CN101186507B - Method for synthesizing beta cellulose in aluminum-carbon refractory material - Google Patents
Method for synthesizing beta cellulose in aluminum-carbon refractory material Download PDFInfo
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- CN101186507B CN101186507B CN2007101602107A CN200710160210A CN101186507B CN 101186507 B CN101186507 B CN 101186507B CN 2007101602107 A CN2007101602107 A CN 2007101602107A CN 200710160210 A CN200710160210 A CN 200710160210A CN 101186507 B CN101186507 B CN 101186507B
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Abstract
The invention relates to a method for synthesis beta sialon within aluminum-carbon refractory, which is characterized in that: nickel nitrate taking up 1 to 3 percent of total weight of material is made into solution with 10 percent of concentration, and fully mixed with alumina used for making aluminum-carbon refractory, then dried for eliminating water; according to the preparation technique ofaluminum-carbon refractory, the alumina material mixed with nickel nitrate and the materials metal silicon powder and sic powder for preparation aluminum-carbon refractory and bond phenolic resin areexperienced the steps: mixing, calendaring, forming, drying and burying carbon sintering under the temperature less than 1450 DEG C, and then the beta-sialon crystal grows out from the aluminum-carbon refractory. The invention has the advantages that: the nitridation sintering process under high temperature, high pressure and nitrogen atmosphere in the existing beta sialon synthesis technique is avoided; the invention has simple preparation technique, low requirement for equipment, low production cost, easy control for technique parameters, large number of beta sialon synthesized inside the aluminum-carbon refractory and good crystal development in a column shape interleaved inside the aluminum carbon refractory.
Description
Technical field
The present invention relates to a kind of method of in aluminum-carbon refractory material, synthesizing beta cellulose.
Background technology
Because the excellent properties of beta cellulose, it is at blast funnace hot blast stove, producer gas generator, position refractory materialss such as electrolytic aluminum groove, chemical industry nitriding furnace apparatus and continuous casting functional element are relative to be under reducing atmosphere and the condition that is not subjected to rapid chemical reaction and to use mutually as the combination of refractory materials, can give full play to the advantage that it improves goods bonding strength, fracture toughness property and resistance to heat shocks; Owing to its excellent high-temperature mechanical property, beta cellulose is also used at other industrial circle and high temperature field simultaneously.The method of at present synthetic beta cellulose mainly contains: the high temperature hot pressed sintering under nitrogen atmosphere with nitride and oxide compound, as not adopting heat pressing process, then must add class additives such as rare earth oxide, complex process, long flow path, cost height; Next is to utilize carbothermic method to prepare the technology of beta cellulose, but also needs high temperature, hot pressing, nitrogenize, and the cost of equipment height, the time is long, quality is low; In refractory materials usually by Pure Silicon Metal, metallic aluminium and oxide compound under nitrogen atmosphere by nitridation sintered direct preparation beta cellulose composite refractory.The above-mentioned various method for preparing beta cellulose all needs to carry out the high-temperature ammonolysis sintering in nitrogen atmosphere, to the requirement height of equipment, complicated process of preparation, condition harshness.
Summary of the invention
The purpose of this invention is to provide a kind of method of in aluminum-carbon refractory material, synthesizing beta cellulose, this method is by introducing nitrate in the aluminum-carbon refractory material preparation process, by the nitrogen and the aluminum oxide that prepare aluminum-carbon refractory material of nitrate at pyrolytic decomposition, silicon carbide, the reaction of metallic silicon raw material realizes beta cellulose synthesizing in aluminum-carbon refractory material, can save in the existing beta cellulose synthesis technique at high temperature, nitridation sintered operation under the high pressure nitrogen atmosphere, it is simple to have preparation technology, low for equipment requirements, low cost of manufacture, the characteristics that every processing parameter is easy to control.
