CN114014527A - Aluminum-sealed phosphate glass powder spray granulation method - Google Patents
Aluminum-sealed phosphate glass powder spray granulation method Download PDFInfo
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- CN114014527A CN114014527A CN202111281096.XA CN202111281096A CN114014527A CN 114014527 A CN114014527 A CN 114014527A CN 202111281096 A CN202111281096 A CN 202111281096A CN 114014527 A CN114014527 A CN 114014527A
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- glass powder
- aluminum
- phosphate glass
- spray granulation
- sealed
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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
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2/00—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
- B01J2/02—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
- B01J2/04—Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a gaseous medium
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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
- C03B19/10—Forming beads
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Glass Compositions (AREA)
- Glanulating (AREA)
Abstract
The invention provides a method for spray granulation of aluminum-sealed phosphate glass powder, which comprises the following steps: s1: adding the adhesive into ethanol, putting the mixture into an oil bath kettle with magnetic stirring at the temperature of 80 ℃, mechanically stirring for 2 hours at the rotating speed of 100-120 r/min, preparing 15% of adhesive standard liquid in mass fraction, enabling the standard liquid to be clear and transparent, and standing for a period of time without adhesive precipitation; s2: adding ethanol into an alumina ceramic ball milling tank, then adding a dispersing agent, fully stirring by using a glass rod, and then adding grinding balls and phosphate glass powder for ball milling; s3: and adding the slurry obtained in the step S2 into the prepared binder standard solution according to the proportion of 1: 3-1: 5. The aluminum-sealed phosphate glass powder spray granulation method provided by the invention utilizes an organic solvent granulation method, preferably decomposes the binder and the dispersant at low temperature, solves the problem of aluminum-sealed phosphate glass granulation, fills the blank of organic solvent granulation, and also provides a granulation method of low-melting-point glass powder.
Description
Technical Field
The invention relates to the field of sealing of aluminum-sealed glass powder, in particular to a method for spraying and granulating aluminum-sealed phosphate glass powder.
Background
The aluminum alloy has a lower melting point of 660.32 ℃, and the sealing process requires that the sealing temperature is lower than the lowest melting point of the related metal, so the sealing temperature of the glass is required to be below 600 ℃, namely the glass needs to be sealed at a low temperature; on the other hand, aluminum has a thermal expansion coefficient of 23X 10-6The thermal expansion coefficient of the glass is (15-23) multiplied by 10 in order to meet the requirement of matching sealing at the temperature of/° C-6Within/° c. Phosphate glasses due to low TgThe larger CTE, has greater potential on aluminum encapsulated glass.
In addition, glass is often made into a glass blank before being used for sealing, in order to be pressed into a compact, glass powder needs to be mixed with organic matters such as a bonding agent, the organic matters need to be removed before a blank body is sintered and compacted, otherwise, bubbles can be generated in the glass body, the softening point of low-temperature sealing glass is generally less than 450 ℃, the complete decomposition temperature of a granulating powder bonding agent prepared by the traditional water-based granulating mode is about 560 ℃, the chemical stability of the glass powder is relatively poor due to the large expansion coefficient of phosphate glass, and the deviation of the components of the glass powder can be caused by water-based granulating.
Therefore, it is necessary to provide a method for spray granulation of aluminum-sealed phosphate glass powder to solve the above technical problems.
Disclosure of Invention
The invention provides a method for spray granulation of aluminum-sealed phosphate glass powder, which solves the problems of deviation of glass powder components, low preparation efficiency, poor sphericity and poor fluidity in the prior art.
In order to solve the technical problem, the aluminum-sealed phosphate glass powder spray granulation method provided by the invention comprises the following steps:
s1: adding the adhesive into ethanol, putting the mixture into an oil bath kettle with magnetic stirring at the temperature of 80 ℃, mechanically stirring for 2 hours at the rotating speed of 100-120 r/min, preparing 15% of adhesive standard liquid in mass fraction, enabling the standard liquid to be clear and transparent, and standing for a period of time without adhesive precipitation;
s2: adding ethanol into an alumina ceramic ball milling tank, then adding a dispersing agent, fully stirring by using a glass rod, adding grinding balls and phosphate glass powder, and ball milling for 40min, wherein the rotating speed is adjusted to 200-250 r/min;
s3: adding the slurry obtained in the step S2 into the prepared binder standard solution according to the proportion of 1: 3-1: 5, adjusting the rotating speed to 280-300 r/min, and performing ball milling for 80 min;
s4: and (4) taking out the glass powder slurry obtained in the step (S3), sieving the glass powder slurry by a 300-mesh sieve, putting the obtained slurry into a conical flask, and carrying out spray granulation.
