CN101654369A - Method for preparing Fe-Sialon fire-proof raw materials - Google Patents
Method for preparing Fe-Sialon fire-proof raw materials Download PDFInfo
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- CN101654369A CN101654369A CN200910092569A CN200910092569A CN101654369A CN 101654369 A CN101654369 A CN 101654369A CN 200910092569 A CN200910092569 A CN 200910092569A CN 200910092569 A CN200910092569 A CN 200910092569A CN 101654369 A CN101654369 A CN 101654369A
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Abstract
The invention relates to a method for preparing Fe-Sialon fire-proof raw materials, belonging to the technical field for preparing fire-proof raw materials. The Fe-Sialon is a novel fire-proof raw material with a heat-resistant property, an inoxidizability, a thermochemical stability and a function of gradient agglomeration. The Fe-Sialon is mainly used for preparing stemming fire-proof raw materials of blast furnace, casting materials of iron tap channel and other heat-resistant materials. The main raw materials of the invention contain iron ore concentrate powder, high-aluminum fly ash and coke powder, etc. Through a component design, carbon thermal azotization reduction action is performed at proper temperature according to the demand of fire-proof raw materials. After cooling, breakingand grinding the reaction product to acquire the Fe-Sialon fire-proof raw materials powder. The components of the Fe-Sialon prepared by the invention contain a majority of Beta-Sialon, Alpha-Sialon,15R, Fe3Si, Fe and a small quantity of Si2N2O, AlN, SiC, FeSi, C, etc. The method of the invention has the advantages of low cost, less energy consumption and low environmental pollution.
Description
Technical field:
The present invention relates to a kind of novel method of the Fe-Sialon of preparation refractory raw material, the powder of this Fe-Sialon refractory raw material is mainly used in the stemming fire-proof material of iron-smelting blast furnace, belongs to the raw material for refractory technical field.
Background technology:
Along with China's rapid development of economy, driven the demand of all trades and professions for iron and steel, China has been that the world produces iron big country.The iron and steel output of China in 2007 reaches 48,966 ten thousand tons, accounts for 36.4% of Gross World Product then.In recent years, furnace volume trends towards maximizing in the blast furnace ironmaking development; Investment for steel industry in all parts of the country is also more and more, and newly-built many new iron and steel enterprises make the iron and steel output of China be zooming trend year by year.
In recent decades, blast-furnace technique obtains develop rapidly, blast furnace campaign is also more and more longer, concrete aspect new technology shows as: the co-content blast furnace does not all begin to adopt new technologies such as high blast, high roof pressure, Gao Yeqiang, big air quantity and oxygen-enriched injection, behind strengthening smelting, the number of times that taps a blast furnace day increases for medium and small blast furnace, and the overwhelming majority is increased to 15 times/day by 12 times/day, what have is increased to 18 times/day, and has cancelled and put slag technology; High furnace capacity is increasing, and is general by original small furnace (300～1000m
3) begin to large blast furnace (2500m
3More than) change; The ironmaking quality increases greatly, and blast furnace can reach high yield and low power consuming; Also than increasing greatly in the past, can extend to more than 15 years blast furnace campaign.The maintenance and operation of iron notch is depended in the safety operation of the behaviour in service of iron-smelting blast furnace, productivity and stokehold to a great extent.
Iron notch is one of position important in the iron-smelting blast furnace structure.The elementary operation of iron notch is slagged tap exactly and is tapped a blast furnace.Iron-smelting blast furnace The Enlargement Tendency and medium and small blast furnace are behind strengthening smelting, and the number of times increase of tapping a blast furnace day etc. has all caused the requirement of blast furnace iron notch stemming consumption and quality more and more higher.
Because blast furnace ironmaking is had higher requirement to the quality of the used stemming of blast furnace now, stemming turns to functional refractory materials from simple expendable refractory materials of past.In order to satisfy the iron-smelting blast furnace requirement of safe production, domestic and international research personnel have carried out many-sided tackling key problem to how improving the stemming quality, in the hope of better improving blast furnace iron notch stemming performance.
High-performance stemming general choice high-quality non-oxidized substance raw material or artificial-synthetic material are as the main material of stemming both at home and abroad, adopt new junction agent and admixture simultaneously, improve the anhydrous stemming quality and obtain stable performance, it is stable to guarantee during use to tap a blast furnace, the time of tapping a blast furnace is long, and the stemming unit consumption greatly reduces.