Method of the present invention is: add 1～3% nickelous nitrate at the blending process of aluminum-carbon refractory material, under the conventional firing process condition of aluminum-carbon refractory material, utilize the synthetic beta celluloses of material such as aluminum oxide, metallic aluminium, Pure Silicon Metal and silicon carbide in nitrogen that nitrate radical decomposites and the carbon composite refractory.
Concrete preparation process is: adopt by sintering plate corundum, α-Al
2O
3, the preparation aluminum-carbon refractory material formed of Si, SiC and graphite raw material, with the nickelous nitrate of gross weight 1～3% that accounts for the raw material of described preparation aluminum-carbon refractory material be mixed with mass percentage concentration be behind 10% aqueous solution with the raw alumina thorough mixing of preparation aluminum-carbon refractory material, and it is dried to remove moisture wherein; Then with raw material graphite, metallic silicon power, carborundum powder and the wedding agent resol of these alumina raw materials that are mixed with nickelous nitrate and preparation aluminum-carbon refractory material according to the preparation technology of aluminum-carbon refractory material prepare burden, mix, moulding, drying, and be not less than bury carbon under 1450 ℃ and burn till after, can in aluminum-carbon refractory material, grow the beta cellulose crystal.
The effect of invention
The present invention is by introducing nitrate in the aluminum-carbon refractory material preparation process, by reaction realization beta cellulose the synthesizing in aluminum-carbon refractory material of nitrate at nitrogen with the aluminum oxide for preparing aluminum-carbon refractory material, silicon carbide, the metallic silicon raw material of pyrolytic decomposition, saved the nitridation sintered operation under high temperature, high pressure nitrogen atmosphere in the existing beta cellulose synthesis technique, it is simple to have preparation technology, low for equipment requirements, low cost of manufacture, the advantage that every processing parameter is easy to control.Synthetic beta cellulose quantity is many in aluminum-carbon refractory material, and crystal development is good, is column and is interwoven in aluminum-carbon refractory material inside.The present invention provides new method and thinking for beta cellulose synthetic.
Description of drawings
Fig. 1 be of the present invention in aluminum-carbon refractory material the stereoscan photograph figure of synthetic beta cellulose;
Fig. 2 be of the present invention in aluminum-carbon refractory material the energy spectrum composition analysis collection of illustrative plates of synthetic beta cellulose.
Embodiment
Embodiment
The physical and chemical index % of table 1 raw material
The proportioning of the various materials of table 2
1) chooses sintering plate corundum, α-Al according to physical and chemical index shown in the table 1
2O
3,, crystalline flake graphite, carborundum powder, metal Si powder and resol and nickelous nitrate; Proportioning according to various materials in the table 2 takes by weighing the plate diamond spar 330g that granularity is 1.0～0mm, the plate diamond spar 300g of＜0.043mm, α-Al respectively
2O
3Powder 80g, crystalline flake graphite 240g, carborundum powder 20g, metallic silicon power 30g, resol 60g is standby;
2) taking by weighing 10 gram nickelous nitrates adds 90 gram distilled water to be mixed with concentration is 10% solution, then it is joined above-mentioned steps 1) in the granularity of the 300g that takes by weighing be thorough mixing in the plate diamond spar powder of＜0.043mm, place loft drier to get rid of to moisture wherein in dry 48 hours down in mixture in 110 ℃, with desciccate place grinding machine for grinding after 30 minutes with 80g α-Al that step 1) is taken by weighing
2O
3Powder, 30g metallic silicon power, 20g carborundum powder mixing for standby use;
3) the 60g resol that takes by weighing in the step 1) is heated 15 minutes in 80 ℃ water-bath after, one joined partly load weighted 330g granularity is in the plate diamond spar of 1.0～0mm in the step 1), in mixing machine, mix and add the good 240g crystalline flake graphite of weighing in the step 1) after 5 minutes, continue to mix after 5 minutes and will add wherein by mixed good fine powder in remaining resol and the step 2, continued to mix after 20 minutes in the plastics bag that mixed material packed into ageing mixture again 5～6 hours;
4) tired good material in the step 3) being pressed into volume density with universal press is 2.7 ± 0.1g/cm
3, be of a size of the adobe of φ 50mm * 50mm, place 180 ℃ loft drier to bury carbon after dry 24 hours adobe and be heated to 1450 ℃, be incubated 4 hours, naturally cool to room temperature and promptly obtain the aluminum-carbon refractory material goods.Goods are placed under the scanning electron microscope observe, can observe well-grown beta cellulose crystal within it.
