CN102718218A - Synthesis process method for green silicon carbide - Google Patents

Synthesis process method for green silicon carbide Download PDF

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Publication number
CN102718218A
CN102718218A CN2012101806393A CN201210180639A CN102718218A CN 102718218 A CN102718218 A CN 102718218A CN 2012101806393 A CN2012101806393 A CN 2012101806393A CN 201210180639 A CN201210180639 A CN 201210180639A CN 102718218 A CN102718218 A CN 102718218A
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silicon carbide
green silicon
refinery coke
synthetic
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CN102718218B (en
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孙福龙
赵建立
由远洪
白周义
焦松强
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Shihezi Fengtuo Silicon Material Science and Technology Co., Ltd.
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XINJIANG YUFENG PHOTOVOLTAIC MATERIAL TECHNOLOGY Co Ltd
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Abstract

The invention discloses a synthesis process method for green silicon carbide, which comprises procedures of material filling, smelting at constant power, cooling and discharging. The synthesis process method has the following points: when performing the synthesis at this time, filling the materials at a side baking area (12) and an upper baking area (13) used in the former synthesis to perform synthesis reaction; filling the baking material at a bottom baking area (11) used in the former synthesis to the side baking area (12) and the upper baking area (13) at this time to perform secondary baking. Compared with the prior art, the synthesis process method adopts the secondary baking and reaction process to effectively prevent raw material and the impurity generated in the baking process at the furnace bottom from directly entering into the next furnace reaction region, avoid the influence to the generation and color of the green silicon carbide, and synchronously replace the recycled insulating material. The method can not only improve the quality of the green silicon carbide, but also greatly reduce power consumption.

