Method for preparing glass beads by utilizing metallurgical recycled raw materials
By using multi-stage air and liquid cooling during the cooling process of glass microbeads, the temperature gradient and internal stress problems caused by the fast cooling rate in the prior art are solved, and the physical properties and structural stability of glass microbeads are significantly improved.
Patent Information
- Application Number
- CN202411414767.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-11
- Publication Date
- 2025-02-18
AI Technical Summary
In the preparation of existing glass microbeads, the cooling stage adopts a one-stage direct cooling, resulting in too fast cooling rate, significant temperature gradient, internal stress concentration and microcrack formation, resulting in a decline in physical properties and poor structural stability.
Using multi-stage air and liquid cooling, the cooling paths of spherical microbeads are divided into three sections: primary cooling, intermediate cooling and slow cooling stages, using natural convection air cooling, water spray cooling and rock wool heat absorption cooling respectively to gradually reduce the temperature , reduce temperature gradient and internal stress.
Through step-by-step cooling, the physical properties and structural stability of glass microbeads are significantly improved, the formation of microcracks is avoided, and the product quality is improved.
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Figure CN119461794A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of glass microbead preparation, and in particular to a method for preparing glass microbeads by utilizing metallurgical recycled raw materials. Background Art
[0002] Glass microspheres are small spheres made of glass materials, with diameters usually ranging from a few microns to a few millimeters. They have good optical and heat-resistant properties. They can be prepared by melting or spraying methods and are widely used in coatings, plastics, medicines, cosmetics and other fields. They are mainly used to enhance material properties and provide reflective effects. In recent years, research on glass microspheres has continued to deepen, focusing on optimizing the preparation process, improving physical properties and expanding application areas.
[0003] In the existing preparation of glass microspheres, a one-step direct cooling method is often used in the cooling stage. The cooling rate of this method is too fast, which can easily lead to a significant temperature gradient, thereby causing the concentration of internal stress and the formation of microcracks, thus resulting in the problem of reduced physical properties of the microspheres and poor structural stability. Summary of the invention
[0004] In view of the shortcomings of the prior art, the present invention provides a method for preparing glass microspheres using metallurgical recycled raw materials, which solves the problem that in the existing preparation of glass microspheres, a one-stage direct cooling method is often used in the cooling stage. The cooling rate of this method is too fast, which easily leads to a significant temperature gradient, thereby causing the concentration of internal stress and the formation of microcracks, thereby causing the physical properties of the microspheres to decrease and the structural stability to deteriorate.
[0005] To achieve the above purpose, the present invention is implemented by the following technical scheme: A method for preparing glass microspheres using metallurgical recycled raw materials, comprising the following steps:
[0006] S1. Raw material preparation: weigh the components according to the formula of 50-80 parts by weight of silica sand, 10-20 parts of soda lime, 1-10 parts of alumina, 5-15 parts of calcium carbonate, and 1-5 parts of a solvent, crush and sieve the raw materials, and the silica sand is separated from metallurgical waste;
[0007] S2. Melting: preheat the high-temperature furnace to 1400 degrees Celsius in advance, put the raw materials into the high-temperature furnace for heating, the heating temperature is 1400-1600 degrees Celsius, and continue heating for 1-4 hours to form a high-temperature liquid;
[0008] S3, molding: changing the high temperature liquid into spherical micro beads by spray molding or spherical molding;
[0009] S4, cooling: introducing multiple sections of air and liquid into the path through which the spherical microbeads pass to cool the spherical microbeads to form glass microbeads;
[0010] S5, post-processing: washing the glass beads with water, polishing the surface with a polishing machine after washing, and drying with hot air in a drying oven after polishing;
[0011] S6. Screening: Use a multi-stage screener to screen the glass beads into different particle sizes;
[0012] S7. Packaging and storage: Glass beads of different particle sizes are packaged separately.
