A method for improving the yield of hollow glass microsphere finished product by positive pressure melting and homogenizing

By applying a positive pressure of 101000–130000 Pa in the melting furnace and stirring and homogenizing, the problem of low yield of hollow glass microspheres was solved, achieving higher yield and uniformity, and improving the quality of hollow glass microspheres.

CN118833997BActive Publication Date: 2026-01-06CNBM RESEARCH INSTITUTE FOR ADVANCED GLASS MATERIALS GROUP CO LTD +1
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Patent Information

Application Number
CN202411010351.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-07-26
Publication Date
2026-01-06
Estimated Expiration
2044-07-26

AI Technical Summary

Technical Problem

The yield of hollow glass microspheres in existing technologies is not high. Traditional melting methods fail to effectively control the retention and uniformity of air bubbles, resulting in insufficient product quality.

Method used

Positive pressure melting technology is adopted, applying a pressure of 101000~130000Pa in the melting furnace to control bubbles to remain in the glass melt, and improving the uniformity of the melting process by stirring and homogenizing, and improving the yield by combining cyclone and bag collection technology.

Benefits of technology

By using pressure melting and homogenization treatment, the yield and quality of hollow glass microspheres were significantly improved, the bubble retention effect was enhanced, and higher yield and uniformity were achieved.

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Abstract

The application discloses a kind of positive pressure melting, homogenization method for improving the yield of hollow glass microsphere, belong to the technical field of hollow glass microsphere preparation, including glass batch ingredient, temperature melting, homogenization, water quenching, crushing classification, powder conveying, hollow spheroidization, collection sorting, also include pressurization processing, before temperature melting, first melt furnace is pressurized, control furnace pressure is at 101000Pa-130000Pa, 0.5-1 hour is used;Then temperature melting, temperature 1450~1550 DEG C, melting time 6~7 hours, and carry out stirring homogenization, after homogenization, melt furnace is discharged gas, adjust the air pressure balance in furnace.The application has the advantages that: batch ingredient is pressurized melting, stirring homogenization, realize the uniformity and completeness of reaction between batch ingredient, reach the best melting, homogenization effect, obtain bubble glass liquid absorption better powder method preparation hollow glass microsphere with high-quality glass raw material.
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Description

Technical Field

[0001] This invention belongs to the field of hollow glass microsphere preparation technology, specifically, it relates to a positive pressure melting and homogenization method for improving the yield of hollow glass microspheres. Background Technology

[0002] Hollow glass microspheres are tiny hollow glass spheres that possess advantages such as light weight, heat insulation, sound insulation, resistance to high and low temperatures, good electrical insulation and thermal stability, and corrosion resistance. Their density is generally between 0.10 and 0.70 g / cm³. 3 The particle size range is generally 5-200μm. Hollow glass microspheres can be used as a novel filler material in resins, and are widely used in deep-sea buoyancy materials, thermal insulation materials, etc. They can also be used to produce low-density cement slurry, drilling fluid, etc., to solve the problems of deep cementing and drilling. They can also be used as special functional materials, such as aerospace ablation materials, hydrogen storage materials, and electromagnetic shielding materials, and have broad application prospects.

[0003] The glass melting process is a complex physicochemical reaction, including the silicate formation stage, the glass formation stage, and the refining and homogenization stage. The refining stage is the process of bubble elimination. During this process, as the temperature rises, the viscosity of the molten glass decreases, and an equilibrium is established between the gas in the bubbles, the furnace gases, and the physically dissolved and chemically combined gases in the molten glass. During the subsequent cooling of the molten glass, as the gases cool, the bubbles shrink under constant gas pressure. This is due to the surface tension of the glass; the pressure inside the bubble increases due to the decrease in radius. Simultaneously, the saturation pressure of the gas in the molten glass is lower than the pressure of the gas inside the bubble, causing the gas inside the bubble to dissipate into the molten glass. Because the bubble radius decreases again after the gas is released, the surface tension of the molten glass further increases the pressure inside the bubble until the bubble is completely absorbed by the molten glass, forming glass. When the molten glass is reheated, the gases dissolved in the glass reappear in the form of bubbles due to external factors.

[0004] The glass powder method for preparing hollow glass microspheres utilizes the aforementioned basic principles. It selects glass raw materials with a specific composition, melts and pulverizes them into particles of a certain size, and then reheats these particles in a hollow spheroidizing furnace. During this process, the molten glass particles spheroidize under surface tension. Simultaneously, changes in temperature, pressure, and atmosphere during spheroidization release gases previously dissolved in the glass. These gases are then rapidly cooled and collected, yielding the hollow glass microsphere product. Traditional glass melting involves melting and refining steps. During refining, bubbles in the molten glass must be fully released to ensure the glass is defect-free, which further explains the low yield of hollow glass microspheres. In contrast, the powder method for preparing hollow glass microspheres uses high-quality glass raw materials. During melting, the foaming agent must be uniformly dissolved in the molten glass. When the melted glass is reheated, the gases dissolved in the glass reappear as bubbles due to external factors, thus improving the yield of hollow glass microspheres. Summary of the Invention

[0005] The purpose of this invention is to overcome the problem of low yield of hollow glass microspheres in the prior art, and to provide a positive pressure melting and homogenization method to improve the yield of hollow glass microspheres.

