CN102424586A - Preparation method of SiC fireproof raw material powder - Google Patents
Preparation method of SiC fireproof raw material powder Download PDFInfo
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- CN102424586A CN102424586A CN2011102625333A CN201110262533A CN102424586A CN 102424586 A CN102424586 A CN 102424586A CN 2011102625333 A CN2011102625333 A CN 2011102625333A CN 201110262533 A CN201110262533 A CN 201110262533A CN 102424586 A CN102424586 A CN 102424586A
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Abstract
Belonging to the technical field of refractory material preparation, the invention relates to a preparation method of SiC fireproof raw material powder. The invention is characterized by subjecting a used silica brick to carbothermic reduction by powdered coke or carbon black under a proper high temperature environment so as to prepare an SiC high temperature resistant raw material, and then conducting fragmentation, crushing, milling and other processes for preparing the Sic fireproof raw material powder, which mainly serves as an Sic fireproof material for preparing kiln furniture, blast furnace bodies, foundry ladle liners, non-ferrous metal smelting crucibles, wear resistant liners, and other fireproof products. The SiC fireproof raw material powder prepared by the invention mainly comprises the components of: beta-SiC, a small amount of C, cristobalite and trace ferrosilicon. The new method for preparing the SiC fireproof raw material powder involved in the invention has the characteristics of simple equipment, low cost and low energy consumption during preparation, thus providing a new technical approach for high efficiency value-added utilization of used silica bricks, and providing a new idea for reducing the production cost of fireproof materials and the metallurgy industry. The method of the invention also has the obvious advantages of environment protection, energy saving and emission reduction, etc.
Description
Technical field:
The present invention relates to a kind of novel method of the SiC of preparation refractory raw material; The powder of this SiC refractory raw material is mainly used in the starting material of refractory products such as preparation kiln furnitures, blast furnace and hot metal ladle liner, non-ferrous metal metallurgy crucible, wear-resistant liner, belongs to the refractory materials preparing technical field.
Background technology:
Since the reform and opening-up, the Iron And Steel Industry of China development is very fast, and crude steel output is from about 100,000,000 tons of about 3,700 ten thousand tons of surges to 1996 in 1980 year, and 2010, Chinese crude steel output will reach 6.27 hundred million tons.Refractory materials development meanwhile is very rapid, and national refractory materials output was 2808.06 ten thousand tons in 2010.Wherein: 1698.92 ten thousand tons of fine and close shaping refractory products; 1044.74 ten thousand tons of unsetting refractory products.Meanwhile, China's refractory materials output increases sharply in recent years, and quality and premium quality product aspect also develop very fast.2010,2808.06 ten thousand tons of national refractory materials output.Wherein: 1698.92 ten thousand tons of fine and close shaping refractory products; 1044.74 ten thousand tons of unsetting refractory products.Mainly adopted following two strategic measures: the advanced production line (technology and equipment) of critical product is made in (1) from external introduction; (2) tissue tackling of key scientific and technical problems; Promoted the development of quality product upgrading and high-grade variety to be effectively: (1) is used for the important refractory products domestic basically self-sufficiency of modernized large-scale associating iron and steel enterprise, steel alloy enterprise and cement rotary kiln; In addition, the annual in recent years refractory product outlet that also has ten thousand tons of 50-80; (2) had the work-ing life of high temperature kiln significant points refractory materials and significantly improve, for example, the MgO-C brick is brought up to several thousand stoves in the work-ing life of oxygen coverter furnace lining from the hundreds of stove, when adopting Technology of Slag Splashingfor Furnace Maintenance even can reach several ten thousand stoves.
