CN113200682A - Method for preparing microcrystalline glass by adopting ferrochrome slag - Google Patents
Method for preparing microcrystalline glass by adopting ferrochrome slag Download PDFInfo
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- CN113200682A CN113200682A CN202110390240.7A CN202110390240A CN113200682A CN 113200682 A CN113200682 A CN 113200682A CN 202110390240 A CN202110390240 A CN 202110390240A CN 113200682 A CN113200682 A CN 113200682A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- 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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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B32/00—Thermal after-treatment of glass products not provided for in groups C03B19/00, C03B25/00 - C03B31/00 or C03B37/00, e.g. crystallisation, eliminating gas inclusions or other impurities; Hot-pressing vitrified, non-porous, shaped glass products
- C03B32/02—Thermal crystallisation, e.g. for crystallising glass bodies into glass-ceramic articles
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- 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
- C03C10/0036—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 SiO2, Al2O3 and a divalent metal oxide as main constituents
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Abstract
The invention discloses a method for preparing microcrystalline glass by adopting ferrochrome slag, which relates to the technical field of microcrystalline glass preparation, and comprises the following steps: s1, respectively drying, crushing and sieving the ferrochromium slag and the quartz sand to obtain ferrochromium slag powder and quartz sand powder; s2, mixing the ferrochrome slag powder and the quartz sand powder, placing the mixture in a high-temperature atmosphere furnace for heating and temperature rise, preserving heat to prepare uniform glass liquid, and performing water quenching to prepare water-quenched base glass; s3, crushing, screening, drying and grinding the water-quenched base glass into powder, carrying out DSC test, and measuring the crystallization temperature; and S4, grinding the water-quenched base glass into powder, sieving, pressing to obtain a rectangular sample, sintering, preserving heat, cooling to a crystallization temperature, preserving heat for the second time, and cooling to obtain the microcrystalline glass.
Description
Technical Field
The invention relates to the technical field of microcrystalline glass preparation, in particular to a method for preparing microcrystalline glass by using ferrochrome slag.
Background
Ferrochrome is the most important raw material for producing stainless steel, and the chromium content of the stainless steel is generally not lower than 12 percent. And 1-1.2 t of waste residue is generated when 1t of ferrochrome is produced. With the development of the stainless steel industry, the quantity of ferrochrome slag is continuously increased every year, which not only occupies cultivated land and wastes land resources, but also causes environmental pollution.
Chromium in the ferrochromium slag belongs to heavy metal elements and is easy to generate valence change, and the heavy metal chromium usually exists in a trivalent state and a hexavalent state, wherein the trivalent chromium is nontoxic and is one of trace elements required by human bodies; however, hexavalent chromium has strong oxidizing property and carcinogenicity, and causes harm to human health and pollution to the ecological environment. Although the spinel phase in the ferrochrome slag has certain chromium fixing capacity, the activity of chromium in the slag is greatly reduced, if the ferrochrome slag is piled in nature for a long time, the residual Cr2O3At the interface in contact with CaO, Cr3+Will diffuse across the interface and O across the interface2Forming CaCrO with CaO4(Cr6+) Every 6-9 months, one gram of Cr in the chromium6+The content was increased by 1000-10000. mu.g. The generated calcium chromate can permeate into underground water circulation along with rainwater under the action of long-term rainwater erosion corrosion. And the rest of Cr2O3The interface with CaO is regenerated, and the process is continuously circulated.
Therefore, finding a clean method to comprehensively utilize the ferrochrome slag to produce materials with high added values has extremely important effects on energy conservation, emission reduction and environmental protection.
Glass-ceramic (glass-ceramic) is a polycrystalline material containing a large number of microcrystalline phases and glass phases, which is prepared by controlling crystallization of base glass with a specific composition in a heating process. The building decoration microcrystalline glass basically belongs to CaO-SiO2-MgO-Al2O3System, diopside [ CaMg (SiO)3)2]And wollastonite (CaSiO)3) Is generally the glassThe main crystalline phase of the glass system. CaO and SiO in low-carbon ferrochrome slag2、MgO、Al2O3The four components account for more than 90% of the total mass of the alloy, and also contain a small amount of Cr2O3、Fe2O3And FeO, which is just an effective nucleating agent component for preparing the slag glass ceramics. Therefore, the ferrochrome slag is used for preparing CaO-SiO2-MgO-Al2O3Is an ideal raw material for the microcrystalline glass.