The used stemming of the big-and-middle-sized ironmaking of lot of domestic and international enterprise's blast furnace generally adds Fe-Si in the preparation at present
3N
4Raw material is because the introducing of metallic iron and silicon nitride makes and adds Fe-Si
3N
4Blast furnace mud not only have good resistance to fouling and scour resistance, make the process ratio of tapping outlet be easier to but also have the gradient sintering function.But Fe-Si
3N
4The production technique cost is higher at present, and energy consumption is bigger, causes price higher, is unfavorable for its popularization in blast furnace mud is used.
Sialon and Si
3N
4Character is close, is Si
3N
4The Si atom and the N atom simultaneously respectively by Al atom and O atomic substitutions and keep electric neutrality, a kind of Si-Al-O-N sosoloid of formation.Adopt Sialon to replace Fe-Si
3N
4In Si
3N
4, can produce and obtain that cost is low, the Fe-Sialon refractory raw material of excellent property.
Aluminous fly-ash is coal and a coal gangue products of combustion in the industry of coal fired power generation, and is one of industrial waste of China's quantity discharged maximum.In recent years, the energy industry stable development of China, and coal fired power generation accounts for the largest percentage in China's power industry.Development of electric power industry has been brought rolling up of aluminous fly-ash quantity discharged thereupon, has caused huge pressure for the economic construction and the ecotope of China.In order to solve the environmental pollution that aluminous fly-ash brings, how China researchist also fully utilizes aluminous fly-ash in research always, reduces environmental pollution.
Summary of the invention:
Fe-Sialon is a kind of novel have high temperature resistant, the good oxidation-resistance and raw material for refractory of thermo-chemical stability, and has the gradient sintering function.It is mainly used in stemming fire-proof material, the casting house mould material of iron-smelting blast furnace, can also be used to prepare other high temperature material.The present invention is a main raw material with fine iron breeze, aluminous fly-ash and coke powder etc., pass through design of components, require under suitable temperature schedule, to carry out the carbothermal reduction-nitridation sintering according to required refractory materials, after the cooling that product is broken and levigate, can prepare the high performance Fe-Sialon refractory raw material powder that is applied to various stemming fire-proof materials.
The present invention relates to a kind of novel method of the Fe-Sialon of preparation refractory raw material, it is characterized by: the present invention is a main raw material with fine iron breeze, aluminous fly-ash and coke powder etc., add the normal temperature wedding agent, ball milling mixes by a certain percentage, the material that ball milling is mixed adds and mixes after adding suitable quantity of water in the mixer, then material is shaped to base substrate (or be configured as spheroidal particle with nodulizer) at shaper, also can directly is contained in admixtion in the saggar or is placed on the fire-resistant supporting plate.Then by drying, loading of kiln, carbothermal reduction-nitridation burn till, technological process such as cooling, grinding and processing, can prepare the powder of Fe-Sialon refractory raw material.The constituent of the prepared iron silicon nitride of the present invention is mainly beta-Sialon, α-Sialon, 15R, Fe mutually
3Si, Fe and a spot of Si
2N
2O, AlN, SiC, FeSi and C etc.The mass percent of the add-on of described fine iron breeze is 0.1～90.0%, the mass percent of described aluminous fly-ash add-on is 0.1～90.0%, the mass percent of described coke powder add-on is 0.1～90.0%, and the described add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
Described fine iron breeze raw material is usually commercially available iron ore raw material, also can replace by other materials that contain ferric oxide and iron with iron phosphorus powder and troilite powder etc.; Require in fine iron breeze or the surrogate that wherein the Fe percentage composition is greater than 50%, median size is less than 0.30mm.
Described aluminous fly-ash is a waste material after the using of producing in the common power-plant operation; Aluminous fly-ash requires wherein SiO
2Percentage composition is greater than 20%, Al
2O
3Percentage composition is greater than 20%, and median size is less than 0.30mm.
Described coke powder is usually commercially available raw material, also can be with other carbon material as replacements such as the charcoal piece that uses front and back and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, gac, coal dusts.Require the C percentage composition greater than 90% in coke powder or the surrogate, median size is less than 0.30mm.Add the normal temperature wedding agent in the described preparation process and adopt industrial dextrin solution or refractory materialss such as calcium lignosulfonate solution or polyvinyl alcohol solution or silicon sol or pitch or tar or resin wedding agent commonly used.