[0013] Preferably, the silica sand in step S1 is obtained from metallurgical waste, and the metallurgical waste is mechanically separated to obtain silica sand with a particle size of 10-20 microns. After separation, the silica sand is pickled for 0.5-2 hours using 1-5M hydrochloric acid at a ratio of 1:5-10. After pickling, the silica sand is dried in an oven at 100-120 degrees Celsius for 1-4 hours. During the drying period, the moisture content is checked every 30 minutes to ensure that the moisture content is 0.5-1%.
[0014] Preferably, the co-solvent comprises the following raw materials in percentage: 10-30% boric acid, 5-15% sodium carbonate, 5-20% calcium stone, 2-10% bauxite, 1-5% magnesium oxide and 1-5% zinc oxide.
[0015] Preferably, the mechanical separation from the metallurgical waste should be carried out using one or more of the following equipment: vibrating screen, rotary screen, flotation machine, gravity separator, air separator, magnetic separator, scraper conveyor, dryer.
[0016] Preferably, the multi-stage air and liquid in step S4 can divide the path of the spherical micro-beads into three sections, the first section is an initial cooling stage, the second section is a medium cooling stage, and the third section is a slow cooling stage.
[0017] Preferably, the initial cooling stage uses natural convection air cooling to reduce the temperature of the spherical microbeads to 620-580 degrees Celsius, the intermediate cooling stage sprays water mist through a water nozzle to reduce the temperature of the spherical microbeads to 320-280 degrees Celsius, and the slow cooling stage is to lay rock wool on the path to reduce the temperature inside the spherical microbeads to room temperature through the rock wool.
[0018] Preferably, the pulverization in step S1 requires the use of one or more of the following equipment: a ball mill, an impact mill, a jet mill, and a roller mill, and the above equipment is used to process each raw material to 5-10 microns.
[0019] Preferably, in step S5, the surface is polished by a polishing machine, and the pressure of the polishing machine is maintained at 1-3 kg / cm 2, continue polishing for 15-60 minutes. After polishing, the surface roughness of the glass beads is 0.05-0.1 microns. The drying oven is maintained at 70 degrees Celsius for 4-12 hours of hot air drying.
[0020] The present invention provides a method for preparing glass microspheres by using metallurgical recycled raw materials. It has the following beneficial effects:
[0021] 1. In the present invention, the path of the spherical microspheres during the cooling stage is divided into three sections, each section corresponds to a different cooling measure, the first section adopts natural convection air cooling, the second section adopts water mist sprayed from a water nozzle for cooling, and the third section adopts rock wool heat absorption cooling, thereby realizing step-by-step cooling of the glass microspheres, thereby improving the existing preparation of glass microspheres, in which one-stage direct cooling is often adopted in the cooling stage. This method has a too fast cooling rate and is likely to lead to a significant temperature gradient, thereby causing the concentration of internal stress and the formation of microcracks, thereby causing the physical properties of the glass microspheres to deteriorate and the structural stability to deteriorate.
[0022] 2. In the present invention, silica sand is extracted from metallurgical waste by mechanical separation, and then pickled and dried to ensure the purity of the silica sand. The processed silica sand is added to the raw material of glass beads, thereby realizing waste utilization and achieving the effect of saving materials. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] Figure 1 It is a flow chart of the manufacturing process of the present invention. DETAILED DESCRIPTION
[0024] The technical solution of the present invention will be described clearly and completely below in conjunction with the accompanying drawings of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.
