CN101691300B - Large-size medium-grained graphite material and production process thereof - Google Patents
Large-size medium-grained graphite material and production process thereof Download PDFInfo
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- CN101691300B CN101691300B CN 200910179699 CN200910179699A CN101691300B CN 101691300 B CN101691300 B CN 101691300B CN 200910179699 CN200910179699 CN 200910179699 CN 200910179699 A CN200910179699 A CN 200910179699A CN 101691300 B CN101691300 B CN 101691300B
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- graphite material
- petroleum coke
- siccative
- binding agent
- roasting
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Abstract
The invention discloses a large-size medium grain graphite material and a production process thereof. The production process comprises the following steps: smashing a raw material; adding an adhesive when the ingredient and the adhesive are subjected to dry-mixing to a certain temperature; and carrying out processes of kneading, cooling, moulding, roasting, impregnating, re-roasting or re-impregnating, re-roasting and graphitizing to prepare the large-size medium grain graphite material. The large-size medium grain graphite material has the advantage that: the graphite material produced by the production process has large size, uniform structure and small pore and is suitable for a large casting die, polysilicon smelting, large blast furnace brickwork and a chemical smelting launder, solves the problems of low efficiency and high production cost caused by small size and multi-block assembling, and also solves the problems of big pore and high permeability caused by coarse grain.
Description
Technical field:
The present invention relates to a kind of graphite material and production technique thereof, relate to especially that massive casting mould, polysilicon are smelted, large blast furnace is built by laying bricks or stones, chemical industry is smelted chute, heat exchanger with big size medium grain graphite material and production technique thereof.
Technical background:
The particle that its specification of existing graphite material is little, specification is big, for being to adopt assembly unit with large-scale graphite material, it installs inconvenient, and efficient is low, and consumption is high and big owing to pore during production, seepage is serious, thereby causes the production cost height.
Summary of the invention
The object of the present invention is to provide and be applicable to the machining large casting mould, polysilicon is smelted, large blast furnace is built by laying bricks or stones, chemical industry is smelted graphite materials such as chute, heat exchanger, without the polylith assembly unit, easy to use, high efficiency, even structure, pore are little, thereby reach a kind of graphite material of the purpose that reduces production costs.
Another object of the present invention is to provide and is applicable to that machining large casting mould, polysilicon are smelted, large blast furnace is built by laying bricks or stones, chemical industry is smelted graphite materials such as chute, heat exchanger, without the polylith assembly unit, easy to use, high efficiency, even structure, pore are little, thereby reach the production technique of a kind of graphite material of the purpose that reduces production costs.
First purpose of the present invention is implemented by following technical scheme: big specification, middle coarse-grained graphite material, it includes raw material through broken, batching and binding agent through overdrying mix that certain temperature adds that the binding agent warp is mixedly pinched, cool material, moulding, roasting, dipping, roasting or dipping, roasting again, graphitization technique make again again, its weight part: siccative comprises forges burnt 100 parts of back, adds 18-28 part binding agent.
Another object of the present invention is implemented by following technical scheme: it comprises that to forge the back burnt through the fragmentation screening, mix with binding agent through batching pinch, cool material, moulding, roasting, dipping, again roasting or again dipping, again roasting after greying process.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 20-40%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 20-40%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 25-45%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 25-40 minute mixed pinching, temperature reaches 110 ℃-125 ℃, mixed the pinching 45-65 minute of binding agent that adds 135 ℃-165 ℃, wherein by weight, as the binding agent that 1. described per 100 parts of siccatives add 18-28 part, drop temperature is at 145 ℃-165 ℃, by cold material, compression moulding;
(2) sinter process:
The product of compression moulding is packed in the stoving oven, under the situation of airtight air-isolation, the stampings of (1) gained were heated to 1200 ℃-1250 ℃ through 450-800 hour obtain baked article;
(3) impregnation technology:
Baked article is preheating to 260-360 ℃, is no less than 12 hours warm up time, flood in the high-pressure impregnation jar of packing into, vacuumize pressurization, moulding pressure 10-15kg/cm
2, 4-8 hour clamping time;
(4) sinter process again:
Impregnated goods are carried out roasting again as described in step (2);
(5) graphitization technique:
Goods after the roasting are again packed in the graphitizing furnace, and greying is carried out in energising under airtight situation, makes goods through 100-180 hour, and temperature reaches 2500-3000 ℃ and promptly gets graphite material.
