CN102249212A - Pressurization roasting method for carbon - Google Patents
Pressurization roasting method for carbon Download PDFInfo
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- CN102249212A CN102249212A CN2010105975194A CN201010597519A CN102249212A CN 102249212 A CN102249212 A CN 102249212A CN 2010105975194 A CN2010105975194 A CN 2010105975194A CN 201010597519 A CN201010597519 A CN 201010597519A CN 102249212 A CN102249212 A CN 102249212A
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- sintering method
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Abstract
The invention provides a pressurization roasting method for carbon, and relates to a carbon roasting process. The pressurization roasting method for the carbon can avoid shell wastes, reduce the crack wastes caused by temperature difference and shorten the roasting time. The method comprises the following steps of: placing a compression green body product in a saggar, and filling a filler between the product and the saggar; and after the product is filled in the saggar, sealing and vacuumizing, inflating nitrogen, placing in a roasting furnace, and heating, wherein the pressure is kept 2.5 to 1.5 MPa, and when the pressure exceeds an upper limit, the pressure can be released through a valve and the valve is closed when the pressure is close to the lower limit. By using the anaerobic state, the shell wastes are avoided. By using the saggar, the periphery of the product is heated uniformly, the temperature difference among positions of the product can be reduced and the crack wastes caused by the temperature difference are reduced. An 804-hour roasting curve is performed for roasting and the roasting time can be reduced by about 12 percent. Through experiment, under the same condition, compared with the conventional carbon roasting method, the pressurization roasting method can obviously improve the product yield, coking rate, volume density and recovery yield.
Description
Technical field
The present invention relates to a kind of carbon baking technology, especially relate to a kind of carbon element hot pressure sintering method.
Background technology
Roasting is the critical process that carbon element is produced.Calcining process is that the carbon element green compact are contained in the stoving oven, carries out pyroprocessing under the protection of stopping composition, makes the pitch carbonization in the green compact.Coal-tar pitch at high temperature, light ends is got rid of volatilization, the rest part coking combines coke granule and fine powder securely, makes carbon element green compact after the roasting have higher physical strength, lower resistance, thermostability and chemical stability preferably.
Chinese patent CN101654239 discloses a kind of isotropic graphite goods and preparation method thereof, its raw material comprises binding agent and aggregate, purified natural micro crystal graphite accounts for 30%～100% of aggregate quality, and its clout is at least a in graphite returns, pitch coke, refinery coke, secondary Jiao and the carbonaceous mesophase spherules; Its preparation method is by binding agent and aggregate are mixed, and again through overmolding, carries out roasting then, through dipping and re-baking, carries out the step of graphitization processing at last and finishes again.
Chinese patent CN1505549 discloses a kind of invention and relates to the various metal alloys of fusion such as nickel, cobalt and/or iron-based superalloy, Stainless Steel Alloy, titanium alloy and Ti-Al alloy in vacuum or low pressure inert atmosphere, in vacuum or low pressure inert atmosphere melt is molded into the manufacturing process that graphite jig is shaped to engineering element afterwards.
Chinese patent CN101348587 discloses a kind of preparation method of ultra-high molecular weight polyethylene/graphite nanoplate matrix material, 1) be ultrahigh molecular weight polyethylene(UHMWPE) 85%～99% by the shared mass percent of each raw material, graphite 1%～15% has been measured ultrahigh molecular weight polyethylene(UHMWPE) and graphite raw material is standby; 2) add in the grinding pot, in the ratio adding coupling agent of graphite quality 0.5%～1.5%; Add mill ball according to 1: 1～6: 1 ratio of grinding media to material; 3) ball grinder is installed to ball milling on the ball mill; 4) ball milling is good dry materials gets masterbatch; 5) masterbatch is used the hot-press molding method moulding, got the ultra-high molecular weight polyethylene/graphite nanoplate matrix material.