[0006] The objective of this invention can be achieved through the following technical solutions:

[0007] A positive pressure melting and homogenization method for improving the yield of hollow glass microspheres includes batching of glass batch material for hollow glass microspheres, pressurization treatment, heating and melting, homogenization, water quenching, crushing and grading, powder conveying, hollow spheroidization, collection and sorting.

[0008] Before heating and melting, the melting furnace is pressurized to control the pressure inside the furnace at 101,000 to 130,000 Pa for 0.5 to 1 hour. Then, the furnace is heated to 1450 to 1550°C for 6 to 7 hours, and the furnace is stirred and homogenized. After homogenization, the gas is discharged from the furnace to adjust the pressure balance inside and outside the furnace.

[0009] To produce hollow glass microspheres, glass must first be melted. During the melting process, air bubbles must be retained inside the glass. However, conventional glass melting methods require removing these air bubbles. This invention, however, uses positive pressure melting (melting under pressure of 101,000–130,000 Pa) to retain air bubbles inside the glass during the melting process. Retaining more air bubbles not only increases the yield of hollow glass microspheres but also improves homogenization through pressure treatment, thereby enhancing the quality of the finished hollow glass microspheres.

[0010] Furthermore, the collection and sorting process is as follows: the powder material after hollow spheroidization in the bead forming furnace is collected, including two parts: cyclone collection and bag collection.

[0011] Furthermore, the furnace pressure is 101000~105000 Pa.

[0012] Furthermore, the pressure inside the furnace is 105000-110000 Pa.

[0013] Furthermore, the pressure inside the furnace is 110,000-120,000 Pa.

[0014] Furthermore, the pressure inside the furnace is 120,000-130,000 Pa.

[0015] Furthermore, the glass batching material for the hollow glass microspheres comprises the following raw materials in the following mass proportions: 56.48 kg of quartz sand, 1.74 kg of feldspar, 8.15 kg of calcium carbonate, 8.14 kg of alumina, 20.15 kg of soda ash, 1.98 kg of lithium carbonate, 1.41 kg of sodium sulfate, and 0.30 kg of iron oxide.

[0016] The beneficial effects of this invention are:

[0017] The batch material is pressurized, melted, and stirred to homogenize, thereby achieving uniformity and completeness of the reaction between the batch materials, achieving the best melting and homogenization effect, and obtaining high-quality glass raw materials for the powder method to prepare hollow glass microspheres with better absorption of air bubbles by the glass melt. Detailed Implementation

[0018] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative effort are within the scope of protection of the present invention.

[0019] Example 1

[0020] Weigh the following raw materials by weight: 56.48 kg of quartz sand, 1.74 kg of feldspar, 8.15 kg of calcium carbonate, 8.14 kg of alumina, 20.15 kg of soda ash, 1.98 kg of lithium carbonate, 1.41 kg of sodium sulfate, and 0.30 kg of iron oxide. Prepare the batch according to these components. First, pressurize the melting furnace until the internal pressure reaches 1.1 atmospheres. Then, melt the glass according to the following melting process: raise the temperature from room temperature to 1100℃ in 2 hours; raise the temperature from 1100℃ to 1500℃ in 2.5 hours and hold for 2 hours, while stirring and homogenizing. After homogenization, vent the gas out of the melting furnace, adjust the pressure balance inside and outside the furnace, start the furnace, discharge the material, quench it in water, crush and classify it, convey the powder, and collect the glass powder after hollow spheroidization in the bead-forming furnace through a cyclone collector and a bag filter. The collected glass powder is then separated into hollow glass microspheres by flotation.

[0021] Example 2

[0022] Weigh the following raw materials by weight: 56.48 kg of quartz sand, 1.74 kg of feldspar, 8.15 kg of calcium carbonate, 8.14 kg of alumina, 20.15 kg of soda ash, 1.98 kg of lithium carbonate, 1.41 kg of sodium sulfate, and 0.30 kg of iron oxide. Prepare the batch according to these components. First, pressurize the melting furnace until the internal pressure reaches 1.2 atmospheres. Then, melt the glass according to the following melting process: raise the temperature from room temperature to 1100℃ in 2 hours; raise the temperature from 1100℃ to 1500℃ in 2.5 hours and hold for 2 hours, while stirring and homogenizing. After homogenization, vent the gas out of the melting furnace, adjust the pressure balance inside and outside the furnace, start the furnace, discharge the material, quench it in water, crush and classify it, and convey the powder. The glass powder heated in the spheroidizing furnace is collected by a cyclone collector and a bag filter. The collected glass powder is then separated into hollow glass microspheres by flotation.

