CN112851123B - Method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag - Google Patents
Method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag Download PDFInfo
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- C03—GLASS; MINERAL OR SLAG WOOL
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- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
- C03C10/0063—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition containing waste materials, e.g. slags
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- C03B19/00—Other methods of shaping glass
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Abstract
The invention discloses a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag. Takes the ferronickel slag as a raw material and the fly ash as a modifier, and induces the components of the ferronickel slag to be directionally transformed by optimizing the proportion of the ferronickel slag and the fly ash and controlling the crystallization temperature of microcrystalline glass (700 ℃ F. and 1000 ℃ C.) to prepare the spinel (MgFe) with the enstatite as a main crystal phase 2 O 4 、MgAl 2 O 4 、MgCr 2 O 4 ) The glass ceramics are reinforced phase glass ceramics, thereby improving the comprehensive performance of the glass ceramics. The density of the enstatite/spinel complex phase glass ceramics prepared by the invention is 3.02-3.09g/cm 3 The acid resistance is more than or equal to 99.95 percent, the alkali resistance is more than or equal to 99.51 percent, the breaking strength is 72-116MPa, and the Mohs hardness is 8-9. The invention has the characteristics of simple process, low production cost and environmental friendliness. The pyroxene-spinel complex phase microcrystalline glass prepared by utilizing the nickel-iron slag has the advantages of good chemical stability, high breaking strength and the like, and has good application prospect.
Description
Technical Field
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, belonging to the technical field of glass ceramics.
Technical Field
With the rapid development of the stainless steel industry, the smelting scale of the needed ferronickel is rapidly increased, and the discharge amount of ferronickel smelting slag is rapidly increased. According to relevant statistics, the annual discharge amount of nickel-iron slag in China is about 3000 ten thousand tons, and the nickel-iron slag becomes the fourth major smelting slag after iron slag, steel slag and red mud. At present, the slag stock in China exceeds 2 hundred million tons, the utilization rate is only about 10 percent, a large amount of land is occupied, and serious environmental pollution is caused. Therefore, how to treat the nickel-iron slag efficiently, reasonably and economically becomes a serious problem in the ferronickel smelting industry.
At present, the treatment mode of the nickel-iron slag mainly comprises stockpiling and landfill, and the research direction mainly focuses on the aspects of underground filling, building material raw materials, synthetic polymers, refractory fiber preparation, valuable metal recovery, heat insulation brick preparation and the like. Compared with iron slag and steel slag, the nickel-iron slag has high magnesium oxide and silicon oxide content (the sum of the two contents accounts for about 75 wt%), contains ferrous oxide (5-10 wt%), aluminum oxide (2-5 wt%) and harmful heavy metal elements (such as Cr and the like), has complex chemical components and low activity, causes small usage amount and low additional value of the nickel-iron slag in the aspects of underground filling, building material raw materials, synthetic polymers and the like, and has long flow and difficult operation in the aspects of preparing refractory fibers and recycling valuable metals.
The method for preparing the microcrystalline glass is a method for efficiently utilizing metallurgical slag. The glass ceramics has the advantages of glass, ceramics and natural stone, has outstanding mechanical property, high chemical stability and good wear resistance,meanwhile, the source of the raw materials for preparing the compound is wide. Accordingly, glass ceramics, especially CaO-Al 2 O 3 -SiO 2 (CAS)、CaO-MgO-Al 2 O 3 -SiO 2 (CMAS) microcrystalline glass becomes a novel building decoration material with wide market application prospect. The CAS and CMAS microcrystalline glass has main crystal phases: diopside, pyroxenes, wollastonite, anorthite, etc., which have excellent mechanical properties, chemical stability and wear resistance, but have not high mohs hardness (5-6). Therefore, the microcrystalline glass is easy to scratch in daily use, and the service life and the decorative effect of the microcrystalline glass are influenced. Meanwhile, as the nickel-iron slag contains higher MgO, the content of magnesium oxide is higher than 20 wt% along with the increase of the adding amount of the nickel-iron slag, and a forsterite phase is easily generated in the heat treatment process of the basic glass, so that the mechanical property of the microcrystalline glass is seriously reduced.