Steel industry is the rich and influential family of refractory consumption rate, it is reported, national iron and steel enterprise refractory consumption rate amount was about more than 900 ten thousand tons in 2004, and using refractory is about 4,000,000 tons.The typical processing mode of a large amount of waste refractory materials is exactly as garbage bury, on a small quantity by coarse utilization, does not produce high added value, and is very low to its treatment effect and renewable resource utilization rate.This not only causes the waste of resource, brings the pollution of environment simultaneously.Its pollution to environment mainly contains following several kinds of modes: the silicosis that the free silica dust causes, the radioactivity of zirconium white raw material, Cr
6+Carinogenicity, the carinogenicity of refractory fibre and asbestos, the pollution of pitch and resin volatile matter.This shows,, not only can realize the solid waste resource recovery application, practice thrift the mineral wealth and the energy of country, reduce the cost and the steel-making cost of refractory materials greatly, also can significantly reduce environmental pollution simultaneously if to carrying out regenerated using with refractory.
Must arrive countries in the world with refractory as the renewable resource of cheapness and fully realize, and obtain significant progress in the country of some advanced technology.Through using the cheap refractory resource of using, improved economic benefit of enterprises significantly; Simultaneously,, be not merely environmental protection and made contribution, produced remarkable social benefit yet through reducing recycling discarded and that improve resource.Along with continuous development with refractory reutilization technology research, with the scientific and technological content of refractory, added value and again utilization ratio will improve rapidly, and progressively stride forward to " zero " emissions object.
Silica, coal and the human resources of China are abundant, help mass production silica brick, and the silica brick YO is at present above 300,000 tons.Silica brick is widely applied in the high-temperature flame-proof industry, and the construction of a lot of in recent years coke ovens, blast furnace and glass kiln needs a large amount of silica brick.This has caused a large amount of waste silica bricks and with the generation of silica brick afterwards, has produced the huge solid waste of quantity.Simultaneously environment has been produced great harm.How to handle quantity huge with back silica brick, reduce environmental pollution, realize that waste utilizes again, the target of energy-saving and emission-reduction is problems that the Chinese government pays much attention to.The utilization again that solves with back silica brick is put forth effort in this research invention, realizes turning waste into wealth, and eliminates environmental pollution, reduces industry production expenses such as metallurgy.Adopt carbo-thermal process to use back silica brick to be converted into SiC, as the raw material of producing refractory materials.
Summary of the invention:
The preparation method who the purpose of this invention is to provide the SiC refractory raw material powder that a kind of technology is simple, cost is lower, energy consumption is lower, thing phase purity is higher.
The present invention relates to a kind of novel method of SiC refractory raw material powder preparing; It is characterized in that: the present invention is to be main raw material with back silica brick and coke powder (or other carbon material is like the charcoal piece that uses front and back and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, active black); Then through moulding (can be dry-pressing formed, half-dried molded or isostatic pressing, also can material forming is spheroidal particle or directly admixtion is contained in the medium refractory product of saggar), drying, loading of kiln, carbothermic reduction burn till, cool off, fragmentation, pulverizing, technological process such as levigate prepare SiC refractory raw material powder.The main moity of the fire-resistant powder raw material of SiC that the present invention is prepared has β-SiC and a small amount of C, cristobalite and micro-ferrosilicon, each thing phase β-SiC+C+SiO
2+ Si
3Fe
5Shared overall proportion is big by 99%, and wherein the shared total thing phase ratio of β-SiC is greater than 95%.This SiC refractory raw material powder is mainly used in kiln furnitures, blast furnace and hot metal ladle liner, non-ferrous metal metallurgy crucible, refractory products such as wear-resistant liner.Said use back silica brick add-on is 0.1～99.0%, and the mass percent of said coke powder (perhaps other carbonaceous reducing agent) add-on is 0.1～99.0%.
The said back silica brick of using is from the blast furnace metallurgy industry; Require SiO in the silica brick
2Percentage composition is greater than 90%.
Said coke powder is common commercially available industrial raw material, also can use other carbon material like replacements such as the charcoal piece before and after using and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, active blacks.Require carbon content per-cent greater than 90% in coke powder or the surrogate, general particle diameter is less than 1.50mm.
The carbon material coke granule that buries that said carbothermic reduction reaction is used is commercially available industrial raw material, and its purity generally is not less than 90%.
