CN111204981A - Direct oxygen blowing melting process of secondary kiln slag and method for preparing microcrystalline glass - Google Patents
Direct oxygen blowing melting process of secondary kiln slag and method for preparing microcrystalline glass Download PDFInfo
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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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- C01B17/00—Sulfur; Compounds thereof
- C01B17/48—Sulfur dioxide; Sulfurous acid
- C01B17/50—Preparation of sulfur dioxide
- C01B17/52—Preparation of sulfur dioxide by roasting sulfides
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- C01B17/74—Preparation
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- 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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- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
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- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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Abstract
The invention relates to a direct oxygen blowing melting process of secondary kiln slag and a method for preparing microcrystalline glass, which comprises the following steps: and (3) high-temperature oxygen blowing and melting of secondary kiln slag: and blowing oxygen-containing gas into the 800-1200 ℃ semi-molten secondary kiln slag, collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and utilizing the heat released by the oxidation reaction to increase the temperature of the secondary kiln slag to 1300-1600 ℃ to melt the secondary kiln slag to form slag. The semi-molten secondary kiln slag is directly oxidized by oxygen blowing, and is melted into slag by using a large amount of heat released by oxidation reaction, so that the slag becomes a raw material for preparing microcrystalline glass, rock wool, cast stone and the like, the comprehensive utilization range of the secondary kiln slag is expanded, the environmental pollution is avoided, the energy conservation and emission reduction are realized, and the production cost is greatly reduced.
Description
Technical Field
The invention belongs to the field of waste recycling, and particularly relates to a direct oxygen blowing melting process for secondary kiln slag and a method for preparing microcrystalline glass.
Background
The steel industry is the industry of the national industry pillar, and a large amount of solid waste can be discharged in the whole steel production process: steel slag, blast furnace slag, ferroalloy slag, dust and mud, and the like. Generally, 0.08 to 0.12 ton of dust is generated in a steel plant for 1 ton of steel, and the dust contains a large amount of valuable elements such as Fe, Zn, Pb, Ag, Cr, Cd and the like. Among them, zinc-containing dust has a high commercial value. The solid waste containing more zinc mainly comprises zinc-containing dust or dust mud collected in the purification process of blast furnace ironmaking gas, zinc-containing dust collected in electric furnace steelmaking smoke, zinc-containing waste slag generated in the wet zinc extraction process and the like. The recovery of the zinc-rich solid wastes by using a rotary kiln method is the most important utilization means at present.
The zinc-rich solid waste is added with 40-50% of coke, and after the metal elements such as zinc, lead and the like are reduced and volatilized at the high temperature of 1100-1300 ℃ in a rotary kiln, a large amount of zinc extraction kiln slag, namely secondary kiln slag, can be generated, wherein the secondary kiln slag is a secondary resource with high value, but the comprehensive recycling of valuable components of the secondary kiln slag is still a worldwide problem at present. In the process of generating secondary kiln slag, when a mixed material of zinc-containing solid waste and coke passes through a high-temperature zone of a rotary kiln, slag materials are in a semi-molten state, the materials are mutually bonded, and a plurality of valuable elements exist in a metal or alloy state or form various compounds, the embedding relation is compact, the mixed material is different from the traditional metallurgical slag, the matrix of the secondary kiln slag is mostly a complex phase in which metal iron and other compounds are tightly combined, and particularly, iron with a part of particles and fine marmatite are often wrapped in particles of a vitreous body and the coke; the gaps between spherical iron and the sphalerite are also filled with ferrous sulfide, and the ferrous sulfide is embedded with fine particles of lead iron, metallic silver and the like, so that pure or high-grade enriched products are difficult to obtain by adopting a general physical method.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a direct oxygen blowing melting process of secondary kiln slag and a method for preparing microcrystalline glass.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the first technical scheme is as follows:
a direct oxygen blowing melting process of secondary kiln slag comprises the following steps: and (3) high-temperature oxygen blowing and melting of secondary kiln slag: and blowing oxygen-containing gas into the 800-1200 ℃ semi-molten secondary kiln slag, collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and utilizing the heat released by the oxidation reaction to increase the temperature of the secondary kiln slag to 1300-1600 ℃ to melt the secondary kiln slag to form slag.