The characteristics of calcining process: goods heat temperature raising curve is long; The energy consumption height; Very easily crack waste product, even the goods cracking, qualification rate is low.Its quality is bigger to the next procedure influence, has determined the casting yield that carbon product is produced, and directly influences product cost.
The roasting curve is meant that stoving oven is heated to the speed and the time of 1250 ℃ intensification from room temperature.The roasting curve of general goods is more than 140～800 hours, indivedual goods even reach thousands of hours.With the increase of goods physical dimension, goods granule material is more little, and the roasting curve is long more.Thereby avoid baked article to crack, shorten curve, be the major measure that cuts down the consumption of energy, improves output, reduces cost.With φ 850 * 700mm (fine particle goods), the granularity of prescription is an example less than 100 purpose goods, carries out the 912h curve, and qualification rate only is 25%, and all the other 75% are the crackle waste product all, burns till afterwards volume density and has only 1.45g/cm
3
Chinese patent CN1061209 discloses a kind of carbon materials goods---metallurgical manufacture method with the earthenware snail, by special metal die, made-up article in its die cavity is exerted pressure, utilize the external heat source heating to finish hot pressure sintering technology, can shorten the production cycle, improve the quality of products, reduce production costs, if directly use carbon raw, promptly thickener or powder serve as above-mentioned made-up article, compression molding and hot pressure sintering once can be finished.
Summary of the invention
The object of the present invention is to provide a kind of duricrust waste product of avoiding producing, reduce the crackle waste product that causes because of the temperature difference, shorten the carbon element hot pressure sintering method of roasting time.
Carbon element hot pressure sintering method of the present invention adopts the traditional carbon ring-form calcining furnace.
Carbon element hot pressure sintering method of the present invention may further comprise the steps:
1) the die mould green article is placed saggar, add stopping composition between goods and the saggar;
In step 1), described saggar can adopt the stainless steel saggar; Top at saggar can be provided with outside seamless tube and the through furnace, extends on the outer seamless tube of stove vacuum pressure gauge, valve are installed successively; The alms bowl wall of described saggar and the distance of goods are not less than 100mm; Described stopping composition can adopt calcined petroleum coke, and the granularity of described stopping composition can be 6～2mm.
2) seal behind the saggar dress goods, vacuumize, fill then with nitrogen;
In step 2) in, the described vacuum tightness that vacuumizes can be less than-0.093MPa, can keep 40min after, fill with nitrogen, nitrogen gas pressure can be 1.5MPa.
3) saggar is placed in the stoving oven, heat temperature raising is regulated the saggar pressure inside and is maintained 2.5～1.5MPa, when pressure can pass through the valve pressure release in limited time above last, near the valve-off of prescribing a time limit down.
In step 3), described heat temperature raising can be by given heating curve heat temperature raising, and described heating curve can adopt 804h roasting curve (referring to table 1).
Table 1
Compare with the traditional carbon roasting method, the present invention has following outstanding advantage:
1) owing to adopted anaerobic state, therefore avoided the generation of duricrust waste product.
2) owing to adopt saggar, so the goods periphery is heated more evenly, reduced the temperature difference between each position of goods, significantly reduced the crackle waste product that causes because of the temperature difference.
3) carry out roasting owing to carry out 804 hours roasting curves, so roasting time can shorten about 12%.
Embodiment
Following examples will the present invention is further illustrated.
Following examples adopt the traditional carbon ring-form calcining furnace, and described carbon element hot pressure sintering method may further comprise the steps:
1) the die mould green article is placed saggar, add calcined petroleum coke between goods and the saggar, its granularity is 6～2mm; Described saggar adopts the stainless steel saggar; Outside the top of saggar is provided with seamless tube and through furnace, extends on the outer seamless tube of stove vacuum pressure gauge, valve are installed successively; The alms bowl wall of described saggar and the distance of goods are not less than 100mm.