Embodiment 2
1) chooses sintering plate corundum, α-Al according to physical and chemical index shown in the table 1
2O
3,, crystalline flake graphite, carborundum powder, metal Si powder and resol and nickelous nitrate; Proportioning according to various materials in the table 2 takes by weighing the plate diamond spar 330g that granularity is 1.0～0mm, the plate diamond spar 300g of＜0.043mm, α-Al respectively
2O
3Powder 80g, crystalline flake graphite 240g, carborundum powder 20g, metallic silicon power 30g, resol 60g is standby;
2) taking by weighing 20 gram nickelous nitrates adds 180 gram distilled water to be mixed with concentration is 10% solution, then it is joined above-mentioned steps 1) in the 300g granularity that takes by weighing be thorough mixing in the plate diamond spar powder of＜0.043mm, place loft drier to get rid of to moisture wherein in dry 48 hours down in mixture in 110 ℃, with desciccate place grinding machine for grinding after 30 minutes with 80g α-Al that step 1) is taken by weighing
2O
3Powder, 30g metallic silicon power, 20g carborundum powder mixing for standby use;
3) the 60g resol that takes by weighing in the step 1) is heated 15 minutes in 80 ℃ water-bath after, one joined partly load weighted 330g granularity is in the plate diamond spar of 1.0～0mm in the step 1), in mixing machine, mix and add the good 240g crystalline flake graphite of weighing in the step 1) after 5 minutes, continue to mix after 5 minutes remaining resol and step 2) in mixed good fine powder add wherein, continued to mix after 20 minutes in the plastics bag that mixed material packed into ageing mixture again 5～6 hours;
4) tired good material in the step 3) being pressed into volume density with universal press is 2.7 ± 0.1g/cm
3, be of a size of the adobe of φ 50mm * 50mm, place 180 ℃ loft drier to bury carbon after dry 24 hours adobe and be heated to 1450 ℃, be incubated 4 hours, naturally cool to room temperature and promptly obtain the aluminum-carbon refractory material goods.Goods are placed under the scanning electron microscope observe, can observe well-grown beta cellulose crystal within it.
Embodiment 3
1) chooses sintering plate corundum, α-Al according to physical and chemical index shown in the table 1
2O
3, graphite, carborundum powder, metal powder and resol and nickelous nitrate; Proportioning according to various materials in the table 2 takes by weighing the plate diamond spar 330g that granularity is 1.0～0mm, the plate diamond spar 300g of＜0.043mm, α-Al respectively
2O
3Powder 80g, crystalline flake graphite 240g, metallic silicon power 30g, carborundum powder 20g, resol 60g are standby;
2) taking by weighing 30 gram nickelous nitrates adds 270 gram distilled water to be mixed with concentration is the granularity that joins the 300g that takes by weighing in the above-mentioned steps behind 10% solution and be thorough mixing in the plate diamond spar of＜0.043mm, place loft drier to get rid of to moisture wherein in dry 48 hours down in mixture in 110 ℃, then desciccate is placed grinding machine for grinding after 30 minutes with 80g α-Al that step 1) is taken by weighing
2O
3Powder, the carborundum powder mixing for standby use of 30g metallic silicon power, 20g;
3) the 60g resol that takes by weighing in the step 1) is heated 15 minutes in 80 ℃ water-bath after, one joined partly load weighted 330g granularity is in the plate diamond spar of 1.0～0mm in the step 1), in mixing machine, mix after 5 minutes and add load weighted 240g crystalline flake graphite in the step 1) again, continue to mix after 5 minutes remaining resol and step 2) in mixed good fine powder add wherein, continue to mix the ageing mixture 5～6 hours of packing into after 20 minutes in the plastics bag again;
4) tired good material in the step 3) being pressed into volume density with universal press is 2.7 ± 0.1g/cm
3, be of a size of the adobe of φ 50mm * 50mm, place 180 ℃ loft drier to bury carbon after dry 24 hours adobe and be heated to 1450 ℃, be incubated 4 hours, naturally cool to room temperature and promptly obtain the aluminum-carbon refractory material goods.The aluminum-carbon refractory material goods are placed under the scanning electron microscope observe, can observe many, the well-grown beta cellulose crystal of quantity within it.