Described binding agent can be medium temperature coal pitch or transformation of the way pitch;
Described compression moulding comprises extrusion molding and vibratory compaction.
The gained baked article can carry out double-steeping as required and three roastings obtain roasting product.
The big size medium grain graphite material that makes according to above-mentioned technology.
Advantage of the present invention is: by the graphite material of this explained hereafter, its specification is big, even structure, little being suitable for of pore are made the massive casting mould, polysilicon is smelted, large blast furnace is built by laying bricks or stones, chemical industry is smelted chute, solved the characteristic that efficient is low, production cost is high that causes because of the little polylith assembly unit of specification, also solved because of particle and slightly caused the characteristic that pore is big, rate of permeation is high.
Embodiment:
Embodiment 1: big specification, middle coarse-grained graphite material, comprise siccative and binding agent through in broken, batching, mixedly pinch, cool material, compression moulding, sinter process, impregnation technology, sinter process or impregnation technology and sinter process and graphitization technique etc. make again more again.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 27%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 40%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 33%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 25 minutes mixed pinching, temperature reaches 110 ℃, mixed the pinching 65 minutes of binding agent that adds 165 ℃, wherein by weight, add 18 parts binding agent as 1. described per 100 parts of siccatives, drop temperature is at 165 ℃, by cold material, compression moulding, specification is 3800mm * 1050mm * 600mm.
(2) sinter process:
The product of compression moulding is packed in the stoving oven, under the situation of airtight air-isolation, the stampings of (1) gained were heated to 1200 ℃ through 450 hours obtain baked article;
(3) impregnation technology:
Baked article is preheating to 320 ℃, is no less than 12 hours warm up time, flood in the high-pressure impregnation jar of packing into, wherein the pumpdown time is no less than 45 minutes, and vacuum tightness is not less than-0.086MPa; Moulding pressure 15kg/cm
2, 4 hours clamping times;
(4) sinter process again:
Impregnated goods are carried out roasting again as described in step (2);
(5) graphitization technique:
Goods after the roasting are again packed in the graphitizing furnace, and greying is carried out in energising under airtight situation, makes goods through 100 hours, and temperature reaches 2500 ℃ and promptly gets graphite material.
Embodiment 2: big size medium grain graphite material, comprise siccative and binding agent through in broken, batching, mixedly pinch, cool material, compression moulding, sinter process, impregnation technology, sinter process or impregnation technology and sinter process and graphitization technique etc. make again more again.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 20%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 35%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 45%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 30 minutes mixed pinching, temperature reaches 112 ℃, mixed the pinching 55 minutes of binding agent that adds 140 ℃, wherein by weight, add 25 parts binding agent as 1. described per 100 parts of siccatives, drop temperature is at 158 ℃, by cold material, compression moulding, specification is 3500mm * 1050mm * 600mm.
(2) sinter process:
The product of die mould product 3500 * 1050 * 600mm is packed in the stoving oven, airtight situation following (1) the die mould product reach 1250 ℃ through roasting in 800 hours and obtain baked article;
(3) impregnation technology:
To be preheating to 300 ℃ of warm up times be 13 hours at the dipping preheating chamber with roasting product, floods in the high-pressure impregnation jar of packing into, and the pumpdown time is 50 minutes, and vacuum tightness reaches-and the 0.086MPa moulding pressure is 13kg/cm
2, reach 5 hours clamping time and then obtained pickled product.
(4) sinter process again: impregnated goods are carried out roasting as described in (2).
(5) graphitization technique: the goods after the roasting are packed in the graphitizing furnace, switched under airtight situation 154 hours, temperature reaches 2800 ℃ and promptly gets graphite material.
Embodiment 3: big specification, middle coarse-grained graphite material, comprise siccative and binding agent through in broken, batching, mixedly pinch, cool material, compression moulding, sinter process, impregnation technology, sinter process or impregnation technology and sinter process and graphitization technique etc. make again more again.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 40%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 35%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 25%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 35 minutes mixed pinching, temperature reaches 120 ℃, mixed the pinching 45 minutes of binding agent that adds 135 ℃, wherein by weight, add 22 parts binding agent as 1. described per 100 parts of siccatives, drop temperature is at 145 ℃, by cold material, compression moulding, specification is 3500mm * 1050mm * 600mm.