2) seal behind the saggar dress goods, vacuumize, fill then with nitrogen; The described vacuum tightness that vacuumizes is less than-0.093MPa, keep 40min after, fill with nitrogen, nitrogen gas pressure is 1.5MPa.
3) saggar is placed in the stoving oven, heat temperature raising is regulated the saggar pressure inside and is maintained 2.5～1.5MPa, when pressure can pass through the valve pressure release in limited time above last, near the valve-off of prescribing a time limit down.Described heat temperature raising is by given heating curve heat temperature raising, and described heating curve can adopt 804h roasting curve (referring to table 1).
Through test, under similarity condition, the comparable traditional carbon roasting method of the present invention obviously improves product percent of pass, coking rate, volume density and casting yield, and its qualification rate can reach 95%, and coking rate can increase by 5%, and volume density can be 1.53g/cm
3, casting yield also improves 5%.
The quality of its molecule of quinoline insolubles is 1800～2600 (units of nucleidic mass) in roasting process, and granular size is the main component that pitch forms coke between 0.5～30 μ m.This part all is converted into coke at the roasting process of common stoving oven.
Toluene insolubles but it is dissolved in the component of quinoline, the quality of its molecule is less, between 1000～1800; Be dissolved in the component of toluene, its molecular weight is littler, is roughly 210～1000.In roasting process, because the less highly volatile of its molecule has reduced the bituminous coking rate.Under the high temperature of the two kinds of components in back in saggar, the highly compressed condition, again can polymerization reaction take place, the new quinoline insolubles of generating portion, it is also coking in roasting process, thereby has improved the bituminous coking rate.
Claims (8)
1. carbon element hot pressure sintering method is characterized in that may further comprise the steps:
1) the die mould green article is placed saggar, add stopping composition between goods and the saggar;
2) seal behind the saggar dress goods, vacuumize, fill then with nitrogen;
3) saggar is placed in the stoving oven, heat temperature raising is regulated the saggar pressure inside and is maintained 2.5～1.5MPa, when pressure is prescribed a time limit by the valve pressure release above last, near the valve-off of prescribing a time limit down.
2. carbon element hot pressure sintering method as claimed in claim 1 is characterized in that in step 1), and described saggar adopts the stainless steel saggar.
3. carbon element hot pressure sintering method as claimed in claim 1 or 2 is characterized in that in step 1), outside the top of saggar is provided with seamless tube and through furnace, extends on the outer seamless tube of stove vacuum pressure gauge, valve are installed successively.
4. carbon element hot pressure sintering method as claimed in claim 1 or 2 is characterized in that in step 1) the alms bowl wall of described saggar and the distance of goods are not less than 100mm.
5. carbon element hot pressure sintering method as claimed in claim 1 is characterized in that in step 1) described stopping composition is a calcined petroleum coke.
6. as claim 1 or 5 described carbon element hot pressure sintering methods, it is characterized in that in step 1) the granularity of described stopping composition is 6～2mm.
7. carbon element hot pressure sintering method as claimed in claim 1 is characterized in that in step 2) in, the described vacuum tightness that vacuumizes is less than-0.093MPa, keep 40min after, fill with nitrogen, nitrogen gas pressure is 1.5MPa.