Claims (1)
1. the method for a synthetic beta cellulose in aluminum-carbon refractory material is characterized in that:
(1), adopts by sintering plate corundum, α-Al
2O
3, the preparation aluminum-carbon refractory material formed of Si, SiC and crystalline flake graphite raw material, the proportioning of various materials is by weight percentage in the above-mentioned raw materials: the sintering plate corundum of granularity 1～0mm: the sintering plate corundum of granularity＜0.043mm 33%: granularity＜5 micron α-Al 30%,
2O
3: the Si:3% of SiC:2%, the granularity＜0.075mm of granularity＜0.18mm graphite 24%, granularity＜0.043mm and will account for the nickelous nitrate and the resol 6% of gross weight 1～3% of the raw material of above-mentioned preparation aluminum-carbon refractory material 8%;
(2), getting nickelous nitrate in the step (1) adds distilled water to be mixed with concentration is 10% solution, the granularity that then it is joined in the above-mentioned steps (1) is thorough mixing in the plate diamond spar powder of＜0.043mm, place loft drier to get rid of to moisture wherein in dry 48 hours down in mixture in 110 ℃, with desciccate place grinding machine for grinding after 30 minutes with α-Al with step (1)
2O
3Powder, metallic silicon power, carborundum powder mixing for standby use;
(3) resol in the step (1) is heated 15 minutes in 80 ℃ water-bath after, the granularity that one is partly joined step (1) is in the plate diamond spar of 1.0～0mm, in mixing machine, mix after 5 minutes and add in the graphite of step (1), continue to mix after 5 minutes and will add wherein by mixed good fine powder in remaining resol and the step (2), continued to mix after 20 minutes in the plastics bag that mixed material packed into ageing mixture again 5～6 hours;
(4) tired good material in the step (3) being pressed into volume density with universal press is 2.7 ± 0.1g/cm
3, be of a size of the adobe of φ 50mm * 50mm, place 180 ℃ loft drier to bury carbon after dry 24 hours adobe and be heated to 1450 ℃, be incubated 4 hours, naturally cool to room temperature and promptly obtain the aluminum-carbon refractory material goods;
(5) goods are placed under the scanning electron microscope observe, can observe well-grown beta cellulose crystal within it.
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| CN2007101602107A CN101186507B (en) | 2007-12-14 | 2007-12-14 | Method for synthesizing beta cellulose in aluminum-carbon refractory material |
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| CN2007101602107A CN101186507B (en) | 2007-12-14 | 2007-12-14 | Method for synthesizing beta cellulose in aluminum-carbon refractory material |
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| CN101186507B true CN101186507B (en) | 2011-02-16 |
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| CN106431431A (en) * | 2016-08-31 | 2017-02-22 | 江苏诺明高温材料股份有限公司 | In-situ generating method for Si2N2O ceramic bonding phases in aluminum-carbon fireproof material with carbon thermal reduction method |
| CN109206144A (en) * | 2018-10-30 | 2019-01-15 | 苏州佳耐材料科技有限公司 | A kind of preparation and detection method of Ultra-low carbon aluminum-carbon refractory material |
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