CN113087398A - Microcrystalline glass prepared from coal gasification furnace slag and preparation method thereof - Google Patents
Microcrystalline glass prepared from coal gasification furnace slag and preparation method thereof Download PDFInfo
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- CN113087398A CN113087398A CN202110394042.8A CN202110394042A CN113087398A CN 113087398 A CN113087398 A CN 113087398A CN 202110394042 A CN202110394042 A CN 202110394042A CN 113087398 A CN113087398 A CN 113087398A
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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
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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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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Abstract
The invention discloses a microcrystalline glass prepared from coal gasification furnace slag and a preparation method thereof, wherein the microcrystalline glass comprises the following components in parts by weight: 60-90% of coal gasification furnace slag and 10-40% of additive powder, wherein the additive powder is a mixture of red mud, ilmenite and limestone; the preparation method comprises the steps of grinding and sieving the slag of the gas furnace, preheating at 980 ℃ under 900-; pouring the basic glass liquid into a preheated mold, demoulding after molding to obtain basic glass, and carrying out microcrystallization treatment on the basic glass to obtain the microcrystalline glass. The method for preparing green microcrystals by using the coal gasification furnace slag as the main raw material for the first time has the coal gasification furnace slag content of more than 60 percent, can effectively utilize the coal gasification furnace slag, can solve the problem of environmental pollution caused by the discharge of the coal gasification furnace slag, can obtain good economic benefit, and opens up a sustainable development road for the coal chemical industry.
Description
Technical Field
The invention belongs to the technical field of inorganic non-metallic materials, and particularly relates to microcrystalline glass prepared from coal gasification furnace slag and a preparation method thereof.
Background
Glass ceramics are a class of solid composite materials containing both a glass phase and a microcrystalline phase prepared by targeted controlled crystallization of a base glass. Compared with the glass and the ceramic with the same components, the microcrystalline glass has the characteristics of high mechanical strength, high hardness, good wear resistance, good chemical stability, excellent thermal stability, excellent electrical insulation performance and the like, and is widely applied to the fields of buildings, electronics, chemical industry, biology, medicine, military and the like. The microcrystalline glass is prepared by taking various metallurgical waste residues, industrial tailings and wastes of coal-fired power plants as main raw materials, so that not only are waste resources recycled, but also the environmental pollution is reduced, and good economic benefits are obtained.
The coal gasification furnace slag is solid waste which is generated by coal chemical industry and mainly comprises amorphous glass bodies. In recent years, with the rapid development of coal chemical industry, the output of coal gasification slag is increasing. The accumulation of a large amount of coal gasification slag causes a series of serious environmental pollution problems. At present, the application research of the coal gasification slag is less, the coal gasification slag is mainly used as a raw material of building materials and ceramic products, but the coal gasification slag has poor activity and contains more residual carbon, so that the two applications are difficult to apply, and the large-scale production is not realized. Therefore, research on finding a new utilization method of the coal gasification slag is urgent.
Disclosure of Invention
Aiming at the problems of few application researches of the coal gasification furnace slag and resource waste in the prior art, the invention provides the microcrystalline glass prepared from the coal gasification furnace slag and the preparation method thereof, wherein the content of the coal gasification furnace slag is more than 60 percent, the coal gasification furnace slag can be effectively utilized, the environmental problem caused by the discharge of the coal gasification furnace slag can be solved, good economic benefit can be obtained, and a sustainable development road is opened up for the coal chemical industry.
The invention is realized by the following technical scheme:
the microcrystalline glass prepared from coal gasification furnace slag is characterized by comprising the following components in percentage by weight: 60-90% of coal gasification furnace slag and 10-40% of additive powder;
the additive powder is a mixture of red mud, ilmenite and limestone.
Furthermore, the mass ratio of the red mud, the ilmenite and the limestone in the additive powder is 4-8: 1-3.
The preparation method of the microcrystalline glass comprises the following steps:
(1) grinding and sieving the slag of the gas furnace, and then carrying out preheating treatment at the temperature of 900-;
(2) mixing the preheated gas furnace slag fine material and the additive powder, mixing and granulating to uniformly mix the materials, simultaneously avoiding the problem of material dusting caused by large temperature difference in the process of adding the materials into a hearth and preventing the components with large density difference from layering in a pot in the melting process, then melting at high temperature of 1500-;
(3) pouring the base glass liquid prepared in the step (2) into a preheated mold, demolding to obtain base glass, carrying out heat treatment on the base glass, and then annealing and cooling to room temperature to obtain the microcrystalline glass.
Further, the heat treatment method of the base glass comprises the following steps: the base glass is heated to the nucleation temperature of 960 ℃ at the speed of 11 ℃/min, the nucleation time is 3h, and then the temperature is heated to 980 ℃ for crystallization, and the crystallization time is 3 h.
Further, the particle size of the fine slag of the coal gas furnace after sieving in the step (1) is 100 meshes.
Further, the granulation in the step (2) adopts an agglomeration type granulation method, and the particle size is 1 cm.
Further, the preheating temperature of the mold in the step (3) is 380 ℃.
