CN101456575A - Method for preparing calcium-hexaluminate ceramic powder by calcium slag - Google Patents
Method for preparing calcium-hexaluminate ceramic powder by calcium slag Download PDFInfo
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- CN101456575A CN101456575A CNA2009100450271A CN200910045027A CN101456575A CN 101456575 A CN101456575 A CN 101456575A CN A2009100450271 A CNA2009100450271 A CN A2009100450271A CN 200910045027 A CN200910045027 A CN 200910045027A CN 101456575 A CN101456575 A CN 101456575A
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Abstract
The invention relates to a method for preparing calcium hexaluminate ceramic powder from calcium slag in the technical field of ceramic materials, which comprises: firstly, adopting the calcium slag and industrial alumina as raw materials, and preparing the calcium hexaluminate ceramic powder by a reaction sintering method, wherein the weight percentage of the calcium slag and the industrial alumina is respectively 10 to20 percent and 80 to 90 percent, and the sum of the weight percentage of the calcium slag and the industrial alumina is 100 percent; secondly, performing uniform mixing and forming, and placing formed blanks into a high-temperature furnace for sintering; and thirdly, naturally cooling the formed blanks to the room temperature, crushing the formed blanks, and obtaining the calcium hexaluminate ceramic powder. The method has simple and convenient technology, has low requirements on the calcium slag raw material, does not need to treat the calcium slag, can prepare the calcium slag into the calcium hexaluminate ceramic powder, not only reduces the production cost of calcium hexaluminate but also realizes recycling of the calcium slag, and changes the waste into the valuable.
Description
Technical field
The present invention relates to a kind of preparation method of technical field of ceramic material, specifically is a kind of method of utilizing the calcium slag to prepare the calcium hexaluminate ceramic powder.
Background technology
The calcium slag is that thermit reduction is produced the product slag in the calcium process.Thermit reduction is produced calcium metal and is come from nineteen twenty-two and invented by Bi Erzi, after U.S. New England lime company improves, becomes the main method that western countries produce commercial calcium.Owing to be subjected to the restriction of chemical reaction process, thermit reduction is produced the product calcium rate of calcium between 30%～40%.Therefore, in the process of utilizing thermit reduction production calcium, just produced a large amount of calcium slags.Calcium hexaluminate (CaAl
12O
19, be abbreviated as CA
6) be CaO-Al
2O
3Al in the system
2O
3The calcium aluminate phase that content is the highest, its theoretical density are 3.79gcm
-3, fusing point is higher than 1875 ℃, and thermal expansivity is 8.0 * 10
-6℃
-1, the solubleness in the iron content slag is low; Stability in reducing atmosphere (CO) is high; Chemical stability in alkaline environment is good; Wettability to molten metal and slag (iron and steel and non-ferrous metal) is low; Main crystallizing field is big, and lower solvability is arranged in several polynary systems; In addition, its thermal expansivity and Al
2O
3Close, can be used with any ratio with aluminum oxide.These characteristics make CA
6Be considered to one of high temperature resistant structure ceramics that has development potentiality.Adopt the synthetic CA of pure chemistry raw material
6The material cost height, this is restricted its commercial applications.Therefore, adopt the CA of low cost method processability excellence
6Material has broad application prospects.
Through the literature search of prior art is found, Li Tianqing etc. on " industrial furnace " (2006, the fourth phase, 43-46 page or leaf), deliver " alumina source material is to synthetic CA
6The porous aggregate Effect on Performance "; proposing in this article with aluminum oxide and lime carbonate is that raw material adopts the synthetic calcium hexaluminate porous aggregate of reaction sintering; concrete grammar is: respectively alumina raw material and lime carbonate are prepared burden in proportion; add an amount of organic bond; mix; moulding, after the drying, adopts the method for reaction sintering to prepare the calcium hexaluminate porous aggregate.Its deficiency is: adopting pure raw alumina and lime carbonate is raw material, and cost is higher, and complex process, and production efficiency is not high, is difficult to be applied.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of method of utilizing the calcium slag to prepare the calcium hexaluminate ceramic powder is provided, with calcium slag and commercial alumina is starting material, under the prerequisite that the calcium slag is left intact, it is synthesized the calcium hexaluminate ceramic powder, reduced the production cost of calcium hexaluminate, realized the cycling and reutilization of calcium slag, turned waste into wealth.