To use back silica brick powder and coke powder (or other carbon material is like the charcoal piece before and after using and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, active black) to mix the back according to a certain ratio and add in the ball mill ball milling 0.1～24h silica brick powder and the two uniform mixing of carbonaceous reducing agent after use, the mode of ball milling can be selected dry ball milling or wet ball grinding for use.Wherein ball-milling medium can be selected Ceramic Balls or agate ball etc. for use, and the ball milling liquid that wet ball grinding is selected for use can be water or absolute ethyl alcohol etc.Then the raw material that mixes is processed base substrate through technological processs such as moulding, dryings; Wherein moulding process can be dry-pressing formed, half-dried molded or isostatic pressing, also can raw material adopted dribbling balling machine to be shaped to spheroidal particle or directly admixtion is contained in the refractory products such as saggar.
The base substrate that drying is good (or the spheroidal particle after being shaped, or directly be contained in the admixtion in the refractory product such as saggar) place the thermal kiln furnace heating to burn till through carbothermic reduction, thermal kiln furnace can be Ma Fushi combustion gas kiln or coal-fired kiln.Base substrate (or the spheroidal particle after being shaped; Or directly be contained in the admixtion in the refractory products such as saggar, fire-resistant supporting plate) through need reducing atmosphere being provided through burying carbon in the carbothermic reduction sintering process in the TR of normal temperature to 1550 ℃ or 1600 ℃; Heat-up rate does not have particular requirement; And after finally being incubated 30 minutes-90 hours under the firing temperature, under reducing atmosphere, naturally cooling to room temperature then, promptly obtain the SiC refractory raw material.
According to needs of production above-mentioned SiC refractory raw material can be prepared said SiC refractory raw material powder through fragmentation, pulverizing, technological process such as levigate.
The main thing phase composite of the fire-resistant powder raw material of SiC that the present invention is prepared is β-SiC and a small amount of C, cristobalite and micro-ferrosilicon etc.; This SiC refractory raw material not only can use as refractory materials separately, also can add in other refractory materialss to improve its performance.
The novel method of this preparation SiC refractory raw material powder that the present invention relates to has that equipment is simple, with low cost, preparation process consumed energy is few, powder thing phase purity is higher and is convenient to outstanding advantage such as scale operation, simultaneously also for the efficient increment utilization of back silica brick, realize that the Sustainable development of energy-saving and emission-reduction in the industrial production, protection environment provides a new technological approaches.
Embodiment:
Embodiment 1
Raw material and proportioning:
Use back silica brick powder add-on to be 55.4wt%, wherein SiO
2Percentage composition is 95.0%, and median size is less than 0.074mm; The coke powder add-on is 44.6wt%, and wherein the C percentage composition is 90.0%, and median size is less than 0.150mm.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry ball milling 8h, the raw material thorough mixing is even, and granularity is less than 0.150mm, the aperture sieve screen over-size is less than 2.0wt%.
Moulding or balling-up:
Material that ball mill mixing is good adds and mixes after adding suitable quantity of water in the mixer, is shaped to base substrate (or be configured as spheroidal particle with nodulizer) to material at shaper then.
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln in 100 ℃ of dry 12h, make water ratio≤1.0% of sample.
Carbothermic reduction is burnt till:
The sample that drying is good is burying carbon in big saggar, carbothermic reduction is burnt till in the retort furnace of packing into behind the sealed sagger, and firing temperature is set at 1600 ℃ and be incubated 6 hours.
The above-mentioned product that burns till is through behind the naturally cooling, can prepare said SiC refractory raw material powder according to needs of production through fragmentation, pulverizing, technological process such as levigate.The main moity of the prepared fire-resistant powder raw material of SiC is β-SiC and a small amount of C and micro-ferrosilicon.