The glass phase of the microcrystalline glass and the crystalline phase have good curing effect on heavy metal chromium ions, and the heavy metal can be effectively cured in the service process, so that the leaching of the chromium ions is reduced. Therefore, the low-carbon ferrochrome slag as a resource of 'misplaced' can be completely and comprehensively utilized by preparing an environment-friendly high-performance glass-ceramic material, the additional value of the low-carbon ferrochrome slag is improved, and the low-carbon ferrochrome slag is an effective way for reducing the problem of environmental pollution, is beneficial to the sustainable development of the metallurgical industry, and promotes the construction of waste-free cities and green water mountains in China.
At present, the preparation method of ferrochrome slag microcrystalline glass mostly adopts a melting method and rarely adopts a sintering method. This is because the solid waste material of ferrochrome slag contains Cr as a nucleating agent for promoting glass crystallization2O3The volume crystallization capability is very strong, and the common sintering method is not easy to sinter and form.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for preparing microcrystalline glass by using ferrochrome slag. The method provided by the invention adopts a heat treatment mode of sintering before crystallization, solves the problems of over-strong volume crystallization capability and difficult sintering and forming in the process of preparing the microcrystalline glass by the ferrochrome slag sintering method, and ensures that the production process of the microcrystalline glass is easy to control and easy to realize mechanization and automation. The solid-to-waste ratio of the low-carbon ferrochrome slag in the raw materials adopted by the method provided by the invention reaches more than 70%, the prepared microcrystalline glass has a smooth surface, basically has no deformation in the sintering process, the breaking strength is more than 70MPa and up to 125MPa, the main crystal phases are diopside, common pyroxene and wollastonite, compared with the traditional building materials of marble and granite, the breaking strength is obviously improved, the hardness is equivalent to the density, the absorptivity is slightly high, the acid resistance is better, the alkali resistance is slightly poor, the comprehensive performance is better than that of the traditional building materials, and the microcrystalline glass can be used as a substitute of natural building materials.
The specific method comprises the following steps:
(1) base glass formulation design
Taking low-carbon ferrochrome slag as a main raw material, quartz sand as a modifier, and taking CaO-SiO with MgO content of 5 percent as reference2-Al2O3And (3) selecting basic glass composition points in wollastonite and pyroxene areas by a ternary system phase diagram, and designing a basic glass formula by combining Factsage thermodynamic calculation to ensure that the basic glass is separated out to have wollastonite and pyroxene as main crystal phases.
The invention comprises the following raw materials in percentage by mass: ferrochrome slag: 72-74 wt%, quartz sand: 26 to 28 weight percent.
(2) Proportioning, melting and water quenching of base glass
And (3) putting the low-carbon ferrochrome slag and the quartz sand into a drying box for drying, crushing by using a roller ball mill, and sieving by using a 200-mesh sieve. Accurately weighing low-carbon ferrochrome slag and quartz sand according to a designed basic glass formula, and placing the low-carbon ferrochrome slag and the quartz sand in a clean and dry mixing tank for mixing for 3 hours to achieve uniform components. And putting the fully and uniformly mixed mixture into a clean corundum crucible, heating the mixture to 1500 ℃ from room temperature in a high-temperature atmosphere furnace with controllable temperature, preserving the heat for 3 hours to fully melt and clarify the mixture to obtain uniform molten glass, taking out the corundum crucible, and quickly pouring the molten glass into water for water quenching to obtain the water-quenched base glass.
(3) Determination of crystallization temperature of base glass
Crushing, screening and drying the water-quenched base glass, grinding the water-quenched base glass into powder, putting the powder into a corundum crucible of an STA + PT1600 type comprehensive thermal analyzer, heating to 1200 ℃ at a heating rate of 10 ℃/min under an argon atmosphere, determining the crystallization temperature of the glass according to a differential thermal analysis result (DSC), and providing a theoretical basis for determining a heat treatment system for preparing the microcrystalline glass by a sintering method.