Dry good base substrate (or the spheroidal particle after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi combustion gas kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, heat-up rate does not have particular requirement, can be incubated certain hour respectively under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheroidal particle after naturally cooling to room temperature, the technological process through grinding and processing can prepare Fe-Si as required
3N
4The powder of the different fineness of refractory raw material.
The constituent of the prepared ferro-silicon nitride of the present invention is mainly beta-Sialon, α-Sialon, 15R, Fe mutually
3Si, Fe and a spot of Si
2N
2O, AlN, SiC, FeSi and C etc.The prepared Fe-Sialon of the present invention wherein can adjust by the control proportion of raw materials by aluminium content, iron level and the silicone content of product.
The novel method of this preparation Fe-Sialon refractory raw material that the present invention relates to has the outstanding advantage that cost is low, the preparation process consumed energy is few.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention is described further:
In the preparation process of the present invention when batching each raw material add-on and specification of quality as follows: fine iron breeze (or iron filings powder, steel rolling iron scale, troilite powder etc. other contain the material of ferric oxide and iron) requires wherein the Fe percentage composition greater than 50%, median size is less than 0.30mm, and add-on is 0.1～90.0%; Aluminous fly-ash requires wherein SiO
2Percentage composition is greater than 20%, Al
2O
3Percentage composition is greater than 20%, and median size is less than 0.30mm, and add-on is 0.1～90.0%; Coke powder (or the charcoal piece before and after using and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, gac, coal dust etc.) requires wherein that the C percentage composition is greater than 90%, and median size is less than 0.30mm, and add-on is 0.1～90.0%; Wedding agent requires to adopt industrial dextrin solution or refractory materialss such as calcium lignosulfonate solution or polyvinyl alcohol solution or silicon sol or pitch or tar or resin wedding agent commonly used, and the add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
The novel method of this preparation Fe-Sialon refractory raw material that the present invention proposes, its principal character is: described method is with various raw material pulverizing or after being ground to desired particle size, is preparing burden in described ratio, joins ball mill and mixes; The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the mixer, then material is shaped to base substrate (or be configured as spheroidal particle with nodulizer) at shaper.Moulding is also dry, dry good adobe (or the spheroidal particle after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi combustion gas kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, heat-up rate does not have particular requirement, can be incubated certain hour respectively under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheroidal particle after naturally cooling to room temperature,, can prepare the powder of the different fineness of Fe-Sialon refractory raw material as required through the technological process of grinding and processing.The novel method of this preparation Fe-Sialon refractory raw material that the present invention relates to has the outstanding advantage that cost is low, the preparation process consumed energy is few.
A kind of preparation technology's flow process of Fe-Sialon high-performance refractory material feedstock is:
Raw material → batching → batch mixing → moulding → drying → nitrogenize is burnt till → is checked
Embodiment 1
Raw material and proportioning:
Fine iron breeze (magnetite) add-on is 8wt.%, and wherein the Fe percentage composition is 60%, and median size is less than 0.088mm; The aluminous fly-ash add-on is 74wt.%, wherein Al
2O
3Percentage composition is 30%, SiO
2Percentage composition is 50%, and median size is less than 0.088mm; The coke powder add-on is 18wt.%, and wherein the C percentage composition is 99.0%, and median size is less than 0.088mm.The add-on that adds the wedding agent silicon sol is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 10h, the raw material thorough mixing is even, and granularity is less than 0.088mm, the aperture sieve screen over-size is less than 2.0wt.%.
Moulding:
The material that ball milling is mixed adds and mixes after adding suitable quantity of water in the mixer, then material is shaped to base substrate (or be configured as spheroidal particle with nodulizer) at shaper.
Dry:
Sample after the moulding is seasoning 10h at room temperature, then in dry kiln prior to 100 ℃ of dry 4h, make water ratio≤3.0% of sample.
Nitrogenize is burnt till:
The sample that drying is good is packed into and is burnt till 1550 ℃ of firing temperatures in the nitriding electric furnace.Calcining system is: 1500 ℃ of insulation 1h, 1550 ℃ are incubated 10 hours.
Check:
Product after burning till is carried out to the branch check on request.
The main thing of resulting product is mutually following: beta-Sialon, α-Sialon, Fe
3Si and Fe.