The present invention is achieved by the following technical solutions, and adopting calcium slag and commercial alumina is starting material, utilizes the CaO, the Al that itself contain in the calcium slag
2O
3, the Al in metal A l and the commercial alumina
2O
3, prepare the calcium hexaluminate ceramic powder by the method for reaction sintering, comprise the steps:
The first step is respectively 10～20% and 80～90% according to the weight percent of calcium slag and commercial alumina, and both sums are 100%, take by weighing calcium slag and commercial alumina starting material, it are mixed moulding;
Second step, base substrate after the moulding places Reaktionsofen to carry out sintering, earlier the heat-up rate with 6 ℃/min～10 ℃/min is heated to 300 ℃～500 ℃, insulation 0.5h～2h under air atmosphere, heat-up rate with 3 ℃/min～5 ℃/min is heated to 1000 ℃～1200 ℃, insulation 0.5h～2h again, and the heat-up rate with 1 ℃/min～3 ℃/min is heated to 1300 ℃～1500 ℃, insulation 3h～5h then;
The 3rd step naturally cooled to room temperature at last under air atmosphere, pulverize, and obtained the calcium hexaluminate powder.
The weight percent of described calcium slag component is: CaO content 20～50%, Al
2O
3Content 10～30%, Al content 10～30%, SiO
2Content 1～3%, MgO content 2～5%, TiO
2Content 0.1～1%, Fe
2O
3Content 0.1～1%.
Al in the described commercial alumina
2O
3Weight percent content is greater than 98.6%.
The technology that the present invention prepares calcium hexaluminate is easy, suitability is extensive, to the calcium slag raw-material require low, need not the calcium slag is done any processing, it can be prepared into purity greater than 94.5% calcium hexaluminate powder, both reduced the production cost of calcium hexaluminate, realized the cycling and reutilization of calcium slag again, turned waste into wealth.
Embodiment
Below embodiments of the invention are elaborated: present embodiment is being to implement under the prerequisite with the technical solution of the present invention, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1:
The weight percent of calcium slag component is: CaO content 41.09%, Al
2O
3Content 22.78%, Al content 22.52%, SiO
2Content 1.06%, MgO content 2.59%, TiO
2Content 0.55%, Fe
2O
3Content 0.59%.The Al of commercial alumina
2O
3Content 98.75%.
Calcium slag 10% and commercial alumina 90% take by weighing 90 kilograms of 10 kilograms of starting material calcium slags and commercial aluminas respectively by weight percentage, mix, moulding, base substrate after the moulding places Reaktionsofen to carry out sintering, heat-up rate with 6 ℃/min is heated to 300 ℃, insulation 2h earlier under air atmosphere, heat-up rate with 3 ℃/min is heated to 1000 ℃, insulation 2h again, heat-up rate with 3 ℃/min is heated to 1300 ℃, insulation 5h then, naturally cool to room temperature at last, pulverize, can obtain the calcium hexaluminate ceramic powder.
The calcium hexaluminate ceramic powder of preparation, main thing is CaAl mutually
12O
19Phase, wherein CaO content 7.09%, Al
2O
3Content 90.78%, SiO
2Content 0.36%, MgO content 0.59%.
Embodiment 2:
The weight percent of calcium slag component is: CaO content 41.09%, Al
2O
3Content 22.78%, Al content 22.52%, SiO
2Content 1.06%, MgO content 2.59%, TiO
2Content O.55%, Fe
2O
3Content 0.59%.The Al of commercial alumina
2O
3Content 98.75%.