Patent 201711326806.X discloses a preparation method of building ceramics prepared from ferronickel slag. Mixing nickel-iron slag serving as a raw material and quartz, a silicon-rich aluminum raw material and a calcium raw material serving as additives according to mass percent, grinding, granulating, forming and roasting to obtain the nickel-iron slag ceramic. The ferronickel slag ceramic material prepared by the method contains anorthite, spinel, olivine and other crystals, has excellent mechanical properties (rupture strength of 85-180MPa) and water absorption of 0.3-7.5%. But the resource utilization rate of the process is not high (60%), and the breaking strength and the water absorption rate are reduced to different degrees along with the increase of the adding amount of the ferronickel slag.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a method for preparing enstatite/spinel complex phase microcrystalline glass by using nickel-iron slag, which obtains the density of 3.08g/cm by optimizing the proportion of the nickel-iron slag and fly ash and controlling the crystallization temperature of the microcrystalline glass to induce the directional transformation of the components of the nickel-iron slag 3 The refractory pyroxene/spinel complex phase glass ceramics with 99.97 percent of acid resistance, 99.70 percent of alkali resistance, 116MPa of breaking strength and 8-9 Mohs hardness greatly improve the utilization rate of the nickel-iron slag.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, which comprises the following steps: mixing the nickel-iron slag and the fly ash to obtain a mixture, melting the mixture to obtain a melt, casting and molding the melt, and annealing to obtain base glass; crystallizing the base glass to obtain enstatite/spinel complex-phase glass ceramics;
in the mixture, the mass fraction of the nickel-iron slag is 65-80%;
the nickel-iron slag contains Cr 2 O 3 ；
Cr in the mixture 2 O 3 The mass fraction of (B) is 1.3-1.7 wt%.
The preparation method of the invention adopts the Cr-containing alloy 2 O 3 The ferronickel slag is used as a raw material and is matched with fly ash, the mass fraction of the ferronickel slag is controlled to be 65-80 percent, and the enstatite/spinel complex phase glass ceramics can be prepared 2 O 3 Can be used as natural nucleating agent for promoting microcrystalline glass crystallization, and MgCr 2 O 4 The crystal barrier of the pyroxene phase can be reduced, and the crystallization of the pyroxene phase can be promoted.
In the invention, Cr in the mixture 2 O 3 The mass fraction of (A) needs to be effectively controlled, and if the content is too large, nucleation and crystallization are excessive, so that the comprehensive performance of the product is influenced.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, wherein the mixture comprises the following chemical components in percentage by mass:
SiO 2 49.2-51.0wt％；Al 2 O 3 8.5-13.5wt％；MgO 18.5-23.5wt％；Fe 2 O 3 10-12wt％；CaO 3.0-4.0％wt％；Cr 2 O 3 1.35-1.70wt％。
further preferably, in the mixture, SiO 2 With Al 2 O 3 The sum of the mass fractions of (A) and (B) is 57.7-64.5 wt%.
Further preferably, in the mixture, MgO and Fe 2 O 3 The sum of the mass fractions of (A) is more than 28 wt%.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, wherein the mass fraction of MgO in the nickel-iron slag is more than or equal to 25 wt%.
The invention relates to a method for preparing enstatite/spinel complex phase microcrystalline glass by using nickel-iron slag, wherein 86% or more of the nickel-iron slag has a grain size of less than 0.074 mm.
The invention relates to a method for preparing enstatite/spinel complex phase microcrystalline glass by using nickel-iron slag, wherein the grain diameter of 86 percent or more of the fly ash grains is less than 0.074 mm.
The invention relates to a method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag, wherein the mass fraction of the nickel-iron slag in the mixture is 70-75%.
The invention relates to a method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag,
the melting temperature is 1500-.
In the actual operation process, the mixture is placed in a muffle furnace for heating and melting, wherein the muffle furnace adopts a high-temperature MoSi rod muffle furnace.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag,
the temperature of the melt is 1500-.