Embodiment 2
Raw material and proportioning:
Fine iron breeze (rhombohedral iron ore) add-on is 11wt.%, and wherein the Fe percentage composition is 55%, and median size is less than 0.088mm; The aluminous fly-ash add-on is 73wt.%, wherein Al
2O
3Percentage composition is 40%, SiO
2Percentage composition is 45%, and median size is less than 0.074mm; The graphite electrode powder add-on is 16wt.%, and wherein the C percentage composition is 98.0%, and median size is less than 0.074mm.The add-on that adds wedding agent (industrial dextrin) is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 12h, the raw material thorough mixing is even, and granularity is less than 0.074mm, the aperture sieve screen over-size is less than 2.0wt.%.
Moulding:
The material adding shaper that ball milling is mixed is molded into base substrate (or spheroidal particle).
Dry:
Base substrate after the moulding is seasoning 12h at room temperature, then in dry kiln prior to 120 ℃ of dry 2h, make water ratio≤3.0% of sample.
Nitrogenize is burnt till:
The sample that drying is the good nitrogen kiln roasting of packing into, 1580 ℃ of firing temperatures.Calcining system is: 1530 ℃ of insulation 1h, 1580 ℃ are incubated 7 hours.
Check:
Product after burning till is carried out to the branch check on request.
The main thing of resulting product is mutually following: beta-Sialon, α-Sialon, Fe
3Si and Fe.
Embodiment 3
Raw material and proportioning:
Fine iron breeze (magnetite) add-on is 13wt.%, and wherein the Fe percentage composition is 63%, and median size is less than 0.074mm; The aluminous fly-ash add-on is 67wt.%, wherein Al
2O
3Percentage composition is 35%, SiO
2Percentage composition is 53%, and median size is less than 0.074mm; The petroleum coke powder add-on is 20wt.%, and wherein the C percentage composition is 90.0%, and median size is less than 0.074mm.The add-on that adds wedding agent (calcium lignin sulphonate) is 2～3% of total batching quality.
Batching, batch mixing:
At first with various raw materials according to the above-mentioned ratio mixer of packing into, dry grinding 10h, the raw material thorough mixing is even, and granularity is less than 0.074mm, the aperture sieve screen over-size is less than 2.0wt.%.
Moulding:
The material adding shaper that ball milling is mixed is molded into base substrate (or spheroidal particle).
Dry:
Sample after the moulding is seasoning 12h at room temperature, then in dry kiln prior to 100 ℃ of dry 4h, make water ratio≤3.0% of base substrate.
Nitrogenize is burnt till:
The base substrate that drying is the good nitrogen kiln roasting of packing into, 1530 ℃ of firing temperatures.Calcining system is: 1500 ℃ of insulation 1h, 1530 ℃ are incubated 15 hours.
Check:
Sample after burning till is carried out to the branch check on request.
The main thing of resulting product is mutually following: beta-Sialon, α-Sialon, Fe
3Si and Fe.
Claims (6)
1, the present invention relates to a kind of novel method of the Fe-Sialon of preparation refractory raw material, the powder of this Fe-Sialon refractory raw material is mainly used in the stemming fire-proof material of iron-smelting blast furnace.It is characterized by: the present invention is a main raw material with fine iron breeze, aluminous fly-ash and coke powder etc.; add the normal temperature wedding agent; mix by a certain percentage; be shaped to spheroidal particle then or be compressed to technological processs such as base substrate (also can directly be contained in admixtion in the saggar or be placed on the fire-resistant supporting plate) drying, loading of kiln, carbothermal reduction-nitridation are burnt till, cooling, grinding and processing, can prepare the powder of Fe-Sialon refractory raw material.The grand constituent of the prepared iron match of the present invention is mainly beta-Sialon, α-Sialon, 15R, Fe mutually
3Si, Fe and a spot of Si
2N
2O, AlN, SiC, FeSi and C etc.The mass percent of the add-on of described fine iron breeze is 0.1～90.0%, the mass percent of described aluminous fly-ash add-on is 0.1～90.0%, the mass percent of described coke powder add-on is 0.1～90.0%, and the described add-on that adds wedding agent commonly used is 0.2～15% of total batching quality.
2, a kind of method for preparing the Fe-Sialon refractory raw material according to claim 1, it is characterized in that: described fine iron breeze raw material is common commercially available iron ore raw material, also can replace by other materials that contain ferric oxide and iron with iron filings powder, steel rolling iron scale (steel scale of steel rolling) and troilite powder etc.; Require in fine iron breeze or the surrogate that wherein the Fe percentage composition is greater than 50%, median size is less than 0.30mm.