Calcium slag 15% and commercial alumina 85% take by weighing 85 kilograms of 15 kilograms of starting material calcium slags and commercial aluminas respectively by weight percentage, mix, moulding, base substrate after the moulding places Reaktionsofen to carry out sintering, heat-up rate with 8 ℃/min is heated to 400 ℃, insulation 1h earlier under air atmosphere, heat-up rate with 4 ℃/min is heated to 1100 ℃, insulation 1h again, heat-up rate with 2 ℃/min is heated to 1400 ℃, insulation 4h then, naturally cool to room temperature at last, pulverize, can obtain the calcium hexaluminate ceramic powder.
The calcium hexaluminate ceramic powder of preparation, main thing is CaAl mutually
12O
19Phase, wherein CaO content 8.29%, Al
2O
3Content 88.28%, SiO
2Content 0.42%, MgO content 0.68%.
Embodiment 3:
The weight percent of calcium slag component is: CaO content 41.09%, Al
2O
3Content 22.78%, Al content 22.52%, SiO
2Content 1.06%, MgO content 2.59%, TiO
2Content 0.55%, Fe
2O
3Content 0.59%.The Al of commercial alumina
2O
3Content 98.75%.
Calcium slag 20% and commercial alumina 80% take by weighing 80 kilograms of 20 kilograms of starting material calcium slags and commercial aluminas respectively by weight percentage, mix, moulding, base substrate after the moulding places Reaktionsofen to carry out sintering, heat-up rate with 10 ℃/min is heated to 500 ℃, insulation 0.5h earlier under air atmosphere, heat-up rate with 5 ℃/min is heated to 1200 ℃, insulation 0.5h again, heat-up rate with 1 ℃/min is heated to 1500 ℃, insulation 3h then, naturally cool to room temperature at last, pulverize, can obtain the calcium hexaluminate ceramic powder.
The calcium hexaluminate ceramic powder of preparation, main thing is CaAl mutually
12O
19Phase, wherein CaO content 9.09%, Al
2O
3Content 87.35%, SiO
2Content 0.50%, MgO content 0.77%.
Claims (6)
1, a kind of method of utilizing the calcium slag to prepare the calcium hexaluminate ceramic powder is characterized in that comprising the steps:
The first step is respectively 10～20% and 80～90% according to the weight percent of calcium slag and commercial alumina, and both sums are 100%, take by weighing calcium slag and commercial alumina starting material, it are mixed moulding;
Second step, base substrate after the moulding places Reaktionsofen to carry out sintering, be heated to 300 ℃～500 ℃, insulation 0.5h～2h under air atmosphere, reheat to 1000 ℃～1200 ℃, insulation 0.5h～2h are heated to 1300 ℃～1500 ℃, insulation 3h～5h then;
The 3rd step naturally cooled to room temperature at last under air atmosphere, pulverize, and obtained the calcium hexaluminate powder.
2, the calcium slag that utilizes according to claim 1 prepares the method for calcium hexaluminate ceramic powder, it is characterized in that, describedly is heated to 300 ℃～500 ℃, and its heat-up rate is 6 ℃/min～10 ℃/min.
3, the calcium slag that utilizes according to claim 1 prepares the method for calcium hexaluminate ceramic powder, it is characterized in that, describedly is heated to 1000 ℃～1200 ℃, and its heat-up rate is 3 ℃/min～5 ℃/min.
4, the calcium slag that utilizes according to claim 1 prepares the method for calcium hexaluminate ceramic powder, it is characterized in that, describedly is heated to 1300 ℃～1500 ℃, and its heat-up rate is 1 ℃/min～3 ℃/min.
5, the calcium slag that utilizes according to claim 1 prepares the method for calcium hexaluminate ceramic powder, it is characterized in that, the weight percent of described calcium slag component is: CaO content 20～50%, Al
2O
3Content 10～30%, Al content 10～30%, SiO
2Content 1～3%, MgO content 2～5%, TiO
2Content 0.1～1%, Fe
2O
3Content 0.1～1%.