(2) sinter process:
The product of compression moulding is packed in the stoving oven, under the situation of airtight air-isolation, the stampings of (1) gained were heated to 1230 ℃ through 620 hours obtain baked article;
(3) impregnation technology:
Baked article is preheating to 360 ℃, is no less than 12 hours warm up time, flood in the high-pressure impregnation jar of packing into, wherein the pumpdown time is no less than 45 minutes, and vacuum tightness is not less than-0.086MPa; Moulding pressure 10kg/cm
2, 8 hours clamping times;
(4) sinter process again:
Impregnated goods are carried out roasting again as described in step (2);
(5) graphitization technique:
Goods after the roasting are again packed in the graphitizing furnace, and greying is carried out in energising under airtight situation, makes goods through 180 hours, and temperature reaches 3000 ℃ and promptly gets graphite material.
Embodiment 4: big specification, middle coarse-grained graphite material, comprise siccative and binding agent through in broken, batching, mixedly pinch, cool material, compression moulding, sinter process, impregnation technology, sinter process or impregnation technology and sinter process and graphitization technique etc. make again more again.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 38%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 20%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 42%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 40 minutes mixed pinching, temperature reaches 125 ℃, mixed the pinching 50 minutes of binding agent that adds 150 ℃, wherein by weight, add 24 parts binding agent as 1. described per 100 parts of siccatives, drop temperature is at 150 ℃, by cold material, compression moulding, specification is 3500mm * 1050mm * 600mm.
(2) sinter process:
The product of die mould product 3500mm * 1050mm * 600mm is packed in the stoving oven, airtight situation following (1) the die mould product reach 1200 ℃ through roasting in 550 hours and obtain roasting product.
(3) impregnation technology:
To be preheating to 260 ℃ of warm up times be 12 hours at the dipping preheating chamber with roasting product, floods in the high-pressure impregnation jar of packing into, and the pumpdown time is 45 minutes, and vacuum tightness reaches-and the 0.086MPa moulding pressure is 11kg/cm
2, reach 7 hours clamping time and then obtained pickled product.
(4) sinter process again: impregnated goods are carried out roasting as described in (2).
(5) graphitization technique: the goods after the roasting are packed in the graphitizing furnace, switched under airtight situation 140 hours, temperature reaches 2700 ℃ and promptly gets graphite material.
Embodiment 5: big specification, middle coarse-grained graphite material, comprise siccative and binding agent through in broken, batching, mixedly pinch, cool material, compression moulding, sinter process, impregnation technology, sinter process or impregnation technology and sinter process and graphitization technique etc. make again more again.
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 32%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 28%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 40%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, did in the pot mixed 33 minutes mixed pinching, temperature reaches 116 ℃, mixed the pinching 58 minutes of binding agent that adds 145 ℃, wherein by weight, add 28 parts binding agent as 1. described per 100 parts of siccatives, drop temperature is at 162 ℃, by cold material, compression moulding, specification is 3500mm * 1050mm * 600mm.
(2) sinter process:
The product of die mould product 3500mm * 1050mm * 600mm is packed in the stoving oven, airtight situation following (1) the die mould product reach 1240 ℃ through roasting in 700 hours and obtain roasting product.
(3) impregnation technology:
To be preheating to 280 ℃ of warm up times be 14 hours at the dipping preheating chamber with roasting product, floods in the high-pressure impregnation cylinder of packing into, and the pumpdown time is 48 minutes, and vacuum tightness reaches-and the 0.086MPa moulding pressure is 14kg/cm
2, reach 5.5 hours clamping time and then obtained pickled product.
(4) sinter process again: impregnated goods are carried out roasting as described in (2).
(5) graphitization technique: the goods after the roasting are packed in the graphitizing furnace, switched under airtight situation 160 hours, temperature reaches 2850 ℃ and promptly gets graphite material.