Further, before blowing oxygen into the secondary kiln slag, discharging the secondary kiln slag into a kiln, and performing oxygen blowing operation in the kiln;
furthermore, the kiln can adopt any one of a rotary kiln, a refining furnace, a slag ladle reaction furnace and a converter.
Further, the sulfur oxide gas includes one or both of sulfur dioxide gas and sulfur trioxide gas.
Further, the secondary kiln slag comprises CaO and SiO2、Al2O3、MgO、Fe2+、S2-(ii) a Wherein the CaO accounts for 5-20% by weight, and SiO accounts for210-25% of Al2O35-20% of (B), 1-8% of MgO, and Fe2+Converted into Fe2O3The percentage content of the S is 28-45 percent2-To SO3The percentage content is 10-30%.
Further, the preparation method of the secondary kiln slag comprises the following steps: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.3-0.6, and then smelting at the high temperature of 1100-1300 ℃ in a reactor to obtain semi-molten secondary kiln slag with the temperature of 800-1200 ℃.
The reactor adopts any one of a rotary kiln and a rotary furnace.
Furthermore, the zinc-rich solid waste adopts one or two of zinc-containing dust or dust mud recovered in the steel-making process and zinc-containing waste slag generated in the wet zinc extraction process.
Furthermore, the oxygen blowing rate of each kilogram of secondary kiln slag is 2.0-5.0L/min in terms of pure oxygen, and the oxygen blowing time is 0.7-3.5 min.
Further, before or during oxygen blowing into the secondary kiln slag, adding a modifier into the secondary kiln slag according to the mass ratio of 1: 0.01-0.2 of the secondary kiln slag to the modifier;
the modifier comprises one or more of silicate raw materials or solid wastes, carbon-containing raw materials or solid wastes, iron-containing raw materials or solid wastes, sulfur-containing raw materials or solid wastes, alkali metal-containing raw materials or solid wastes, and organic component-containing raw materials or solid wastes.
Further, the silicate raw material or the solid waste is quartz sand, and the carbon-containing raw material or the solid waste is carbon powder.
Further, discharging the molten slag into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
and (3) placing the mother glass in a heat preservation furnace at 900 ℃ for 1h, nucleating and crystallizing, cooling to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and annealing to obtain the microcrystalline glass.
Furthermore, before the slag is discharged into the mold, a mixture of reducing gas and/or coal powder and air is blown into the slag for blowing;
and then, standing the blown slag for 5-20 minutes until delamination occurs, directly discharging the silicate melt at the upper layer into a mold preheated to 900 ℃, and independently discharging the iron-rich melt at the lower layer to obtain the bread iron.
The reducing gas comprises one or more of natural gas, coal gas and liquefied gas.
Further, the residual sulfur content in the microcrystalline glass is not more than 4%.
Further, the blowing rate of a mixture of reducing gas and/or coal powder and air corresponding to each kilogram of molten slag is 2.0-5.0L/min, and the blowing time is 0.7-3.5 min;
the second technical scheme is as follows:
the method for preparing the microcrystalline glass specifically comprises the following steps:
step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, then smelting at the high temperature of 1100-1300 ℃ in a reactor, and discharging semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, blowing oxygen-containing gas into the semi-molten secondary kiln slag at 800-1200 ℃, simultaneously collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and melting the secondary kiln slag after the temperature of the secondary kiln slag is raised to 1300-1600 ℃ by utilizing the heat released by the oxidation reaction to form molten slag;
step 3, mother glass preparation: discharging the slag prepared in the step 2 into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
step 4, preparing microcrystalline glass: and (3) placing the mother glass obtained in the step (3) in a heat preservation furnace, preserving heat for 1h at 900 ℃, performing nucleation, then cooling the mother glass to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and performing annealing treatment to obtain the microcrystalline glass.