Description

The green silicon carbide synthetic process
Technical field
The present invention relates to a kind of green silicon carbide synthetic process method.
Background technology
When green silicon carbide is produced at present, particularly in synthesis technique, adopt synthetic furnace to produce; The burner hearth of its synthetic furnace is an elongated slot body, and the two ends of cell body are provided with electrode, the cell body between electrode therefrom around the mind-set according to being divided into combustion chamber district, reaction material district and roasting material district; The filling electrically conductive graphite in the combustion chamber district, the filling reaction material in the reaction material district, filling roasting material in the roasting material district; Reaction material district around the electrically conductive graphite is owing to the distance apart from electrically conductive graphite, and the difference of the temperature in actual production has been divided into resolver and reaction zone again; Being the resolver apart from the nearer zone of calcium carbide China ink promptly, is reaction zone apart from calcium carbide China ink reaction material district far away promptly.
In the present production, be with silica sand and refinery coke compound as roasting material, when a new round is synthetic, the used roasting material of the furnace bottom of a last stove is joined the reaction zone that epicycle is produced.
This furnace bottom compound behind the bakes to burn the article is directly dropped into the reaction zone situation, cause behind the bakes to burn the article green silicon carbide to generate and become chromatic effect bad.
Because silica sand and the petroleum coke mixtures material of heat preservation zone for recycling for a long time can not in time be discharged the interior impurity of reaction zone fully.Even discharge impurity also is the impurity level that continues to strengthen material in the heat preservation zone.And because more furnace bottom adopts refractory brick to pave and forms; The brickwork joint crack can be by clogged up with material behind the life-time service; Cause silica sand and refinery coke compound can not react or react not thorough each other fully, put into next stove reaction zone again after, also can cause green silicon carbide to generate and quality bad.
The silit formation reaction is a thermo-negative reaction, under high temperature (about 1800~2600 ℃) condition, carries out.Smelt (smelting duration was generally about 28 hours) under the duration with regard to same permanent power, certainly will need more thermal energy just can produce the higher green silicon carbide of quality.If things go on like this will cause the silit quality to descend, production cost strengthens, particularly ton power consumption aspect.
Summary of the invention
The purpose of this invention is to provide a kind of Sic content that can effectively prevent in the green silicon carbide reduces; Cause that the silicon carbide products quality is bad, impurity discharges that proportion is not enough, current consumption increases, and then improved silit quality and the green silicon carbide synthetic process method that reduces production costs greatly.
The present invention realizes through following technical scheme: comprise charge, permanent power smelting, cooling and discharging process flow; Is that axis is divided into electrically conductive graphite district (4) with the burner hearth in the synthetic furnace with the electrode of two ends burner; With electrically conductive graphite district (4) therefrom mind-set be divided into resolver (3), reaction zone (2) and roast area (1) outward successively; Said filling material process comprises: bottom in body of heater, and promptly end roast area (11) is packed the compound of refinery coke and silica sand into as roasting material, the upper area of its end roast area (11); Promptly descend the reaction material district to load the bottom reaction material; Put the dividing plate of feeding then, mark off side roast area (12), side reaction material district and electrically conductive graphite district (4), in each above-mentioned functional zone, load electrically conductive graphite, sidepiece reaction material and sidepiece roasting material; Remove the charging dividing plate afterwards; Load top reaction material and top roasting material at last on top successively, it is characterized in that: when epicycle is synthetic, at least in reaction zone (3) the filling front-wheel synthetic in used side roast area (12) and upward the material of roast area (13) carry out building-up reactions; With front-wheel synthetic in the roasting material of roast area of the used end (11) the side roast area (12) and the last roast area (13) that are filled into epicycle carry out re-baking.
As improvement, said silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.6~0.9 weight part refinery coke, YValue ( The Y value doesSilicon carbon ratio) ratio range is 1.42~1.50
Above-mentioned silica sand and refinery coke compound are preferably: silica sand: SiO 2Content>=99.3%, Al 2O 3Content≤0.3%, Fe 2O 3Content≤0.2%, CaO content≤0.1%, igloss content≤0.2%; Refinery coke: fixed carbon>=90%; Ash≤0.8%; Fugitive constituent≤7%; Sulfur≤1%.
Said silica sand and refinery coke compound granularity are preferably: quartz sand size requires to be preferably: ﹤ 2mm<1%, 2~4mm accounts for 20~25%, and ﹥ 4~8mm accounts for 65~70%, and ﹥ 8~10mm accounts for 5~15%.