[0025] Please see attached Figure 1 The embodiment of the present invention provides a method for preparing glass microspheres by using metallurgical recycled raw materials, which is characterized by comprising the following steps:
[0026] S1. Raw material preparation: weigh the components according to the formula of 50-80 parts by weight of silica sand, 10-20 parts of soda lime, 1-10 parts of aluminum oxide, 5-15 parts of calcium carbonate, and 1-5 parts of a solvent, crush and screen the raw materials, separate silica sand from metallurgical waste, silica sand is the main component in glass microspheres, and improves the strength, heat resistance and optical properties of glass microspheres, soda lime can reduce the melting temperature of raw materials, thereby reducing energy consumption and improving production efficiency, aluminum oxide can improve the mechanical strength and toughness of glass microspheres, making them more durable, and calcium carbonate helps to improve the fluidity of raw materials, making the molding process smoother;
[0027] S2. Melting: preheat the high-temperature furnace to 1400 degrees Celsius in advance, put the raw materials into the high-temperature furnace for heating, the heating temperature is 1400-1600 degrees Celsius, and continue heating for 1-4 hours to form a high-temperature liquid;
[0028] S3, molding: changing the high temperature liquid into spherical micro beads by spray molding or spherical molding;
[0029] S4, cooling: introducing multiple sections of air and liquid into the path through which the spherical microbeads pass to cool the spherical microbeads to form glass microbeads;
[0030] S5, post-processing: washing the glass beads with water, polishing the surface with a polishing machine after washing, and drying with hot air in a drying oven after polishing;
[0031] S6. Screening: Use a multi-stage screener to screen the glass beads into different particle sizes;
[0032] S7. Packaging and storage: Glass beads of different particle sizes are packaged separately.
[0033] The silica sand in step S1 is obtained from metallurgical waste, and the metallurgical waste is mechanically separated to obtain silica sand with a particle size of 10-20 microns, thereby removing obvious impurities and non-silicon materials, and obtaining silica sand particles of suitable particle size. After separation, the silica sand is pickled for 0.5-2 hours using hydrochloric acid at a concentration of 1-5M in a ratio of 1:5-10, thereby removing impurities such as iron ions. After pickling, the silica sand is dried in an oven at 100-120 degrees Celsius for 1-4 hours. The moisture content is checked every 30 minutes during the drying period to ensure that the moisture content is 0.5-1%, thereby making the extracted silica sand higher in purity and having a better subsequent processing effect.
[0034] The co-solvent includes the following raw materials in percentage: 10-30% boric acid, 5-15% sodium carbonate, 5-20% calcium stone, 2-10% bauxite, 1-5% magnesium oxide and 1-5% zinc oxide. Boric acid can reduce the melting temperature of the raw materials and improve fluidity. Sodium carbonate can increase the melting rate of the raw materials and reduce the melting point. Calcium stone can improve the chemical resistance and strength of the glass. Bauxite can improve the stability and heat resistance of the glass microspheres. Magnesium oxide can improve the heat resistance and aging resistance of the glass microspheres. Zinc oxide can improve the optical properties and surface gloss of the glass microspheres.
[0035] Mechanical separation from metallurgical waste should use one or more of the following equipment in combination: vibrating screen, rotary screen, flotation machine, gravity separator, air separator, magnetic separator, scraper conveyor, dryer.
[0036] The multi-stage air and liquid in step S4 can divide the path of the spherical microbeads into three sections, the first section is the initial cooling stage, the second section is the intermediate cooling stage, and the third section is the slow cooling stage, thereby effectively reducing the temperature gradient, reducing the internal stress, and improving the structural stability and product quality of the spherical microbeads.
[0037] In the initial cooling stage, natural convection air cooling is used to reduce the temperature of the spherical microbeads to 620-580 degrees Celsius, so that the glass microbeads can still remain flexible and facilitate the stability of their shape. In the intermediate cooling stage, water mist is sprayed through the water nozzle to reduce the temperature of the glass microbeads to 320-280 degrees Celsius, thereby reducing the thermal stress inside the glass microbeads and ensuring the uniformity of the glass microbead structure. In the slow cooling stage, rock wool is laid on the path to reduce the temperature inside the glass microbeads to room temperature through the rock wool, thereby ensuring that the internal stress of the glass microbeads is fully released, avoiding the generation of cracks, and thus improving the mechanical strength of the glass microbeads.