Embodiment 2
Raw material and proportioning:
Use back silica brick powder powder add-on to be 45.45wt%, wherein SiO
2Percentage composition is 95.0%, and median size is less than 0.074mm; The coke powder add-on is 54.55wt%, and wherein the C percentage composition is 90.0%, and median size is less than 0.150mm.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry ball milling 10h, the raw material thorough mixing is even, and granularity is less than 0.150mm, the aperture sieve screen over-size is less than 2.0wt%.
Moulding or balling-up:
Raw material that ball mill mixing is good adds and mixes after adding suitable quantity of water in the mixer, on shaper, is shaped to base substrate (or be configured as spheroidal particle with nodulizer) to material then.
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln in 100 ℃ of dry 12h, make water ratio≤1.0% of base substrate sample.
Carbothermic reduction is burnt till:
The sample that drying is good is burying carbon in big saggar, carbothermic reduction is burnt till in the retort furnace of packing into behind the sealed sagger, and firing temperature is set at 1600 ℃ and be incubated 3 hours.
The above-mentioned product that burns till is through behind the naturally cooling, can prepare said SiC refractory raw material powder according to needs of production through fragmentation, pulverizing, technological process such as levigate.The main moity of the prepared fire-resistant powder raw material of SiC is β-SiC and a spot of C, cristobalite and micro-ferrosilicon.
Embodiment 3
Raw material and proportioning:
Use back silica brick powder add-on to be 55.45wt%, wherein SiO
2Percentage composition is 95.0%, and median size is less than 0.074mm; The carbon black add-on is 44.55wt%, and wherein the C percentage composition is 99.0%, and median size is less than 0.088mm.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry ball milling 10h, the raw material thorough mixing is even, and granularity is less than 0.150mm, the aperture sieve screen over-size is less than 2.0wt%.
Moulding or balling-up:
Raw material that ball mill mixing is good adds and mixes after adding suitable quantity of water in the mixer, on shaper, is shaped to base substrate (or be configured as spheroidal particle with nodulizer) to material then.
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln in 100 ℃ of dry 12h, make water ratio≤1.0% of base substrate sample.
Carbothermic reduction is burnt till:
The sample that drying is good is burying carbon in big saggar, carbothermic reduction is burnt till in the retort furnace of packing into behind the sealed sagger, and firing temperature is set at 1550 ℃ and be incubated 6 hours.
The above-mentioned product that burns till is through behind the naturally cooling, can prepare said SiC refractory raw material powder according to needs of production through fragmentation, pulverizing, technological process such as levigate.The main moity of the prepared fire-resistant powder raw material of SiC is β-SiC and a small amount of C, cristobalite and micro-ferrosilicon etc.
Claims (5)
1. the present invention relates to a kind of novel method of SiC refractory raw material preparation, it is characterized by carbothermic reduction and prepare SiC refractory raw material powder with back silica brick.The staple of the SiC refractory raw material powder that the present invention is prepared has β-SiC and a small amount of C, cristobalite and micro-ferrosilicon, each thing phase β-SiC+C+SiO
2+ Si
3Fe
5Shared overall proportion is greater than 99%, and wherein β-SiC proportion is greater than 95%.This SiC refractory raw material powder is mainly used in the SiC refractory materials of refractory products such as preparation kiln furnitures, blast furnace and hot metal ladle liner, non-ferrous metal metallurgy crucible, wear-resistant liner.
2. the preparation method of a kind of SiC refractory raw material powder according to claim 1 is characterized in that: said use back silica brick for the blast furnace lining after using with back silica brick through fragmentation, pulverizing, levigate after resulting powder, its main chemical compositions is SiO
2, containing small amounts of iron impurity simultaneously, granularity is not for being higher than 74 μ m.In addition, preferably write exactly and wherein contain SiO
2The percentage composition shared separately with other impurity.