The refinery coke granularity requirements is preferably :≤4mm, wherein≤and 2mm accounts for 65~75%, and ﹥ 2~4mm accounts for 25~35%.
Compared with prior art; The present invention adopts re-baking and reaction process, and material can be reacted to each other fully, and helps the discharge and the collection of impurity; After cooling, also be beneficial in the discharging process and collect the caked impurity of sintering, can prevent that impurity is (like Al in starting material and the furnace bottom roasting process 2O 3,MgO, CaO, Fe 2O 3, Nacl) directly enter into next stove reaction zone; Influence the generation and the quality of green silicon carbide, simultaneously also replace the insulation material that recycles for a long time, factors such as the many and ventilation property of impurity is bad are improved; The ton power consumption drops to 6600~7100kwh from 7500~8000kwh per ton; Not only improve the quality of green silicon carbide product, also saved the energy simultaneously, reduced production cost.
Description of drawings
The synoptic diagram that the burner hearth functional area was divided when Fig. 1 was material of the present invention filling.
Shown in the figure: 1 is roast area, and 11 is end roast area, and 12 is the side roast area, and 13 is last roast area, and 2 is reaction zone, and 3 is the resolver, and 4 is the electrically conductive graphite district, and 5 is body of heater.
Embodiment
Embodiment 1:With reference to Fig. 1, the synoptic diagram that the burner hearth functional area is divided when being material of the present invention filling.Is that the zone of axis is divided into electrically conductive graphite district 4 with the burner hearth in the synthetic furnace with the electrode of two ends burner; Therefrom be divided into resolver 3, reaction zone 2 and roast area 1 successively in the mind-set periphery with electrically conductive graphite district 4; Said roast area 1 is divided into end roast area 11, side roast area 12 and last roast area 13 again; After second takes turns production; Every filling material process of taking turns production is following: when epicycle is synthetic; Roast area 11 is packed virgin material into as roasting material the end of at, with front-wheel synthetic in used side roast area 12 and the material of going up roast area 13 be loaded in epicycle synthetic reaction zone 2 and the resolver 3, with front-wheel synthetic in the roasting material of roast area of the used end 11 side roast area 12 that is filled into epicycle carry out roasting with last roast area 13.
Embodiment 2:Compare with embodiment 1; The difference of present embodiment is: when epicycle is synthetic; With front-wheel synthetic in used side roast area 12 and the material of going up roast area 13 be loaded in the epicycle synthetic reaction zone 2 virgin material of then packing in the resolver 3 around the electrically conductive graphite district 4.
Embodiment 3:Compare with embodiment 1, the difference of present embodiment is: in the said virgin material preparation, silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.6~0.9 weight part refinery coke Described silica sand and refinery coke compound are: silica sand: SiO 2Content>=99.3%, Al 2O 3Content≤0.3%, Fe 2O 3Content≤0.2%, CaO content≤0.1%, igloss content≤0.2%; Refinery coke: fixed carbon>=90%; Ash≤0.8%; Fugitive constituent≤7%; Sulfur≤1%.
Embodiment 4:Compare with embodiment 1, the difference of present embodiment is: said quartz sand size requirement is: ﹤ 2mm's is that 0.5%, 2~4mm accounts for 25%, and ﹥ 4~8mm accounts for 65%, and ﹥ 8~10mm accounts for 9.5%.The refinery coke granularity requirements is: wherein≤2mm accounts for 70%, and ﹥ 2~4mm accounts for 30%.
Embodiment 5:Compare with embodiment 4, the difference of present embodiment is: quartz sand size is: 0.5%, 2~4mm of ﹤ 2mm accounts for 20%, and ﹥ 4~8mm accounts for 70%, and ﹥ 8~10mm accounts for 9.5%.The refinery coke granularity is :≤2mm accounts for 65%, and ﹥ 2~4mm accounts for 35%.
Embodiment 6:Compare with embodiment 4, the difference of present embodiment is: quartz sand size is: 2~4mm accounts for 25%, and ﹥ 4~8mm accounts for 70%, and ﹥ 8~10mm accounts for 5%.The refinery coke granularity is :≤2mm accounts for 75%, and ﹥ 2~4mm accounts for 25%.
Embodiment 7:Compare with embodiment 4, the difference of present embodiment is: quartz sand size is: 2~4mm accounts for 23%, and ﹥ 4~8mm accounts for 70%, and ﹥ 8~10mm accounts for 7%.The refinery coke granularity is :≤2mm accounts for 68%, and ﹥ 2~4mm accounts for 32%.
Embodiment 8:Compare with embodiment 3, the difference of present embodiment is: said silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.65 weight part refinery coke
Embodiment 9:Compare with embodiment 3, the difference of present embodiment is: in the said virgin material preparation, silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.85 weight part refinery coke
Embodiment 10:Compare with embodiment 3, the difference of present embodiment is: in the said virgin material preparation, silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.7 weight part refinery coke
Embodiment 11:Compare with embodiment 3, the difference of present embodiment is: in the said virgin material preparation, silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.8 weight part refinery coke
Embodiment 12:Compare with embodiment 3, the difference of present embodiment is: in the said virgin material preparation, silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.75 weight part refinery coke