8. carbon element hot pressure sintering method as claimed in claim 1 is characterized in that in step 3), and described heat temperature raising is by given heating curve heat temperature raising, and described heating curve adopts 804h roasting curve as follows:
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201010597519 CN102249212B (en) | 2010-12-20 | 2010-12-20 | Pressurization roasting method for carbon |
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| CN 201010597519 CN102249212B (en) | 2010-12-20 | 2010-12-20 | Pressurization roasting method for carbon |
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| CN102249212B CN102249212B (en) | 2013-02-20 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795620A (en) * | 2012-09-07 | 2012-11-28 | 宝丰县五星石墨有限公司 | Compression roasting furnace for producing high-purity graphite |
| CN109809386A (en) * | 2019-04-02 | 2019-05-28 | 四川启明星铝业有限责任公司 | The method that ring-form calcining furnace is used for lithium cell cathode material carbonation process |
| CN112745123A (en) * | 2021-01-25 | 2021-05-04 | 焦作钧菲津材科技有限公司 | Preparation method of carbon material |
| CN114015860A (en) * | 2021-10-11 | 2022-02-08 | 上海策立工程技术有限公司 | Method and system for controlling furnace temperature of double-heat-storage type heating furnace |
| CN117447204A (en) * | 2023-12-22 | 2024-01-26 | 成都中超碳素科技有限公司 | Preparation method of mechanical carbon material |
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| JPS6291412A (en) * | 1985-10-03 | 1987-04-25 | Tokai Carbon Co Ltd | Method for charging isotropic carbon molded body to baking furnace |
| CN85104678A (en) * | 1985-06-10 | 1987-08-19 | 沈阳铝镁设计研究院 | A kind of tunnel furnace to the carbon product re-baking behind bituminizing |
| JPH04160060A (en) * | 1990-10-22 | 1992-06-03 | Tokai Carbon Co Ltd | Burning method for molded carbon body |
| JP2007204283A (en) * | 2006-01-31 | 2007-08-16 | Sumitomo Bakelite Co Ltd | Carbon material and method for manufacturing the same |
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| CN85104678A (en) * | 1985-06-10 | 1987-08-19 | 沈阳铝镁设计研究院 | A kind of tunnel furnace to the carbon product re-baking behind bituminizing |
| JPS6291412A (en) * | 1985-10-03 | 1987-04-25 | Tokai Carbon Co Ltd | Method for charging isotropic carbon molded body to baking furnace |
| JPH04160060A (en) * | 1990-10-22 | 1992-06-03 | Tokai Carbon Co Ltd | Burning method for molded carbon body |
| JP2007204283A (en) * | 2006-01-31 | 2007-08-16 | Sumitomo Bakelite Co Ltd | Carbon material and method for manufacturing the same |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102795620A (en) * | 2012-09-07 | 2012-11-28 | 宝丰县五星石墨有限公司 | Compression roasting furnace for producing high-purity graphite |
| CN109809386A (en) * | 2019-04-02 | 2019-05-28 | 四川启明星铝业有限责任公司 | The method that ring-form calcining furnace is used for lithium cell cathode material carbonation process |
| CN112745123A (en) * | 2021-01-25 | 2021-05-04 | 焦作钧菲津材科技有限公司 | Preparation method of carbon material |
| CN114015860A (en) * | 2021-10-11 | 2022-02-08 | 上海策立工程技术有限公司 | Method and system for controlling furnace temperature of double-heat-storage type heating furnace |
| CN114015860B (en) * | 2021-10-11 | 2024-01-02 | 上海策立工程技术有限公司 | Method and system for controlling furnace temperature of double heat accumulating type heating furnace |
| CN117447204A (en) * | 2023-12-22 | 2024-01-26 | 成都中超碳素科技有限公司 | Preparation method of mechanical carbon material |
| CN117447204B (en) * | 2023-12-22 | 2024-03-15 | 成都中超碳素科技有限公司 | Preparation method of mechanical carbon material |
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| CN102249212B (en) | 2013-02-20 |
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Owner name: FUJIAN CHAOYANG SILICON MATERIALS CO., LTD. Free format text: FORMER OWNER: GONG BINGSHENG Effective date: 20111115 |
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Effective date of registration: 20111115 Address after: 364211 Nanyang Industrial Zone, Nanyang Town, Shanghang County, Longyan, Fujian Applicant after: FUJIAN XING THE ZHAOYANG SILICON MATERIALS Co.,Ltd. Address before: Nanyang town Longyan city Fujian province 364211 Ma Shanghang County Yang Dong River Road No. 1 Applicant before: Gong Bingsheng |
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