6, the calcium slag that utilizes according to claim 1 prepares the method for calcium hexaluminate ceramic powder, it is characterized in that Al in the described commercial alumina
2O
3Weight percent content is greater than 98.6%.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161591A (en) * | 2010-12-23 | 2011-08-24 | 河南科技大学 | Lightweight calcium hexaluminate-magnesia alumina spinel composite microporous refractory aggregate and preparation method thereof |
| CN103420684A (en) * | 2012-07-25 | 2013-12-04 | 田玉明 | Calcium hexaluminate CA6/anorthite CAS2 composite light heat-insulation refractory material and preparation method thereof |
| CN103553101A (en) * | 2013-08-26 | 2014-02-05 | 西南科技大学 | Method for preparing lightweight calcium hexaaluminate at low temperature |
| CN108439961A (en) * | 2018-05-21 | 2018-08-24 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of preparation method of the high-purity calcium hexaluminate of densification-corundum composite diphase material |
| CN108863406A (en) * | 2018-06-25 | 2018-11-23 | 屯留县彬烨钙合金工贸有限公司 | A kind of method of calcium metal slag production aluminate high temperature adhesives |
| CN109053181A (en) * | 2018-07-22 | 2018-12-21 | 衢州学院 | A kind of calcium hexaluminate lightweight Materials with High Strength and preparation method thereof |
| CN109369202A (en) * | 2018-12-20 | 2019-02-22 | 东北大学 | A method of high-quality calcium hexaluminate refractory raw material is prepared using two one-step baking methods |
| CN111574214A (en) * | 2020-04-02 | 2020-08-25 | 北京科技大学 | Calcium hexaluminate complex phase material and preparation method thereof |
-
2009
- 2009-01-08 CN CN2009100450271A patent/CN101456575B/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102161591A (en) * | 2010-12-23 | 2011-08-24 | 河南科技大学 | Lightweight calcium hexaluminate-magnesia alumina spinel composite microporous refractory aggregate and preparation method thereof |
| CN103420684A (en) * | 2012-07-25 | 2013-12-04 | 田玉明 | Calcium hexaluminate CA6/anorthite CAS2 composite light heat-insulation refractory material and preparation method thereof |
| CN103553101A (en) * | 2013-08-26 | 2014-02-05 | 西南科技大学 | Method for preparing lightweight calcium hexaaluminate at low temperature |
| CN108439961A (en) * | 2018-05-21 | 2018-08-24 | 中钢集团洛阳耐火材料研究院有限公司 | A kind of preparation method of the high-purity calcium hexaluminate of densification-corundum composite diphase material |
| CN108439961B (en) * | 2018-05-21 | 2021-02-05 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of compact high-purity calcium hexaluminate-corundum complex phase material |
| CN108863406A (en) * | 2018-06-25 | 2018-11-23 | 屯留县彬烨钙合金工贸有限公司 | A kind of method of calcium metal slag production aluminate high temperature adhesives |
| CN109053181A (en) * | 2018-07-22 | 2018-12-21 | 衢州学院 | A kind of calcium hexaluminate lightweight Materials with High Strength and preparation method thereof |
| CN109369202A (en) * | 2018-12-20 | 2019-02-22 | 东北大学 | A method of high-quality calcium hexaluminate refractory raw material is prepared using two one-step baking methods |
| CN109369202B (en) * | 2018-12-20 | 2021-06-29 | 东北大学 | Method for preparing high-quality calcium hexaluminate refractory raw material by two-step roasting method |
| CN111574214A (en) * | 2020-04-02 | 2020-08-25 | 北京科技大学 | Calcium hexaluminate complex phase material and preparation method thereof |
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|---|---|
| CN101456575B (en) | 2010-12-08 |
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