In the practical operation of the invention, the temperature of the melt discharged from the furnace is 1550 ℃, namely, the casting molding is directly carried out without cooling.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag,
the mold for casting molding is a stainless steel mold preheated to 200-500 ℃.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag,
the temperature of the annealing treatment is 600-650 ℃, and the time of the annealing treatment is 0.5-2 h.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, wherein the crystallization treatment temperature is 864-907 ℃, the crystallization treatment time is 1-3h, and the temperature rise speed is 4-9 ℃/min, preferably 4-6 ℃/min.
In the invention, the enstatite/spinel complex-phase glass ceramics are obtained by controlling the temperature rise speed and adopting a one-step crystallization method, wherein the crystallization temperature of spinel is 700 plus 900 ℃, and the crystallization temperature of enstatite is 800 plus 1000 ℃, however, the inventor surprisingly discovers that the crystallization temperature is controlled to be between the crystallization temperatures of spinel and enstatite, the separation of a pyroxene phase can be promoted by utilizing spinel, the complex-phase glass ceramics taking enstatite as a main crystal phase and spinel as a strengthening phase can be successfully prepared, and the separation of forsterite is avoided.
Therefore, in the present invention, the temperature and temperature rise rate of the crystallization treatment are required to be controlled effectively, and if the temperature rise rate is too high, crystallization nucleation is insufficient, and a large shrinkage rate is caused. And if the crystallization temperature is too low, the crystal growth is incomplete, and the performance of the material is reduced. The excessive crystallization temperature can cause excessive growth of nuclei, the crystal phases can be connected with each other, an ideal complex phase structure cannot be obtained, the performance is reduced, and meanwhile, the energy consumption is increased due to the high temperature.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, wherein the atmosphere of crystallization treatment is air atmosphere.
The invention relates to a method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag, wherein the density of the enstatite/spinel complex phase glass ceramics is 3.02-3.09g/cm 3 The acid resistance is more than or equal to 99.95 percent, the alkali resistance is more than or equal to 99.51 percent, the breaking strength is 72-116MPa, and the Mohs hardness is 8-9.
Principles and advantages
Because the nickel-iron slag has the characteristics of high magnesium and high iron, the preparation of the enstatite-phase glass ceramics by singly utilizing the nickel-iron slag is difficult to realize from the aspect of target composition, a certain amount of conditioner is generally required to be added to improve a chemical composition system of raw materials, and the mohs hardness of the pyroxene-phase glass ceramics is not high, so that scratches are easily generated in the ordinary use process, and the service life and the decorative effect of the pyroxene-phase glass ceramics are influenced. Meanwhile, with the improvement of the use proportion of the nickel-iron slag, the excessive magnesium oxide can generate forsterite in the crystallization process, so that the mechanical property of the microcrystalline glass is remarkably reduced (such as breaking strength), and the benefit of the nickel-iron slag in the aspect of preparing the microcrystalline glass is greatly limited. At present, the use ratio of the microcrystalline glass prepared from the ferronickel slag is generally 30-50 wt%, so that the ferronickel slag cannot be utilized to the maximum extent, and the cost of the microcrystalline glass is increased.
The invention adopts the Cr-containing alloy 2 O 3 The ferronickel slag is used as a raw material and is matched with the fly ash, and under the condition that the mass ratio of the ferronickel slag reaches 65-80%, the enstatite/spinel complex phase glass ceramics with excellent performance is obtained, and the forsterite is prevented from being separated out.
According to the invention, on one hand, the content of MgO in the mixture is less than 25 wt% by controlling the mutual matching of the nickel-iron slag and the fly ash, on the other hand, the temperature is controlled to be in the middle of the crystallization temperature of spinel and enstatite by controlling the temperature rise speed and adopting a one-step crystallization method, and the spinel is added to promote the precipitation of a pyroxene phase, so that the precipitation of forsterite is avoided.