Claims (3)
1. the production technique of a big size medium grain graphite material is characterized in that comprising the steps:
(1) siccative and binding agent mix pinch, cool material, compression moulding:
1. the preparation of after-smithing petroleum coke siccative: get broken back and be following varigrained after-smithing petroleum coke preparation after-smithing petroleum coke siccative: wherein by weight percentage: granularity is that the after-smithing petroleum coke of 1.0-0.5mm is 20-40%; Granularity is that the after-smithing petroleum coke of 0.5-0.15mm is 20-40%; Granularity is that the following after-smithing petroleum coke of 0.15mm is 25-45%;
2. siccative and binding agent mix and pinch: the siccative that will 1. be prepared, mix to 110 ℃-125 ℃ mixing to pinch to do in the pot, add 135 ℃-165 ℃ mixed the pinching of binding agent, wherein by weight, the binding agent that adds 18-28 part as 1. described per 100 parts of siccatives is by cold material, compression moulding; Described compression moulding comprises extrusion molding and vibratory compaction;
(2) sinter process:
The product of compression moulding is packed in the stoving oven, under the situation of airtight air-isolation, the stampings of (1) gained were heated to 1200 ℃-1250 ℃ through 450-800 hour obtain baked article;
(3) impregnation technology:
Baked article is preheating to 260-360 ℃, is no less than 12 hours warm up time, flood in the high-pressure impregnation jar of packing into, vacuumize pressurization, 4-8 hour clamping time;
(4) sinter process again:
Impregnated goods are carried out roasting again as described in step (2);
(5) graphitization technique:
Goods after the roasting are again packed in the graphitizing furnace, and greying is carried out in energising under airtight situation, makes goods through 100-180 hour, and temperature reaches 2500-3000 ℃ and promptly gets graphite material.
2. the production technique of a kind of big size medium grain graphite material according to claim 1 is characterized in that described binding agent is medium temperature coal pitch or transformation of the way pitch.
3. the production technique of a kind of big size medium grain graphite material according to claim 1 is characterized in that the gained baked article can be carried out double-steeping as required and three roastings obtain roasting product.
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| CN 200910179699 CN101691300B (en) | 2009-10-20 | 2009-10-20 | Large-size medium-grained graphite material and production process thereof |
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| CN101691300B true CN101691300B (en) | 2013-07-31 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101948675B (en) * | 2010-08-26 | 2011-08-31 | 大同市新成特炭有限公司 | Heat accumulation and energy storage graphite material for solar thermal power generation and preparation method thereof |
| CN101985760B (en) * | 2010-10-29 | 2013-02-13 | 万基控股集团石墨制品有限公司 | Components of graphitized anode and preparation method thereof |
| CN102249237B (en) * | 2010-12-20 | 2013-06-05 | 福建兴朝阳硅材料股份有限公司 | Graphite crucible |
| CN102502603B (en) * | 2011-11-01 | 2013-04-17 | 雅安恒圣高纯石墨科技有限责任公司 | Production process of large isotropic and isostatic high purity graphite with fine particles |
| CN104150467B (en) * | 2014-07-08 | 2016-05-18 | 大同新成新材料股份有限公司 | A kind of graphite material for train cast steel wheel casting mould and preparation method thereof |
| CN104828809A (en) * | 2015-04-23 | 2015-08-12 | 成都蓉光炭素股份有限公司 | Processing method for extrusion molded medium size structure graphite material |
| CN108448131B (en) * | 2018-03-14 | 2020-11-13 | 安徽锦美碳材科技发展有限公司 | Processing method of fuel cell composite material bipolar plate |
| CN109852081B (en) * | 2018-12-20 | 2021-07-30 | 淄博大陆石墨科技有限公司 | Preparation method of paste homogenization for special graphite by vibration-compression molding |
| CN109865815B (en) * | 2019-03-12 | 2021-03-16 | 泗阳敏于行精密机械有限公司 | Manufacturing method of graphite shunt cone used in aluminum hub die-casting process |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357761A (en) * | 2008-09-09 | 2009-02-04 | 河南天利碳素材料有限公司 | High pure graphitic profile and preparation technique thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101357761A (en) * | 2008-09-09 | 2009-02-04 | 河南天利碳素材料有限公司 | High pure graphitic profile and preparation technique thereof |
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