Further, the annealing cooling rate in the step (3) is 1.5 ℃/min.
Advantageous effects
The method for preparing green microcrystals by using the coal gasification furnace slag as the main raw material for the first time has the coal gasification furnace slag content of more than 60 percent, can effectively utilize the coal gasification furnace slag, can solve the problem of environmental pollution caused by the discharge of the coal gasification furnace slag, can obtain good economic benefit, and opens up a sustainable development road for the coal chemical industry.
Drawings
Fig. 1 is an XRD spectrum of the crystallized glass prepared in example 1 of the present invention;
fig. 2 is a scanning electron microscope picture of the microcrystalline glass prepared in example 1 of the present invention.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention in conjunction with the following examples, but it will be understood that the description is intended to illustrate the features and advantages of the invention further, and not to limit the invention.
Pretreatment of coal gasification furnace slag:
example 1
(1) Grinding coal gasification furnace slag to obtain fine materials with the granularity of 100 meshes, and preheating the coal gasification furnace slag in a muffle furnace at the treatment temperature of 950 ℃; the pretreated coal gasification furnace slag comprises the following components:
CaO 9.67%，SiO2 51.96%，Al2O3 16.89%，MgO 0.83%，TiO2 1.22%，K2O 2.64%，Na2O 0.63%，Fe2O3 12.42%，SO3 2.53%；
(2) weighing 80g of coal gasification furnace slag subjected to preheating treatment in the step (1) and 20g of additive powder (14 g of red mud, 4g of ilmenite and 2g of limestone), uniformly mixing, granulating the mixture by adopting an agglomeration type granulation method, wherein the particle size is 1cm, then feeding the mixture into a high-temperature electric furnace at the temperature of 1550 ℃ for melting, and preserving heat for 20 hours to obtain base glass liquid;
(3) pouring the basic glass liquid obtained in the step (1) into a forming die preheated to 380 ℃, demoulding after forming to obtain basic glass, placing the basic glass into a muffle furnace, heating to 960 ℃ at a heating rate of 11 ℃/min, preserving heat for 3h, continuously heating to 980 ℃, preserving heat for 3h, and annealing to room temperature at 1.5 ℃/min after heat treatment is finished to obtain a microcrystalline glass finished product.
The XRD spectrum of the glass ceramic prepared in this example is shown in fig. 1, and it can be seen from fig. 1 that the glass ceramic prepared in this example precipitates a predominant crystalline phase of spodumene, and a minor crystalline phase of gehlenite and wollastonite; as shown in fig. 2, the SEM image shows that the microcrystalline glass has high crystallinity, uniform crystal grain distribution, and dense arrangement, as shown in fig. 2.
Example 2:
as described in example 1, except that the preheating temperature for the pretreatment in step (1) was 900 ℃.
Example 3
As described in example 1, except that the pre-heating temperature for the pre-treatment in step (1) was 980 ℃.
Example 4
The process is carried out as described in example 1, except that 60g of the coal gasification slag pretreated in step (3) and 20g of the additive are used.
Example 5
The process is carried out as described in example 1, except that 90g of the coal gasification slag pretreated in step (3) and 10g of the additive were used.
Example 6
As described in example 1, except that the melting temperature in step (3) was 1500 ℃.
Example 7
As described in example 1, except that the melting temperature in step (3) was 1600 ℃.
Example 8
The process was carried out as described in example 1, except that the holding time in step (3) was 18 hours.
Example 9
The difference was that the incubation time in step (3) was 24 hours, as described in example 1.
Comparative example 1
(1) Grinding coal gasification furnace slag to obtain fine materials with the granularity of 100 meshes, and preheating the coal gasification furnace slag in a muffle furnace at the treatment temperature of 950 ℃; the pretreated coal gasification furnace slag comprises the following components:
CaO 9.67%，SiO2 51.96%，Al2O3 16.89%，MgO 0.83%，TiO2 1.22%，K2O 2.64%，Na2O 0.63%，Fe2O3 12.42%，SO3 2.53%；
(2) weighing 80g of coal gasification furnace slag subjected to preheating treatment in the step (1) and 20g of additive powder (14 g of red mud, 4g of ilmenite and 2g of limestone), uniformly mixing, then feeding into a high-temperature electric furnace at 1550 ℃ for melting, and preserving heat for 20 hours to obtain base glass metal;
(3) pouring the basic glass liquid obtained in the step (1) into a forming die preheated to 380 ℃, demoulding after forming to obtain basic glass, placing the basic glass into a muffle furnace, heating to 960 ℃ at a heating rate of 11 ℃/min, preserving heat for 3h, continuously heating to 980 ℃, preserving heat for 3h, and annealing to room temperature at 1.5 ℃/min after heat treatment is finished to obtain a microcrystalline glass finished product.