In the present invention, Cr-containing alloy is used 2 O 3 The ferronickel slag is used as a raw material, and the ferronickel slag contains Cr 2 O 3 Can be used as natural nucleating agent for promoting microcrystalline glass crystallization, and MgCr 2 O 4 The crystal barrier of the pyroxene phase can be reduced, and the crystallization of the pyroxene phase can be promoted. Through the thought, the nickel-iron slag components are induced to realize directional conversion by optimizing the components and controlling crystallization, so that the complex-phase glass ceramics taking enstatite as a main crystal phase and spinel as a strengthening phase is obtained, the performance is excellent, and the standard of China is met.
The method has the advantages of 'treating waste by waste', environmental friendliness and utilization rate of the nickel-iron slag of about 75 percent, not only can well solve the environmental problem caused by the large-scale stockpiling of the nickel-iron slag, but also can prepare the microcrystalline glass with excellent performance. Also in the process of the present invention, Cr 2 O 3 Can be solidified in the spinel, can reduce the adverse effect of chromium in the ferronickel slag on the environment, and in general,the invention has good economic benefit and social benefit.
The invention has the characteristics of simple process, low production cost and environmental friendliness. The pyroxene-spinel complex phase microcrystalline glass prepared by utilizing the nickel-iron slag has the advantages of good chemical stability, high breaking strength and the like, and has good application prospect.
Detailed Description
The present invention will be described in detail with reference to the following specific embodiments, and it is apparent that the embodiments described are only a part of the embodiments of the present invention, rather than the whole embodiments, and all other embodiments obtained by those skilled in the art without inventive labor based on the embodiments of the present invention belong to the protection scope of the present invention.
In order to avoid repetition, the raw materials related to this specific embodiment are described below in a unified manner, and are not described in detail in the specific embodiment:
the ferronickel slag comprises the following components in percentage by mass:
SiO 2 48.25 wt%, MgO 28.32 wt%, Fe 2 O 3 13.92 wt% of Al 2 O 3 2.27 wt%, CaO 3.71 wt%, Cr 2 O 3 The content was 2.09 wt%, and the balance was impurities.
The fly ash comprises the following components in percentage by mass:
SiO 2 53.49 wt%, MgO 0.49 wt%, Fe 2 O 3 2.92 wt% of Al 2 O 3 33.77 wt%, CaO 3.89 wt%, and impurities in balance.
The particle size of the nickel-iron slag is 86% and is less than 0.074 mm.
The particle size of the fly ash is 86% and is less than 0.074 mm.
The chemical stability test (acid resistance and alkali resistance) in the performance of the microcrystalline glass comprises the following test methods:
chemical stability testing the microcrystalline glass samples were placed at 20% H, referenced against standard JC/T2283-2014 2 SO 4 And 20% NaOH solutionHeating in water bath to boiling state for 1 hr. Chemical stability: c ═ m 1 -m 2 )/m 1 X 100% where m 1 Mass m of sample before non-etching 2 The sample mass after corrosion.
Example 1
Uniformly mixing 80 wt% of nickel-iron slag and 20 wt% of fly ash, and melting the mixture into molten glass at a high temperature of 1550 ℃ for 3 h; then taking out of the furnace and casting the stainless steel die preheated to 300 ℃ for cooling and forming, and annealing at 650 ℃ to eliminate stress for 2 h; then cooling the furnace to obtain the base glass.
And putting the prepared base glass into a muffle furnace for heat treatment. Heating to 864 deg.C at a speed of 5 deg.C/min for nucleation, with crystallization time of 2 h; the furnace is cooled to obtain the microcrystal glass with enstatite phase as main crystal phase and spinel phase as strengthening phase.
In this example 1, the enstatite, which is prepared from the ferronickel slag, is used as a main crystal phase, and the spinel is used as a microcrystalline glass of a strengthening phase: density 3.09g/cm 3 99.95 percent of acid resistance, 99.51 percent of alkali resistance, 78MPa of breaking strength and 8-9 percent of Mohs hardness.
Example 2
Uniformly mixing 75 wt% of nickel-iron slag and 25 wt% of fly ash, and melting the mixture into molten glass at a high temperature of 1550 ℃ for 3 h; then taking out of the furnace and casting the stainless steel mold which is preheated to 200-500 ℃ for cooling and forming, and annealing at 650 ℃ for eliminating stress for 2 h; then cooling the furnace to obtain the base glass.