(4) Heat treatment process
Grinding the water-quenched base glass into powder, sieving the powder by a 200-mesh sieve, controlling the sample preparation pressure to be 2-6MPa, pressing the powder into a rectangular strip sample with the thickness of 4mm multiplied by 40mm, and specifically sintering technological parameters: the temperature is below 1000 ℃, and the heating rate is 15 ℃/min; the temperature is increased to 1195 ℃ with the temperature rise rate of 10 ℃/min to 1185 ℃ with the sintering temperature, the temperature is kept for 4 to 6min, then the temperature is reduced to 1003 ℃ with the temperature drop rate of 5 ℃/min with the crystallization temperature, the temperature is kept for 55 to 65min, and the microcrystalline glass is prepared after the temperature is cooled to the room temperature along with the furnace after the power failure.
The invention has the beneficial effects that:
(1) the method provided by the invention adopts a heat treatment mode of sintering before crystallization, solves the problems of over-strong volume crystallization capability and difficult sintering and forming in the process of preparing the microcrystalline glass by the ferrochrome slag sintering method, and ensures that the production process of the microcrystalline glass is easy to control and easy to realize mechanization and automation. The solid-to-waste ratio of the low-carbon ferrochrome slag in the raw materials adopted by the method provided by the invention reaches more than 70%, the prepared microcrystalline glass has a smooth surface, basically has no deformation in the sintering process, the breaking strength is more than 70MPa and up to 125MPa, the main crystal phases are diopside, common pyroxene and wollastonite, compared with the traditional building materials of marble and granite, the breaking strength is obviously improved, the hardness is equivalent to the density, the absorptivity is slightly high, the acid resistance is better, the alkali resistance is slightly poor, the gray green color is realized, the comprehensive performance is better than that of the traditional building materials, and the microcrystalline glass can be used as a substitute of natural building materials.
(2) The method provided by the invention adopts a new sintering method to convert the ferrochrome slag into a new environment-friendly high-added-value glass-ceramic material, has comprehensive performance superior to that of the traditional building material, can be used as a substitute of a natural building material, and simultaneously solidifies heavy metal chromium ions in the ferrochrome slag, thereby reducing environmental pollution and being beneficial to the sustainable development of the metallurgical industry.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or portions are generally identified by like reference numerals. In the drawings, elements or portions are not necessarily drawn to scale.
FIG. 1 is a graph showing the differential thermal curves of base glasses # 1 and # 2 prepared in the examples;
FIG. 2 is a graph showing the differential thermal curves of base glasses # 3 and # 4 obtained in the examples;
FIG. 3 is a graph showing the differential thermal curves of base glasses # 5 and # 6 obtained in the examples;
FIG. 4 is an XRD spectrum of microcrystalline glass # 1-6 prepared by the example;
FIG. 5 is an SEM photograph of a crystallized glass 1# obtained in example;
FIG. 6 is an SEM photograph of a crystallized glass 2# obtained in example;
FIG. 7 is an SEM photograph of a crystallized glass No. 3 obtained in example;
FIG. 8 is an SEM photograph of a crystallized glass No. 4 obtained in example;
FIG. 9 is an SEM photograph of a crystallized glass 5# obtained in example;
fig. 10 is an SEM photograph of glass ceramics 6# obtained in example.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Examples
1. Crushing the ferrochromium slag and the quartz sand, and sieving by a 200-mesh sieve to obtain ferrochromium slag powder and quartz sand powder.
2. Accurately weighing ferrochrome slag powder and quartz sand powder according to the mass proportion in the table 1, mixing in a mixer for 3 hours to obtain mixed raw materials, weighing 400g of the mixed raw materials, filling the mixed raw materials into a corundum crucible, placing the corundum crucible into a silicon-molybdenum rod electric furnace, heating to 1500 ℃ in air atmosphere, melting for 3 hours to form uniform glass liquid, taking out the crucible, rapidly pouring the crucible into cooling water at room temperature, and carrying out water quenching treatment to obtain water-quenched base glass No. 1-6;
3. crushing, screening, drying and grinding the water-quenched base glass No. 1-6 into powder, respectively taking a small amount of the powder to perform differential thermal analysis, wherein differential thermal analysis (DSC) curves are respectively shown in figures 1-3, and the crystallization temperature in the preparation process of the microcrystalline glass is respectively the exothermic peak temperature of the DSC curve: 1003 deg.C, 1000 deg.C, 995 deg.C.