3. the preparation method of a kind of SiC refractory raw material powder according to claim 1; It is characterized in that: being characterized as of said SiC refractory raw material novel preparation method: the present invention is being main raw material with back silica brick and coke powder (also can be Graphite Powder 99 or carbon black); It is mixed by a certain percentage; Then through moulding (can be dry-pressing formed, half-dried molded or isostatic pressing, also can with material forming be spheroidal particle or directly with admixtion be contained in the saggar, in the refractory product such as fire-resistant supporting plate), drying, loading of kiln, carbothermic reduction burn till, cool off, fragmentation, pulverizing, technological process such as levigate are prepared SiC refractory raw material powder.Said use back silica brick add-on is 0.1～99.0% (mass percent), said coke powder, graphite or carbon black add-on be 0.1～99.0% (mass percent).
4. a kind of method for preparing SiC refractory raw material powder according to claim 1; It is characterized in that: said coke powder is common commercially available industrial raw material, also can use other carbon material like replacements such as the charcoal piece before and after using and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, active blacks.Require carbon content per-cent greater than 90% in coke powder or the surrogate, general particle diameter is less than 1.50mm.
5. a kind of method for preparing SiC refractory raw material powder according to claim 1; It is characterized in that: said carbothermic reduction process adopts buries carbon technology; The used carbon material that buries is the industrial raw material coke granule, and its purity generally is not less than 90%, and granularity is 0.1-1mm.
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| CN2011102625333A CN102424586A (en) | 2011-09-06 | 2011-09-06 | Preparation method of SiC fireproof raw material powder |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826851A (en) * | 2012-08-31 | 2012-12-19 | 中国地质大学（北京） | Preparation method of zirconium boride-silicon carbide complex phase high temperature resistance powder material |
| CN103030412A (en) * | 2012-12-31 | 2013-04-10 | 郑州振中电熔锆业有限公司 | Recycling method of waste high-zirconium brick |
| CN103435367A (en) * | 2013-08-20 | 2013-12-11 | 青岛云路新能源科技有限公司 | Preparation method of antioxidant coating on surface of graphite |
| CN107176608A (en) * | 2016-03-10 | 2017-09-19 | 天地未来(北京)科技发展有限公司 | A kind of method for producing carborundum using tunnel cave by raw material of silicon chip cutting waste material |
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| CN101428800A (en) * | 2008-11-28 | 2009-05-13 | 首钢总公司 | Method for synthesis of SiC with used refractory materials |
| CN101734936A (en) * | 2009-12-23 | 2010-06-16 | 中国地质大学（北京） | Preparation method of Si3N4-SiC-C fire-resistant material powder |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101428800A (en) * | 2008-11-28 | 2009-05-13 | 首钢总公司 | Method for synthesis of SiC with used refractory materials |
| CN101734936A (en) * | 2009-12-23 | 2010-06-16 | 中国地质大学（北京） | Preparation method of Si3N4-SiC-C fire-resistant material powder |
Non-Patent Citations (1)
| Title |
|---|
| 赛音***等: "一种废弃硅砖合成SiC耐火原料的方法", 《2010年全国能源环保生产技术会议文集》, 22 June 2010 (2010-06-22), pages 473 - 475 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102826851A (en) * | 2012-08-31 | 2012-12-19 | 中国地质大学（北京） | Preparation method of zirconium boride-silicon carbide complex phase high temperature resistance powder material |
| CN103030412A (en) * | 2012-12-31 | 2013-04-10 | 郑州振中电熔锆业有限公司 | Recycling method of waste high-zirconium brick |
| CN103030412B (en) * | 2012-12-31 | 2014-05-28 | 郑州振中电熔新材料有限公司 | Recycling method of waste high-zirconium brick |
| CN103435367A (en) * | 2013-08-20 | 2013-12-11 | 青岛云路新能源科技有限公司 | Preparation method of antioxidant coating on surface of graphite |
| CN103435367B (en) * | 2013-08-20 | 2015-10-07 | 青岛云路新能源科技有限公司 | A kind of preparation method of graphite surface oxidation resistant coating |
| CN107176608A (en) * | 2016-03-10 | 2017-09-19 | 天地未来(北京)科技发展有限公司 | A kind of method for producing carborundum using tunnel cave by raw material of silicon chip cutting waste material |
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Application publication date: 20120425 |