[0038] The crushing in step S1 requires the use of one or more of the following equipment: ball mill, impact mill, air flow mill and roller mill. The above equipment is used to process each raw material to 5-10 microns, thereby ensuring that uniform glass beads can be obtained in the subsequent melting and molding process.
[0039] In step S5, the surface is polished by a polishing machine, and the pressure of the polishing machine is maintained at 1-3 kg / cm 2 , continue polishing for 15-60 minutes. After polishing, the surface roughness of the glass beads is 0.05-0.1 microns. The polishing machine can further improve the surface quality and glossiness of the beads. The drying oven is maintained at 70 degrees Celsius for 4-12 hours of hot air drying. The drying oven is used to remove moisture and volatiles to ensure the quality and stability of the final product.
[0040] The following is further introduced in conjunction with specific embodiments:
[0041] Embodiment 1:
[0042] A method for preparing glass microspheres using metallurgical recycled raw materials comprises the following steps:
[0043] S1. Raw material preparation: weigh the components according to the formula of 80 parts by weight of silica sand, 20 parts by weight of soda lime, 10 parts by weight of alumina, 15 parts by weight of calcium carbonate, and 5 parts by weight of a solvent, and crush and sieve the raw materials. The silica sand is separated from metallurgical waste;
[0044] S2. Melting: preheat the high-temperature furnace to 1400 degrees Celsius in advance, put the raw materials into the high-temperature furnace for heating at 1500 degrees Celsius, and continue heating for 3 hours to form a high-temperature liquid;
[0045] S3, molding: changing the high temperature liquid into spherical micro beads by spray molding or spherical molding;
[0046] S4, cooling: introducing multiple sections of air and liquid into the path through which the spherical microbeads pass to cool the spherical microbeads to form glass microbeads;
[0047] S5, post-processing: washing the glass beads with water, polishing the surface with a polishing machine after washing, and drying with hot air in a drying oven after polishing;
[0048] S6. Screening: Use a multi-stage screener to screen the glass beads into different particle sizes;
[0049] S7. Packaging and storage: Glass beads of different particle sizes are packaged separately.
[0050] The multi-stage air and liquid in step S4 can divide the path of the spherical micro-beads into three sections, the first section is the initial cooling stage, the second section is the intermediate cooling stage, and the third section is the slow cooling stage.
[0051] In the initial cooling stage, natural convection air cooling is used to reduce the temperature of the spherical microbeads to 620 degrees Celsius. In the intermediate cooling stage, water mist is sprayed through the water nozzle to reduce the temperature of the spherical microbeads to 320 degrees Celsius. In the slow cooling stage, rock wool is laid on the path to reduce the temperature inside the spherical microbeads to room temperature.
[0052] Embodiment 2:
[0053] The difference between this embodiment and the above-mentioned embodiment 1 is that:
[0054] In the initial cooling stage, natural convection air cooling is used to reduce the temperature of the spherical microbeads to 600 degrees Celsius. In the intermediate cooling stage, water mist is sprayed through the water nozzle to reduce the temperature of the spherical microbeads to 300 degrees Celsius. In the slow cooling stage, rock wool is laid on the path to reduce the temperature inside the spherical microbeads to room temperature.
[0055] Embodiment 3:
[0056] The difference between this embodiment and the above-mentioned embodiment 1 and embodiment 2 is that:
[0057] In the initial cooling stage, natural convection air cooling is used to reduce the temperature of the spherical microbeads to 580 degrees Celsius. In the intermediate cooling stage, water mist is sprayed through the water nozzle to reduce the temperature of the spherical microbeads to 280 degrees Celsius. In the slow cooling stage, rock wool is laid on the path to reduce the temperature inside the spherical microbeads to room temperature.