And putting the prepared base glass into a muffle furnace for heat treatment. Heating to 867 ℃ at the speed of 5 ℃/min for crystallization, wherein the crystallization time is 2 h; then, the furnace is cooled to obtain the microcrystalline glass which takes the enstatite phase as a main crystal phase and takes the spinel phase as a strengthening phase.
In this example 2, the enstatite is used as the main crystal phase and the spinel is the microcrystalline glass of the strengthening phase, which is prepared from the ferronickel slag: density 3.08g/cm 3 99.97 percent of acid resistance, 99.70 percent of alkali resistance, 116MPa of breaking strength and 8-9 of Mohs hardness.
Example 3
Uniformly mixing 70 wt% of nickel-iron slag and 30 wt% of fly ash, and melting the mixture into molten glass at a high temperature of 1550 ℃ for 3 h; then taking out of the furnace and casting the stainless steel die preheated to 300 ℃ for cooling and forming, and annealing at 650 ℃ to eliminate stress for 2 h; then cooling the furnace to obtain the base glass.
And putting the prepared base glass into a muffle furnace for heat treatment. Heating to 883 ℃ at the speed of 5 ℃/min for crystallization for 2 h; then, the furnace is cooled to obtain the microcrystalline glass which takes the enstatite phase as a main crystal phase and takes the spinel phase as a strengthening phase.
In this example 3, the enstatite is used as the main crystal phase and the spinel is the glass-ceramic of the strengthening phase, which is prepared from the ferronickel slag: density 3.06g/cm 3 The acid resistance is more than 99.99 percent, the alkali resistance is 99.74 percent, the breaking strength is 101.5MPa, and the Mohs hardness is 8-9.
Example 4
Uniformly mixing 65 wt% of nickel-iron slag and 35 wt% of fly ash, and melting the mixture into molten glass at a high temperature of 1550 ℃ for 3 h; then, taking out the stainless steel die, casting the stainless steel die to 200-500 ℃, cooling and forming, and annealing at 650 ℃ to eliminate stress for 2 h; then cooling the furnace to obtain the base glass.
And putting the prepared base glass into a muffle furnace for heat treatment. Heating to 907 ℃ at the speed of 5 ℃/min for crystallization, wherein the crystallization time is 2 h; then, the furnace is cooled to obtain the microcrystalline glass with the enstatite phase as a main crystal phase and the spinel phase as a strengthening phase.
Example 4 microcrystalline glass prepared from ferronickel slag with pyroxene as the main crystal phase and spinel as the strengthening phase: density 3.02g/cm 3 The acid resistance is more than 99.99 percent, the alkali resistance is 99.89 percent, the breaking strength is 72MPa, and the Mohs hardness is 8-9.
Comparative example 1
The other conditions were the same as in example 1 except that 90 wt% of the ferronickel slag was mixed uniformly with 10 wt% of the fly ash.
Through detection, the microcrystalline glass prepared from the ferronickel slag in the comparative example 1 comprises the following components: density 3.16g/cm 3 99.84 percent of acid resistance, 99.47 percent of alkali resistance and 61MPa of breaking strength.
Comparative example 2
The temperature was raised to 867 ℃ at a rate of 10 ℃/min for crystallization under the same conditions as in example 1.
Through detection, the microcrystalline glass prepared from the ferronickel slag in the comparative example 2 comprises the following steps: density 3.05g/cm 3 99.75 percent of acid resistance, 99.14 percent of alkali resistance and 45MPa of breaking strength.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof, and it is therefore intended that the present embodiments be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the specification describes embodiments, not every embodiment includes only a single embodiment, and such description is for clarity purposes only, and it will be understood by those skilled in the art that the specification as a whole and the embodiments may be suitably combined to form other embodiments as will be apparent to those skilled in the art.