Further, in the step 3, before the slag prepared in the step 2 is discharged into a mould preheated to 900 ℃, a mixture of reducing gas and/or coal powder and air is blown into the slag prepared in the step 2 for converting;
and then, standing the blown slag for 5-20 minutes until delamination occurs, directly discharging the silicate melt at the upper layer into a mold preheated to 900 ℃, and independently discharging the iron-rich melt at the lower layer to obtain the bread iron.
Further, the blowing rate of a mixture of reducing gas and/or coal powder and air corresponding to each kilogram of molten slag is 2.0-5.0L/min, and the blowing time is 0.7-3.5 min;
compared with the prior art, the invention has the advantages that:
1. the method utilizes the characteristics that the secondary kiln slag contains iron and sulfur, most of the secondary kiln slag exists in FeS and other mineral phases, and few of the secondary kiln slag exists in other forms, directly blows oxygen to oxidize the semi-molten secondary kiln slag generated in the zinc extraction process, melts the secondary kiln slag into slag by utilizing a large amount of heat released by oxidation reaction, and becomes raw materials for preparing microcrystalline glass, rock wool, cast stone and the like.
2. In the process of oxygen blowing and oxidation of the secondary kiln slag, the invention makes S in the secondary kiln slag2-Oxidized into sulfur dioxide and sulfur trioxide gas, and prepared into sulfuric acid by a flue gas recovery process, thereby realizing the recycling of resources.
Drawings
FIG. 1 is a process flow diagram of one embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
Step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, and then smelting at the high temperature of 1100-1300 ℃ in a rotary kiln to obtain semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, blowing oxygen-containing gas into the semi-molten secondary kiln slag at 800-1200 ℃, simultaneously collecting sulfur oxide gas, enabling the oxygen in the oxygen-containing gas and the secondary kiln slag to perform oxidation reaction in the process of blowing the oxygen-containing gas, releasing heat, and utilizing the heat released by the oxidation reaction to increase the temperature of the secondary kiln slag to 1500 ℃ to melt the secondary kiln slag to form slag; the oxygen blowing rate is as follows: the oxygen blowing rate corresponding to each kilogram of secondary kiln slag is 3.5L/min in terms of pure oxygen, and the oxygen blowing time is 1 min;
step 3, mother glass preparation: directly discharging the slag prepared in the step 2 into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
step 4, preparing microcrystalline glass: and (3) placing the mould containing the mother glass in the step (3) in a heat preservation furnace, preserving heat for 1h at 900 ℃, nucleating and crystallizing, and then cooling the mother glass to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and annealing to obtain the microcrystalline glass.
The microcrystalline glass produced in this example had a flexural strength of 59.0MPa, a water absorption of 0.3%, and a residual S content of 0.89%.
Example 2
Step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, and then smelting at the high temperature of 1100-1300 ℃ in a rotary kiln to obtain semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, blowing oxygen-containing gas into the 900 ℃ semi-molten secondary kiln slag, collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and raising the temperature of the secondary kiln slag to 1400 ℃ by using the heat released by the oxidation reaction to melt the secondary kiln slag to form slag; the oxygen blowing rate is as follows: the oxygen blowing rate corresponding to each kilogram of secondary kiln slag is 2.5L/min calculated by pure oxygen, and the oxygen blowing time is 1 min;
step 3, mother glass preparation: directly discharging the slag prepared in the step 2 into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
step 4, preparing microcrystalline glass: and (3) placing the mould containing the mother glass in the step (3) in a heat preservation furnace, preserving heat for 1h at 900 ℃, nucleating and crystallizing, and then cooling the mother glass to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and annealing to obtain the microcrystalline glass.
The microcrystalline glass produced in this example had a flexural strength of 40.24MPa and a water absorption of 0.4%.