[0058] Table 1:
[0059] contrast Example 1 Example 2 Example 3 Standard value Compressive strength(MPa) 450 425 380 300 Impact resistance (J) 3.6 3.2 2.7 1 Scattered light intensity (%) 6.5 7.4 8.2 9 Light transmittance (%) 94 90 88 85 Melting point (Celsius) 770 740 695 650
[0060] The comparison in Table 1 is for compressive strength, impact resistance, scattered light intensity, light transmittance and melting point. The standard values in Table 1 are obtained based on experiments on glass beads prepared without adopting staged cooling in the cooling stage. By changing the temperature of the segmented cooling in each embodiment, the results of Examples 1-3 in Table 1 are obtained. Table 1 shows that the performance of the glass beads can be effectively improved by segmented cooling.
[0061] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.
Claims
1. A method for preparing glass microspheres using metallurgical recycled raw materials, characterized in that: The following steps are involved: S1. Raw material preparation: weigh the components according to the formula of 50-80 parts by weight of silica sand, 10-20 parts of soda lime, 1-10 parts of alumina, 5-15 parts of calcium carbonate, and 1-5 parts of a solvent, crush and sieve the raw materials, and the silica sand is separated from metallurgical waste; S2, melting: preheat the high-temperature furnace to 1400 degrees Celsius in advance, put the raw materials into the high-temperature furnace for heating, the heating temperature is 1400-1600 degrees Celsius, and the heating is continued for 1-4 hours to form high-temperature glass liquid; S3, molding: changing the high temperature glass liquid into spherical micro beads by spray molding or spherical molding; S4, cooling: introducing multiple sections of air and liquid into the path through which the spherical microbeads pass to cool the spherical microbeads to form glass microbeads; S5, post-processing: washing the glass beads with water, polishing the surface with a polishing machine after washing, and drying with hot air in a drying oven after polishing; S6. Screening: Use a multi-stage screener to screen the glass beads into different particle sizes; S7. Packaging and storage: Glass beads of different particle sizes are packaged separately.
2. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: The silica sand in step S1 is obtained from metallurgical waste. The metallurgical waste is mechanically separated to obtain silica sand with a particle size of 10-20 microns. After separation, the silica sand is pickled for 0.5-2 hours using hydrochloric acid with a concentration of 1-5M at a ratio of 1:5-10. After pickling, the silica sand is dried in an oven at 100-120 degrees Celsius for 1-4 hours. During the drying period, the moisture content is checked every 30 minutes to ensure that the moisture content is 0.5-1%.
3. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: The co-solvent comprises the following raw materials in percentage: 10-30% boric acid, 5-15% sodium carbonate, 5-20% calcium stone, 2-10% bauxite, 1-5% magnesium oxide and 1-5% zinc oxide.
4. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: The mechanical separation from metallurgical waste should be carried out using one or more of the following equipment: vibrating screen, rotary screen, flotation machine, gravity separator, air separator, magnetic separator, scraper conveyor, dryer.
5. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: The multi-stage air and liquid in step S4 can divide the path of the spherical micro-beads into three sections, the first section is the initial cooling stage, the second section is the intermediate cooling stage, and the third section is the slow cooling stage.
6. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 5, characterized in that: The initial cooling stage uses natural convection cooling to reduce the temperature of the spherical microbeads to 620-580 degrees Celsius. The intermediate cooling stage sprays water mist through a water nozzle to reduce the temperature of the spherical microbeads to 320-280 degrees Celsius. The slow cooling stage is to lay rock wool on the path to reduce the temperature inside the spherical microbeads to room temperature through the rock wool.
7. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: The pulverization in step S1 requires the use of one or more of the following equipment: a ball mill, an impact mill, a jet mill, and a roller mill. The above equipment is used to process each raw material into 5-10 microns.
8. The method for preparing glass microspheres by using metallurgical recycled raw materials according to claim 1, characterized in that: In step S5, the surface is polished by a polishing machine, and the pressure of the polishing machine is maintained at 1-3 kg / cm 2 , continue polishing for 15-60 minutes. After polishing, the surface roughness of the glass beads is 0.05-0.1 microns. The drying oven is maintained at 70 degrees Celsius for 4-12 hours of hot air drying.
Citation Information
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