Comparative example 2
(1) Grinding coal gasification furnace slag to obtain fine materials with the granularity of 100 meshes, and preheating the coal gasification furnace slag in a muffle furnace at the treatment temperature of 950 ℃; the pretreated coal gasification furnace slag comprises the following components: CaO 9.67%, SiO251.96%，Al2O3 16.89%，MgO 0.83%，TiO2 1.22%，K2O 2.64%，Na2O 0.63%，Fe2O3 12.42%，SO32.53%；
(2) Weighing 80g of coal gasification furnace slag subjected to preheating treatment in the step (1) and 20g of additive powder (16 g of red mud and 4g of ilmenite), uniformly mixing, granulating the mixture by adopting an agglomeration granulation method, wherein the particle size of the mixture is 1cm, then feeding the mixture into a high-temperature electric furnace at the temperature of 1550 ℃ for melting, and preserving heat for 20 hours to obtain base glass liquid;
(3) pouring the base glass liquid obtained in the step (1) into a forming die preheated to 380 ℃, demoulding after forming to obtain base glass, placing the base glass into a muffle furnace, heating to 960 ℃ at a heating rate of 11 ℃/min, preserving heat for 3h, continuously heating to 980 ℃, preserving heat for 3h, annealing to room temperature at 1.5 ℃/min after heat treatment is finished, and obtaining a finished product of the microcrystalline glass.
Performance detection
The microcrystalline glasses prepared in examples 1 to 9 and comparative examples 1 and 2 were examined for flexural strength, acid resistance and alkali resistance.
(1) Flexural Strength test
The test method is a three-point bending method, the size of a test sample is 3mm multiplied by 4mm multiplied by 40mm, the span is 30mm, and the loading speed of 0.5mm multiplied by S-1 is selected. The formula for calculating the breaking strength of the microcrystalline glass is as follows:
in the formula: p-load, N;
l-span, mm;
b-width of the fracture in mm;
h-height of fracture, mm.
(2) And (3) testing acid resistance:
a18 mm by 18mm standard sample was subjected to ultrasonic cleaning and drying, and then weight recording was performed (G)1) Adding 1% by volume of H2SO4And sealing the solution by using a preservative film, and corroding for 24 hours. After the corrosion was completed, the sample was ultrasonically cleaned, dried and then weighed (G)2). The quality of the chemical stability (C) is judged by calculating the mass loss rate of the sample before and after corrosion, and the calculation formula is as follows:
in the formula: c-chemical stability;
G1-pre-corrosion specimen mass (mg);
G2sample mass after corrosion (mg).
(3) Alkali resistance test
A18 mm by 18mm standard sample was subjected to ultrasonic cleaning and drying, and then weight recording was performed (G)1) And adding a sodium hydroxide solution with the mass fraction of 1% and sealing by using a preservative film, wherein the corrosion time is 24 hours. After the corrosion was completed, the sample was ultrasonically cleaned, dried and then weighed (G)2). The quality of the chemical stability (C) is judged by calculating the mass loss rate of the sample before and after corrosion, and the calculation formula is as follows:
in the formula: c-chemical stability;
G1-pre-corrosion specimen mass (mg);
G2sample mass after corrosion (mg).
The results of testing the breaking strength, acid resistance and alkali resistance of the microcrystalline glass prepared in the examples and comparative examples are shown in the following table 1:
table 1 analysis results of properties of microcrystalline glasses prepared in examples and comparative examples
Claims (8)
1. The microcrystalline glass prepared from coal gasification furnace slag is characterized by comprising the following components in percentage by weight: 60-90% of coal gasification furnace slag and 10-40% of additive powder;
the additive powder is a mixture of red mud, ilmenite and limestone.
2. The microcrystalline glass according to claim 1, wherein the mass ratio of the red mud, the ilmenite and the limestone in the additive powder is 4-8: 1-3.
3. A method for producing a crystallized glass according to claim 1 or 2, characterized by comprising the steps of:
(1) grinding and sieving the slag of the gas furnace, and then carrying out preheating treatment at the temperature of 900-;
(2) mixing the preheated fine slag material of the gas furnace with the additive powder, granulating after mixing, then melting at the high temperature of 1500-;
(3) pouring the base glass liquid prepared in the step (2) into a preheated mold, demolding to obtain base glass, carrying out heat treatment on the base glass, and then annealing and cooling to room temperature to obtain the microcrystalline glass.
4. The manufacturing method according to claim 3, wherein the base glass heat treatment method in the step (3) is: the base glass is heated to the nucleation temperature of 960 ℃ at the speed of 11 ℃/min, the nucleation time is 3h, and then the temperature is heated to 980 ℃ for crystallization, and the crystallization time is 3 h.
5. The method according to claim 3, wherein the fine material of the gas furnace slag after the sieving in the step (1) has a particle size of 100 mesh.
6. The method according to claim 3, wherein the granulation in the step (2) is performed by an agglomeration granulation method, and the particle size is 1 cm.
7. The method according to claim 3, wherein the preheating temperature of the mold in the step (3) is 380 ℃.
8. The method of claim 3, wherein the annealing temperature reduction rate in the step (3) is 1.5 ℃/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114835396A (en) * | 2022-03-30 | 2022-08-02 | 国家能源集团宁夏煤业有限责任公司 | Composition for microcrystalline glass, microcrystalline glass and preparation method thereof |
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