Claims (8)
1. A method for preparing enstatite/spinel complex phase glass ceramics by using nickel-iron slag is characterized in that: the method comprises the following steps: mixing the nickel-iron slag and the fly ash to obtain a mixture, melting the mixture to obtain a melt, casting and molding the melt, and annealing to obtain base glass; crystallizing the base glass to obtain enstatite/spinel complex-phase glass ceramics;
in the mixture, the mass fraction of the nickel-iron slag is 70-75%;
the nickel-iron slag contains Cr 2 O 3 ；
The mixture comprises the following chemical components in percentage by mass:
SiO 2 49.2-51.0wt%；Al 2 O 3 8.5-13.5wt%；MgO 18.5-23.5wt%；Fe 2 O 3 10-12wt%；CaO 3.0-4.0%wt%；Cr 2 O 3 1.35-1.70wt%；
the temperature of the crystallization treatment is 864-907 ℃, the time of the crystallization treatment is 1-3h, and the temperature rise speed is 4-9 ℃/min.
2. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that:
the particle size of more than 86% of the particle sizes of the ferronickel slag particles is less than 0.074 mm;
the grain diameter of more than 86% of the grain diameters of the fly ash grains is less than 0.074 mm.
3. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that:
in the mixture, the mass fraction of the nickel-iron slag is 70-75%.
4. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that: the melting temperature is 1500-.
5. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that: the temperature of the melt is 1500-.
6. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that: the die for casting molding is a stainless steel die preheated to 200-500 ℃.
7. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that: the temperature of the annealing treatment is 600-650 ℃, and the time of the annealing treatment is 0.5-2 h.
8. The method for preparing enstatite/spinel complex-phase glass ceramics by using nickel-iron slag according to claim 1, which is characterized in that: the atmosphere of the crystallization treatment is an air atmosphere.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3002346A1 (en) * | 1980-01-23 | 1981-08-13 | Licencia Találmányokat Ertékesítö Vállalat, Budapest | METHOD FOR PRODUCING MELTED SILICATE MATERIALS |
| CN106673448A (en) * | 2016-12-21 | 2017-05-17 | 江苏省冶金设计院有限公司 | Diopside ceramic glass prepared from chromic slag and coal gangue and preparation method of diopside ceramic glass |
| CN107935555A (en) * | 2017-12-13 | 2018-04-20 | 北京科技大学 | A kind of ferronickel slag ceramics and preparation method thereof |
| CN109399940A (en) * | 2018-12-10 | 2019-03-01 | 兰州理工大学 | A kind of preparation method of nickel slag microcrystalline glass |
| CN109399941A (en) * | 2018-12-21 | 2019-03-01 | 河北工业大学 | A method of micro-crystalline ceramic is prepared using flyash and waste slag |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101020968A (en) * | 2006-12-29 | 2007-08-22 | 金川集团有限公司 | Process of comprehensively utilizing high temperature nickel smelting slag |
| CN103553333B (en) * | 2013-11-11 | 2016-03-30 | 武汉理工大学 | Rich iron nickel slag microcrystalline glass and preparation method |
| CN105063362B (en) * | 2015-08-26 | 2017-03-22 | 西南科技大学 | Preparation method for active nickel iron residues |
| CN112125516B (en) * | 2020-09-21 | 2023-04-07 | 西安鹏远冶金设备有限公司 | Additive and method for preparing microcrystalline glass from iron-containing nickel slag |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3002346A1 (en) * | 1980-01-23 | 1981-08-13 | Licencia Találmányokat Ertékesítö Vállalat, Budapest | METHOD FOR PRODUCING MELTED SILICATE MATERIALS |
| CN106673448A (en) * | 2016-12-21 | 2017-05-17 | 江苏省冶金设计院有限公司 | Diopside ceramic glass prepared from chromic slag and coal gangue and preparation method of diopside ceramic glass |
| CN107935555A (en) * | 2017-12-13 | 2018-04-20 | 北京科技大学 | A kind of ferronickel slag ceramics and preparation method thereof |
| CN109399940A (en) * | 2018-12-10 | 2019-03-01 | 兰州理工大学 | A kind of preparation method of nickel slag microcrystalline glass |
| CN109399941A (en) * | 2018-12-21 | 2019-03-01 | 河北工业大学 | A method of micro-crystalline ceramic is prepared using flyash and waste slag |
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