Example 3
Step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, and then smelting at the high temperature of 1100-1300 ℃ in a rotary kiln to obtain semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, and then mixing the secondary kiln slag, quartz sand and carbon powder in a weight ratio of 1: 0.1: 0.05 (namely, 10 wt.% of quartz sand and 5 wt.% of carbon powder), modifier quartz sand and carbon powder (the quartz sand contains SiO2>90 wt.%, and the carbon powder contains C >90 wt.%) are added into the secondary kiln slag, then oxygen-containing gas is blown into the secondary kiln slag, sulfur oxide gas is collected, oxygen in the oxygen-containing gas and the secondary kiln slag are subjected to oxidation reaction during the blowing of the oxygen-containing gas, heat is released, and the temperature of the secondary kiln slag is increased to 1500 ℃ by utilizing the heat released by the oxidation reaction, and the secondary kiln slag is melted to form slag; the oxygen blowing rate is as follows: the oxygen blowing rate corresponding to each kilogram of secondary kiln slag is 3.5L/min in terms of pure oxygen, and the oxygen blowing time is 2.5 min;
step 3, mother glass preparation: directly discharging the slag prepared in the step 2 into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
step 4, preparing microcrystalline glass: and (3) placing the mould containing the mother glass in the step (3) in a heat preservation furnace, preserving heat for 1h at 900 ℃, performing nucleation, then cooling the mother glass to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and performing annealing treatment to obtain the microcrystalline glass.
The microcrystalline glass produced in this example had a flexural strength of 124MPa, a water absorption of 0.20%, and a residual S content of 0.98%.
Example 4
Step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, and then smelting at the high temperature of 1100-1300 ℃ in a rotary kiln to obtain semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, adding modifier carbon powder (carbon powder contains C90 wt.%) into the carbon powder according to the weight ratio of the secondary kiln slag to the carbon powder of 1:0.05(5 wt.%), blowing oxygen-containing gas into the carbon powder, collecting sulfur oxide gas, enabling oxygen in the oxygen-containing gas to have an oxidation reaction with the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and utilizing the heat released by the oxidation reaction to increase the temperature of the secondary kiln slag to 1500 ℃ and melt the secondary kiln slag to form slag; the oxygen blowing rate is as follows: the oxygen blowing rate corresponding to each kilogram of secondary kiln slag is 3.5L/min in terms of pure oxygen, and the oxygen blowing time is 1.5 min;
step 3, converting: blowing a mixture of natural gas (reducing gas) and oxygen into the molten slag prepared in the step 2, and carrying out reduction blowing on the molten slag to obtain part of simple substance iron; blowing in reducing gas and/or coal powder and air mixture corresponding to each kilogram of slag at a blowing rate of 3.2L/min for 2.0 min;
step 3, preparing mother glass and bread iron: standing the slag blown in the step 3 for 10 minutes until the slag is layered, and directly discharging the upper-layer silicate melt into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass; discharging the lower layer iron-rich melt independently to obtain the bread iron;
step 4, preparing microcrystalline glass: and (3) putting the mould containing the mother glass into a muffle furnace at 900 ℃ for heat preservation for 1h to form nucleation, and then cooling to 650 ℃ at a cooling speed of 5 ℃/min for heat preservation for 1h for annealing treatment.
The microcrystalline glass obtained in this example had a flexural strength of 87.23MPa, a water absorption of 0.45% and a residual S content of 3.524%.
The embodiments described above are only preferred embodiments of the invention and are not exhaustive of the possible implementations of the invention. Any obvious modifications to the above would be obvious to those of ordinary skill in the art, but would not bring the invention so modified beyond the spirit and scope of the present invention.
Claims (10)
1. A direct oxygen blowing melting process of secondary kiln slag is characterized by comprising the following steps: and (3) high-temperature oxygen blowing and melting of secondary kiln slag: and blowing oxygen-containing gas into the 800-1200 ℃ semi-molten secondary kiln slag, collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and utilizing the heat released by the oxidation reaction to increase the temperature of the secondary kiln slag to 1300-1600 ℃ to melt the secondary kiln slag to form slag.
2. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 1, wherein the secondary kiln slag is discharged into a kiln before oxygen blowing is performed to the secondary kiln slag, and oxygen blowing operation is performed in the kiln.
3. The direct oxygen-blown melting of secondary kiln slag as claimed in claim 1The process is characterized in that the secondary kiln slag comprises CaO and SiO2、Al2O3、MgO、Fe2+、S2-(ii) a Wherein the CaO accounts for 5-20% by weight, and SiO accounts for210-25% of Al2O35-20% of (B), 1-8% of MgO, and Fe2+With Fe2O3The percentage content of the S is 28-45 percent2-With SO3The percentage content is 10-30%.
4. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 1, wherein the preparation method of the secondary kiln slag comprises the following steps: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.3-0.6, and then smelting at the high temperature of 1100-1300 ℃ in a reactor to obtain semi-molten secondary kiln slag with the temperature of 800-1200 ℃.
5. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 4, wherein the zinc-rich solid waste adopts one or two of zinc-containing dust or dust mud recovered in the steel making process and zinc-containing waste slag generated in the wet zinc extraction process.
6. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 1,
the oxygen blowing rate corresponding to each kilogram of secondary kiln slag is 2.0-5.0L/min calculated by pure oxygen, and the oxygen blowing time is 0.7-3.5 min.
7. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 1, wherein before or during oxygen blowing into the secondary kiln slag, a modifier is added into the secondary kiln slag according to the mass ratio of 1: 0.01-0.2 of the secondary kiln slag to the modifier;
the modifier comprises one or more of silicate raw materials or solid wastes, carbon-containing raw materials or solid wastes, iron-containing raw materials or solid wastes, sulfur-containing raw materials or solid wastes, alkali metal-containing raw materials or solid wastes, and organic component-containing raw materials or solid wastes.
8. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 1, wherein the slag is discharged into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
and (3) placing the mother glass in a heat preservation furnace at 900 ℃ for 1h, nucleating and crystallizing, cooling to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and annealing to obtain the microcrystalline glass.
9. The direct oxygen blowing melting process of the secondary kiln slag as claimed in claim 8, wherein before the slag is discharged into the mold, a mixture of reducing gas and/or pulverized coal and air is blown into the slag for blowing;
and then, standing the blown slag for 5-20 minutes until delamination occurs, directly discharging the silicate melt at the upper layer into a mold preheated to 900 ℃, and independently discharging the iron-rich melt at the lower layer to obtain the bread iron.
10. The method for preparing the microcrystalline glass is characterized by comprising the following steps:
step 1, discharging secondary kiln slag: adding the zinc-rich solid waste into coke according to the mass ratio of the zinc-rich solid waste to the coke of 1: 0.4-0.5, then smelting at the high temperature of 1100-1300 ℃ in a reactor, and discharging semi-molten secondary kiln slag at the temperature of 800-1200 ℃;
step 2, high-temperature oxygen blowing and melting of secondary kiln slag: directly discharging the secondary kiln slag prepared in the step 1 into a kiln, blowing oxygen-containing gas into the semi-molten secondary kiln slag at 800-1200 ℃, simultaneously collecting sulfur oxide gas, carrying out oxidation reaction on the oxygen in the oxygen-containing gas and the secondary kiln slag in the process of blowing the oxygen-containing gas, releasing heat, and melting the secondary kiln slag after the temperature of the secondary kiln slag is raised to 1300-1600 ℃ by utilizing the heat released by the oxidation reaction to form molten slag;
step 3, mother glass preparation: discharging the slag prepared in the step 2 into a mold preheated to 900 ℃ for cooling for 1min to obtain mother glass;
step 4, preparing microcrystalline glass: and (3) placing the mother glass obtained in the step (3) in a heat preservation furnace, preserving heat for 1h at 900 ℃, performing nucleation, then cooling the mother glass to 650 ℃ at a cooling speed of 5 ℃/min, preserving heat for 1h, and performing annealing treatment to obtain the microcrystalline glass.
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| CN111204981B (en) | 2022-04-01 |
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