Preferably, the binder is a low-temperature decomposition binder, and the prepared standard liquid solvent is consistent with the ball-milling powder solvent.
Preferably, the dispersant is an active polymeric dispersant soluble in organic solvents.
Preferably, the particle size of the phosphate glass powder is between 40 and 60 microns, and the grinding balls are zirconia balls.
Preferably, the ball-feed ratio during ball milling in the S2 is 1.2-1.5: 1, and the charging height is not higher than one third of the ball milling tank.
Preferably, the pH value of the slurry obtained in S3 is 6-7, and the Zeta potential is 15-25 mV.
Preferably, the spray granulator in S4 is an airflow pressure spray granulator with a tail gas recovery device, the inlet temperature of the spray granulator is 150-160 ℃, the outlet temperature of the spray granulator is 70-80 ℃, the feeding speed of the spray granulator is 15-20 mL/min, and the air flow rate of the spray granulator is 0.6-0.7 m3The nitrogen flow is 0.02-0.05 m3Min, the air pressure at the nozzle is 0.1 MPa.
Preferably, the powder prepared in the S4 is spherical particles, the particle size distribution range is 100-150 mu m, the angle of repose is 22-26 degrees, and the bulk density is 0.70-0.81 g/cm3The tap density is 0.83 to 1.04g/cm3。
Compared with the related technology, the aluminum-sealed phosphate glass powder spray granulation method provided by the invention has the following beneficial effects:
the invention provides a method for granulating aluminum-sealed phosphate glass powder by spraying, which utilizes an organic solvent granulation method, preferentially decomposes a binder and a dispersing agent at low temperature, solves the difficult problem of granulation of aluminum-sealed phosphate glass, fills the blank of granulation by an organic solvent, and also provides a method for granulating low-melting-point glass powder.
Detailed Description
The present invention will be further described with reference to the following embodiments.
First embodiment
The aluminum-sealed phosphate glass powder spray granulation method comprises the following steps:
s1: adding 30g of acrylic resin into 170g of ethanol, putting the mixture into an oil bath kettle with magnetic stirring at 80 ℃, rotating at 100r/min, and mechanically stirring for 2 h. Preparing 15% of adhesive standard solution in mass fraction, wherein the standard solution is clear and transparent, and no adhesive is separated out after standing for a period of time;
s2: adding 63g of ethanol into an alumina ceramic ball milling tank, then adding 1g of dispersing agent, fully and uniformly stirring by using a glass rod, adding 130g of grinding balls and 100g of phosphate glass powder, and ball milling for 40min at a rotation speed of 250 r/min;
s3: and (4) adding 20g of prepared standard binder solution into the slurry obtained in the step (S2), adjusting the rotating speed to 300r/min, and performing ball milling for 80 min.
S4: and (4) taking out the glass powder slurry obtained in the step (S3), sieving the glass powder slurry by a 300-mesh sieve, putting the slurry into a conical flask, and performing spray granulation.
The inlet temperature of spray granulation is 150 ℃, the outlet temperature is 80 ℃, the feeding speed is 20mL/min, and the air flow is 0.6m3Min, nitrogen flow 0.04m3Min, the air pressure at the nozzle is 0.1 MPa.
According to the scheme, the pH of the slurry in S3 is 6, the Zeta potential is 20mV, the powder prepared in S4 is spherical particles, the particle size distribution range is 100-150 mu m, the angle of repose is 22 degrees, the apparent density is 0.72g/cm3, and the tap density is 0.76 g/cm.
