.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
Step 4. middle nonoxidizing atmosphere is under inert gas shielding or method isolation air buried by coke powder.
A kind of method preparing isotropic graphite material from sintering, it is characterised in that: described
Step 5. middle nonoxidizing atmosphere is under inert gas shielding or method isolation air buried by coke powder.
8. a kind of method preparing isotropic graphite material from sintering as described in any one of claim 1-7, its feature exists
In: the isotropic graphite material that described method prepares, its rupture strength is 35-100MPa, and comprcssive strength is 90-
250MPa, bulk density is 1.6-1.8g/cm3, isotropism degree is 1.02-1.07.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675292A (en) * | 2018-07-20 | 2018-10-19 | 济宁碳素集团有限公司 | The method that combination method prepares isotropic graphite material |
| CN109503169A (en) * | 2018-12-24 | 2019-03-22 | 成都阿泰克特种石墨有限公司 | A kind of special graphite and preparation method thereof |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
| CN114163236A (en) * | 2021-12-14 | 2022-03-11 | 中钢集团南京新材料研究院有限公司 | Method for improving isotropy of graphite |
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| CN1156123A (en) * | 1996-02-02 | 1997-08-06 | 中国科学院山西煤炭化学研究所 | Method for improving non-melting process of asphalt balls |
| CN104876581A (en) * | 2015-05-14 | 2015-09-02 | 湖南省长宇新型炭材料有限公司 | Preparation method of low-resistivity isotropic graphite |
| CN105645960A (en) * | 2015-12-11 | 2016-06-08 | 天津工业大学 | Method for preparing isotropic graphite from isotropic asphalt with high softening point through self-sintering |
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2016
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| CN1156123A (en) * | 1996-02-02 | 1997-08-06 | 中国科学院山西煤炭化学研究所 | Method for improving non-melting process of asphalt balls |
| CN104876581A (en) * | 2015-05-14 | 2015-09-02 | 湖南省长宇新型炭材料有限公司 | Preparation method of low-resistivity isotropic graphite |
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| E. VILAPLANA-ORTEGO等: "Stabilisation of low softening point petroleum pitch fibres by HNO3", 《CARBON》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108675292A (en) * | 2018-07-20 | 2018-10-19 | 济宁碳素集团有限公司 | The method that combination method prepares isotropic graphite material |
| CN109503169A (en) * | 2018-12-24 | 2019-03-22 | 成都阿泰克特种石墨有限公司 | A kind of special graphite and preparation method thereof |
| CN110655413A (en) * | 2019-09-18 | 2020-01-07 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
| CN110655413B (en) * | 2019-09-18 | 2022-03-04 | 济宁碳素集团有限公司 | Preparation method of isotropic graphite material |
| CN114163236A (en) * | 2021-12-14 | 2022-03-11 | 中钢集团南京新材料研究院有限公司 | Method for improving isotropy of graphite |
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Effective date of registration: 20180508 Address after: No. 99, Ren Cheng Avenue, Jining, Shandong Province, Shandong Applicant after: Jining Carbon Group Co., Ltd. Applicant after: JINING KENON NEW CARBON MATERIALS TECHNOLOGY CO., LTD. Address before: 272000 the 105 National Road East of the village of Jiang Miao village, twenty Mile Shop, Rencheng District, Jining, Shandong Applicant before: Shandong Chenyang New Carbon Material Co., Ltd. |
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Application publication date: 20161109 |