3, a kind of method for preparing the Fe-Sialon refractory raw material according to claim 1 is characterized in that: described aluminous fly-ash is a waste material after the using of producing in the common power-plant operation; Aluminous fly-ash requires SiO
2Percentage composition is greater than 20%, Al
2O
3Percentage composition is greater than 20%, and median size is less than 0.30mm.
4, a kind of method for preparing the Fe-Sialon refractory raw material according to claim 1, it is characterized in that: described coke powder is common commercially available raw material, also can be with other carbon material as replacements such as the charcoal piece that uses front and back and graphite electrode powder, electric calcined anthracite powder, asphalt powder, petroleum coke powder, gac, coal dusts.Require the C percentage composition greater than 90% in coke powder or the surrogate, median size is less than 0.30mm.
5, a kind of method for preparing the Fe-Sialon refractory raw material according to claim 1 is characterized in that: add the normal temperature wedding agent in the described preparation process and adopt industrial dextrin solution or refractory materialss such as calcium lignosulfonate solution or polyvinyl alcohol solution or silicon sol or pitch or tar or resin wedding agent commonly used.
6, a kind of method for preparing the Fe-Sialon refractory raw material according to claim 1, it is characterized in that: dry good base substrate (or the spheroidal particle after being shaped) places thermal kiln furnace loading of kiln, heating and carbothermal reduction-nitridation to burn till, and thermal kiln furnace can be the nitriding furnace, microwave nitriding furnace, induction nitriding furnace, tubular type nitriding furnace, vertical nitriding furnace of nitriding electric furnace, Ma Fushi combustion gas kiln or coal-fired kiln or oil-firing kiln etc.Base substrate places the nitrogen kiln to adopt and buries the carbon granule protection.Burn till through the carbothermal reduction-nitridation in the temperature range of normal temperature to 1700 ℃, heat-up rate does not have particular requirement, can be incubated certain hour respectively under corresponding temperature, and insulation is 10 minutes～50 hours under the highest roasting; Take out base substrate or spheroidal particle after naturally cooling to room temperature,, can prepare the powder of the different fineness of Fe-Sialon refractory raw material as required through the technological process of grinding and processing.
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|---|---|---|---|
| CN200910092569A CN101654369A (en) | 2009-09-18 | 2009-09-18 | Method for preparing Fe-Sialon fire-proof raw materials |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910092569A CN101654369A (en) | 2009-09-18 | 2009-09-18 | Method for preparing Fe-Sialon fire-proof raw materials |
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ID=41708859
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219532A (en) * | 2011-03-29 | 2011-10-19 | 中国地质大学（北京） | Preparation method of refractory Fe-Sialon raw material |
| CN102617150A (en) * | 2012-03-22 | 2012-08-01 | 大连工业大学 | Method for preparing Fe-Sialon composite powder |
| CN103172389A (en) * | 2011-12-22 | 2013-06-26 | 中冶建筑研究总院有限公司 | Blast furnace gun mud added with SiAlON synthesized through coal ash and preparation method of blast furnace gun mud |
| CN103804010A (en) * | 2013-12-27 | 2014-05-21 | 西安宝德粉末冶金有限责任公司 | Porous composite sialon ceramic and preparation method for same |
| CN111253165A (en) * | 2020-03-19 | 2020-06-09 | 西安澳秦新材料有限公司 | Preparation method of low-cost porous silicon nitride refractory brick |
-
2009
- 2009-09-18 CN CN200910092569A patent/CN101654369A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102219532A (en) * | 2011-03-29 | 2011-10-19 | 中国地质大学（北京） | Preparation method of refractory Fe-Sialon raw material |
| CN103172389A (en) * | 2011-12-22 | 2013-06-26 | 中冶建筑研究总院有限公司 | Blast furnace gun mud added with SiAlON synthesized through coal ash and preparation method of blast furnace gun mud |
| CN102617150A (en) * | 2012-03-22 | 2012-08-01 | 大连工业大学 | Method for preparing Fe-Sialon composite powder |
| CN103804010A (en) * | 2013-12-27 | 2014-05-21 | 西安宝德粉末冶金有限责任公司 | Porous composite sialon ceramic and preparation method for same |
| CN111253165A (en) * | 2020-03-19 | 2020-06-09 | 西安澳秦新材料有限公司 | Preparation method of low-cost porous silicon nitride refractory brick |
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Application publication date: 20100224 |