[0023] Example 3

[0024] Weigh the following raw materials by weight: 56.48 kg of quartz sand, 1.74 kg of feldspar, 8.15 kg of calcium carbonate, 8.14 kg of alumina, 20.15 kg of soda ash, 1.98 kg of lithium carbonate, 1.41 kg of sodium sulfate, and 0.30 kg of iron oxide. Prepare the batch according to these components. First, pressurize the melting furnace until the internal pressure reaches 1.3 atmospheres. Then, melt the glass according to the following melting process: raise the temperature from room temperature to 1100℃ in 2 hours; raise the temperature from 1100℃ to 1500℃ in 2.5 hours and hold for 2 hours, while stirring and homogenizing. After homogenization, discharge the gas from the melting furnace, adjust the pressure balance inside and outside the furnace, start the furnace, and proceed with water quenching, crushing and grading, powder conveying, and glass powder that has been hollowed out in the bead-forming furnace. Collect the glass powder through a cyclone collector and a bag filter. The collected glass powder is then separated into hollow glass microspheres using a flotation method.

[0025] Comparative Example 1

[0026] Weigh the following raw materials by weight: 56.48 kg of quartz sand, 1.74 kg of feldspar, 8.15 kg of calcium carbonate, 8.14 kg of alumina, 20.15 kg of soda ash, 1.98 kg of lithium carbonate, 1.41 kg of sodium sulfate, and 0.30 kg of iron oxide. Prepare the batch according to these components. Melt the glass under normal pressure: raise the temperature from room temperature to 1100℃ in 2 hours; raise the temperature from 1100℃ to 1500℃ in 2.5 hours and hold for 2 hours, while stirring and homogenizing. Start the furnace, discharge the glass, quench it in water, crush and classify it, convey the powder, and collect the glass powder after hollow spheroidization in the bead-forming furnace using a cyclone collector and a bag filter. Separate the collected glass powder into hollow glass microspheres using a flotation method.

[0027] The above three embodiments and one comparative example use the same glass batch and different melting regimes. The difference is that in Embodiments 1, 2 and 3, different furnace pressures were selected according to the pressurized melting and stirring homogenization method of the present invention: 1.1 standard atmospheres, 1.2 standard atmospheres and 1.3 standard atmospheres, respectively. Comparative Example 1 uses the existing conventional atmospheric pressure melting and clarification method, which reduces the number of bubbles in the glass melt, as shown in Table 1.

[0028] Table 1 Comparison of the effects of the embodiments and comparative examples.

[0029]

[0030] As can be seen from the table above, the pressing and homogenization method proposed in this invention can increase the amount of residual bubbles in the glass melt, and obtain high-quality glass raw materials for the powder method to prepare hollow glass microspheres with better absorption of bubbles by the glass melt.

[0031] The above description is merely an example and illustration of the present invention. Those skilled in the art can make various modifications or additions to the specific embodiments described, or use similar methods to replace them, as long as they do not deviate from the invention or exceed the scope defined in the claims, they should all fall within the protection scope of the present invention.

Claims

1. A method for improving the yield of hollow glass microsphere products by positive pressure melting and homogenization, comprising the steps of: preparing a glass batch for hollow glass microspheres, melting at an elevated temperature, homogenization, water quenching, crushing and grading, powder conveying, hollow sphere formation, and collection and sorting, characterized in that, The pressure treatment is performed before the melting process, and the pressure in the furnace is controlled at 101000-130000 Pa for 0.5-1 hour, and then the melting process is performed at a temperature of 1450-1550 DEG C for 6-7 hours with stirring and homogenization.

2. The method according to claim 1, wherein the method is characterized by, The collecting and sorting process is: collecting the powder after the hollow spheroidization in the beading furnace, including cyclone collection and cloth bag collection.

3. The method of claim 1, wherein the method is characterized by, The pressure in the furnace is 101000-105000 Pa.

4. The method of claim 1, wherein the method is characterized by, The pressure in the furnace is 105000-110000 Pa.

5. The method of claim 1, wherein the method is characterized by, The pressure in the furnace is 110000-120000 Pa.

6. The method of claim 1, wherein the method is characterized by, The pressure in the furnace is 120000-130000 Pa.

7. The method of claim 1, wherein the method is characterized by, The glass batch for the hollow glass microsphere includes the following raw materials in mass ratio: quartz sand 56.48 kg, feldspar 1.74 kg, calcium carbonate 8.15 kg, alumina 8.14 kg, soda ash 20.15 kg, lithium carbonate 1.98 kg, mirabilite 1.41 kg, and iron oxide 0.30 kg.

Citation Information

Patent Citations

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