Claims (5)

1. green silicon carbide synthetic process; Comprise charge, permanent power smelting, cooling and discharging process flow; Is that axis is divided into electrically conductive graphite district (4) with the burner hearth in the synthetic furnace with the electrode of two ends burner; With electrically conductive graphite district (4) therefrom mind-set be divided into resolver (3), reaction zone (2) and roast area (1) outward successively; It is characterized in that: when epicycle is synthetic, at least in reaction zone (3) the filling front-wheel synthetic in used side roast area (12) and upward the material of roast area (13) carry out building-up reactions; With front-wheel synthetic in the roasting material of roast area of the used end (11) the side roast area (12) and the last roast area (13) that are filled into epicycle carry out re-baking.
2. green silicon carbide synthetic process according to claim 1 is characterized in that: said silica sand and refinery coke hybrid reaction material proportioning are: 1 weight part silica sand adds 0.6~0.9 weight part refinery coke .
3. green silicon carbide synthetic process according to claim 1 and 2 is characterized in that: said silica sand and refinery coke compound are: silica sand: SiO 2Content>=99.3%, Al 2O 3Content≤0.3%, Fe 2O 3Content≤0.2%, CaO content≤0.1%, igloss content≤0.2%; Refinery coke: fixed carbon>=90%; Ash≤0.8%; Fugitive constituent≤7%; Sulfur≤1%.
4. green silicon carbide synthetic process according to claim 1 and 2 is characterized in that: said quartz sand size is: ﹤ 2mm<1%, 2~4mm accounts for 20~25%, and ﹥ 4~8mm accounts for 65~70%, and ﹥ 8~10mm accounts for 5~15%; Said refinery coke granularity is :≤4mm, wherein≤and 2mm accounts for 65~75%, and ﹥ 2~4mm accounts for 25~35%.
5. green silicon carbide synthetic process according to claim 3 is characterized in that: said quartz sand size is: ﹤ 2mm<1%, 2~4mm accounts for 20~25%, and ﹥ 4~8mm accounts for 65~70%, and ﹥ 8~10mm accounts for 5~15%; Said refinery coke granularity is :≤4mm, and wherein≤and 2mm accounts for 65~75%, and ﹥ 2~4mm accounts for 25~35%.
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103350999A (en) * 2013-07-24 2013-10-16 新疆益丰西部陶瓷材料科技有限公司 Green silicon carbide reaction mixture and synthetic technology and charging baffle plate finished by adopting same
CN103601193A (en) * 2013-11-29 2014-02-26 新疆益丰西部陶瓷材料科技有限公司 Brand new green silicon carbide material roasting synthesis method
CN104045085A (en) * 2014-02-14 2014-09-17 鸡西市兴中科技有限公司 Novel smelting composting method of vacuum temperature-control pressure-regulating silicon carbide smelting furnace
CN108658078A (en) * 2018-08-08 2018-10-16 宁夏和兴碳基材料有限公司 A kind of silicon carbide smelting technique
CN114149007A (en) * 2020-09-04 2022-03-08 中国科学院过程工程研究所 Preparation method of silicon carbide

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Publication number Priority date Publication date Assignee Title
CN1157808A (en) * 1996-12-24 1997-08-27 苏占忠 Method for producing silicon carbide by using electric resistance furnace
CN101691218A (en) * 2009-09-14 2010-04-07 通化宏信研磨材有限责任公司 Process for smelting macrocrystalline green silicon carbide

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Publication number Priority date Publication date Assignee Title
CN1157808A (en) * 1996-12-24 1997-08-27 苏占忠 Method for producing silicon carbide by using electric resistance furnace
CN101691218A (en) * 2009-09-14 2010-04-07 通化宏信研磨材有限责任公司 Process for smelting macrocrystalline green silicon carbide

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Title
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103350999A (en) * 2013-07-24 2013-10-16 新疆益丰西部陶瓷材料科技有限公司 Green silicon carbide reaction mixture and synthetic technology and charging baffle plate finished by adopting same
CN103601193A (en) * 2013-11-29 2014-02-26 新疆益丰西部陶瓷材料科技有限公司 Brand new green silicon carbide material roasting synthesis method
CN104045085A (en) * 2014-02-14 2014-09-17 鸡西市兴中科技有限公司 Novel smelting composting method of vacuum temperature-control pressure-regulating silicon carbide smelting furnace
CN108658078A (en) * 2018-08-08 2018-10-16 宁夏和兴碳基材料有限公司 A kind of silicon carbide smelting technique
CN108658078B (en) * 2018-08-08 2021-10-26 宁夏和兴碳基材料有限公司 Silicon carbide smelting process
CN114149007A (en) * 2020-09-04 2022-03-08 中国科学院过程工程研究所 Preparation method of silicon carbide

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