Wherein, the DSC curves of 1# and 2# are shown in figure 1; the DSC curves of # 3 and # 4 are shown in FIG. 2; the DSC curves of # 5 and # 6 are shown in FIG. 3;
4. grinding the water-quenched base glass into powder with different particle sizes, sieving, pressing under different sample preparation pressures, sintering, maintaining the temperature, cooling to crystallization temperature, maintaining the temperature for the second time, and cooling to obtain microcrystalline glass No. 1-6.
Wherein the conditions of sintering, crystallization temperature and the like are respectively according to the heat treatment process parameters in the table 2 to prepare the microcrystalline glass from No. 1 to No. 6.
TABLE 1 raw material proportions and chemical composition of base glasses
TABLE 2 examples Heat treatment Process parameters
Test examples
The physical and chemical properties of the microcrystalline glass No. 1-6 prepared in the examples were measured
Table 3 shows the performance data of the microcrystalline glass 1# -6# prepared by the experiment and the traditional building materials of marble and granite. The data of marble with 'Tuo' in the table is from GB/T19766-; the data of the granite band "+" are from GB/T18601-.
TABLE 3 comparison of the physical and chemical properties of the microcrystalline glass sample in the examples with those of conventional building materials
The method for testing the physical and chemical properties comprises the following steps:
(1) measurement of flexural Strength
The microcrystalline glass samples 1# -6# prepared in the examples (length 40mm, width 4mm, height 4mm) were subjected to surface grinding and then to test on an electronic universal tester with a span of 30mm, a loading speed set at 0.5mm/min, each group of samples was tested three times, and the breaking strength was calculated by taking the average value according to the following formula:
in the formula: sigma-the flexural strength of the sample, MPa;
p-the load to which the specimen is subjected when it breaks, N;
l-sample span, mm;
b-fracture width, mm;
h-fracture height, mm.
(2) Measurement of hardness
The smooth surfaces of the samples of the microcrystalline glass No. 1-6 prepared in the examples are scribed by a Mohs hardness pen by adopting a scratching method, and if the samples are not scratched, the hardness of the samples of the microcrystalline glass is higher than the hardness value; if a scratch occurs, it indicates that the hardness of the microcrystalline glass sample is lower than the hardness value. Specific hardness values are compared to ten minerals as shown in table 4.
The method comprises the following specific operation steps: the glass ceramic sample is placed on a hard support smoothly with the smooth side facing upwards. The surface of the sample is scribed by Mohs pens with different Mohs values from small to large, and the force is moderate but not too large or too small. The lowest hardness value which just can generate obvious scratches is taken as a detection result, and the minimum value tested by each group of samples is taken as a test result.
TABLE 4 Mohs hardness Standard control Table
(3) Density determination
The density of the microcrystalline glass sample No. 1-6 prepared in the example was measured by the drainage method. First, a sample is weighed and placed in a50 mL volumetric flask with a previously calibrated volume, and titrated with a50 mL burette. When the liquid level in the volumetric flask reaches 50mL of scale mark, the volume of the residual liquid is directly read from the burette, namely the volume of the sample. The density is calculated according to the following formula:
in the formula: rho-density of the sample, g/mL;
m-mass of sample, g;
v-volume of liquid remaining in burette, mL.
(4) Water absorption measurement
The microcrystalline glass # 1-6 prepared in the examples was cut into samples of the same size by a disc cutter, the cut samples were placed in a drying oven, dried for 1 hour, weighed, immersed in deionized water at room temperature for 7 days, wiped to dry the surface, placed on an electronic balance to read the value, and then substituted into the following formula to calculate the water absorption.
In the formula: water absorption of the W-sample,%;
m1-mass of sample before water absorption, g;
m2mass after water absorption of the sample, g.
(5) Acid (alkali) resistance measurement
The microcrystalline glass No. 1-6 prepared in the example was cut into samples of the same size by a disc cutter, the cut samples were placed in a drying oven, dried for 1 hour and then weighed, and the samples were placed in a prepared 1% wtH2SO4The solution and 1% wtNaOH solution were etched for 3 days, and the surface was wiped dry and then placed on an electronic balance to read the value, and then substituted into the following formula to calculate the acid (base) resistance.
In the formula: w-corrosion rate of sample,%;
m1-post-corrosion mass, g;
m2-mass before corrosion, g.
(6) Determination of mineral composition and microstructure
The main crystal phases of the microcrystalline glasses 1# -6# prepared in the examples were examined by an X-ray diffractometer, and the microstructure thereof was examined by a scanning electron microscope.
The specific operating conditions are as follows: XRD analysis is carried out on the 1# to 6# samples of the microcrystalline glass after heat treatment by adopting an X' Pert PRO diffractometer of Philips, Netherlands, and the mineral composition of the 1# to 6# samples of the microcrystalline glass is measured, wherein the working voltage is 40Kv, and the working current is 80 mA. The scanning angle range is set to be 20-80 degrees, and the scanning angular speed is 2 degrees/min. XRD detection results of the microcrystalline glasses 1# -6# prepared in the examples are shown in FIG. 4;
the microstructure of the 1# -6# sample of the microcrystalline glass is observed by a German Zeiss Sigma500 field emission scanning electron microscope, and the preparation process of the sample comprises the following steps: cutting, grinding and polishing the section, then corroding in 5 percent by mass of HF acid for 30s, cleaning with distilled water, spraying gold, and observing the microstructure, wherein SEM results of No. 1-6 of the microcrystalline glass prepared in the example are shown in figures 5-10.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; such modifications and substitutions do not depart from the spirit and scope of the present invention, and they should be construed as being included in the following claims and description.
Claims (10)
1. A method for preparing microcrystalline glass by using ferrochrome slag is characterized by comprising the following steps: the method comprises the following steps: s1, respectively drying, crushing and sieving the ferrochromium slag and the quartz sand to obtain ferrochromium slag powder and quartz sand powder; s2, mixing the ferrochrome slag powder and the quartz sand powder, placing the mixture in a high-temperature atmosphere furnace for heating and temperature rise, preserving heat to prepare uniform glass liquid, and performing water quenching to prepare water-quenched base glass; s3, crushing, screening, drying and grinding the water-quenched base glass into powder, carrying out DSC test, and measuring the crystallization temperature; and S4, grinding the water-quenched base glass into powder, sieving, pressing to obtain a rectangular sample, sintering, preserving heat, cooling to a crystallization temperature, preserving heat for the second time, and cooling to obtain the microcrystalline glass.
2. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S1, the sieving is 200 mesh sieving.
3. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S2, the mixing is performed for 3 hours at a stirring speed of 60-80 rpm.
4. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S2, the heating temperature is increased to 1500 ℃, and the temperature is maintained for 3 hours.
5. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S2, the mass ratio of the ferrochrome slag powder to the quartz sand powder is 72-74: 26-28.
6. The method for preparing the glass-ceramic by adopting the ferrochrome slag according to claim 1, which is characterized in that: in step S3, the instrument used for DSC measurement is STA + PT1600 type comprehensive thermal analyzer, and the DSC measurement is performed under an argon atmosphere at a temperature rise rate of 10 ℃/min up to 1200 ℃.
7. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S4, the sieving is 200 mesh sieving, and the pressure for pressing is 2-6 Mpa.
8. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S4, the rectangular sample has dimensions of 4mm × 4mm × 40 mm.
9. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S4, the sintering conditions are that the temperature is raised to 1000 ℃ at a heating rate of 15 ℃/min, and the temperature is raised to 1185-1195 ℃ at a heating rate of 10 ℃/min.
10. The method for preparing glass ceramics by using ferrochrome slag according to claim 1, which is characterized in that: in step S4, the heat preservation is carried out for 4-6 min; the temperature is reduced to the crystallization temperature of 995-1003 ℃ at a cooling rate of 5 ℃/min; and the second heat preservation is heat preservation for 55-65 min.
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| CN101914639A (en) * | 2010-09-08 | 2010-12-15 | 北京科技大学 | Method for recycling iron on line from iron-containing industrial slag and preparing glass ceramics frit |
| CN102211874A (en) * | 2011-05-10 | 2011-10-12 | 北京科技大学 | Microcrystalline glass and preparation method thereof |
| CN108059351A (en) * | 2017-12-14 | 2018-05-22 | 北京工业大学 | A kind of method that sintering process prepares rich iron lead skim devitrified glass |
| CN111908796A (en) * | 2020-08-28 | 2020-11-10 | 江西鼎盛新材料科技有限公司 | Tailing slag microcrystalline glass and production method thereof |
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