Second embodiment
The aluminum-sealed phosphate glass powder spray granulation method comprises the following steps:
s1: adding 30g of acrylic resin into 170g of ethanol, putting the mixture into an oil bath kettle with magnetic stirring at 80 ℃, rotating at 100r/min, and mechanically stirring for 2 h. Preparing 15% of adhesive standard solution by mass fraction, wherein the standard solution is clear and transparent, and no adhesive is separated out after standing for a period of time.
S2: adding 83g of ethanol into an alumina ceramic ball milling tank, then adding 1.1g of dispersing agent, fully and uniformly stirring by using a glass rod, adding 150g of grinding balls and 100g of phosphate glass powder, and ball milling for 40min at a rotation speed of 250 r/min.
S3: and (4) adding 33g of prepared standard binder solution into the slurry obtained in the step S2, adjusting the rotating speed to 300r/min, and ball milling for 80 min.
S4: and (4) taking out the glass powder slurry obtained in the step (S3), sieving the glass powder slurry by a 300-mesh sieve, putting the slurry into a conical flask, and performing spray granulation.
The inlet temperature of spray granulation is 150 ℃, the outlet temperature is 80 ℃, the feeding speed is 20mL/min, and the air flow is 0.6m3Min, nitrogen flow 0.04m3Min, the air pressure at the nozzle is 0.1 MPa.
According to the scheme, the pH of the slurry obtained in S3 is 7, the Zeta potential is 18.2mV, the powder prepared in S4 is spherical particles, the particle size distribution range is 80-130 mu m, the angle of repose is 24 degrees, and the apparent density is 0.75g/cm3The tap density is 0.94g/cm3。
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes performed by the present invention or directly or indirectly applied to other related technical fields are included in the scope of the present invention.
Claims (8)
1. The aluminum-sealed phosphate glass powder spray granulation method is characterized by comprising the following steps:
s1: adding the adhesive into ethanol, putting the mixture into an oil bath kettle with magnetic stirring at the temperature of 80 ℃, mechanically stirring for 2 hours at the rotating speed of 100-120 r/min, preparing 15% of adhesive standard liquid in mass fraction, enabling the standard liquid to be clear and transparent, and standing for a period of time without adhesive precipitation;
s2: adding ethanol into an alumina ceramic ball milling tank, then adding a dispersing agent, fully stirring by using a glass rod, adding grinding balls and phosphate glass powder, and ball milling for 40min, wherein the rotating speed is adjusted to 200-250 r/min;
s3: adding the slurry obtained in the step S2 into the prepared binder standard solution according to the proportion of 1: 3-1: 5, adjusting the rotating speed to 280-300 r/min, and performing ball milling for 80 min;
s4: and (4) taking out the glass powder slurry obtained in the step (S3), sieving the glass powder slurry by a 300-mesh sieve, putting the obtained slurry into a conical flask, and carrying out spray granulation.
2. The method for spray granulation of aluminum-sealed phosphate glass powder according to claim 1, wherein the binder is a low-temperature decomposition binder, and the prepared standard liquid solvent is consistent with the ball-milled powder solvent.
3. The method of claim 1, wherein the dispersant is an active polymeric dispersant soluble in an organic solvent.
4. The method for spray granulation of an aluminum-sealed phosphate glass powder according to claim 1, wherein the particle size of the phosphate glass powder is between 40 μm and 60 μm, and the grinding balls are zirconia balls.
5. The spray granulation method of the aluminum-sealed phosphate glass powder according to claim 1, wherein the ball-to-feed ratio in the ball milling in S2 is 1.2-1.5: 1, and the charging height is not higher than one third of the ball milling tank.
6. The method for spray granulation of aluminum-sealed phosphate glass powder according to claim 1, wherein the pH value of the slurry obtained in S3 is 6-7, and the Zeta potential is 15-25 mV.
7. The method for spray granulation of aluminum-sealed phosphate glass powder according to claim 1, wherein the spray granulator used in S4 is an air-flow pressure spray granulator with a tail gas recovery device, the inlet temperature of the spray granulation is 150-160 ℃, the outlet temperature is 70-80 ℃, the feeding speed is 15-20 mL/min, and the air flow rate is 0.6-0.7 m3The nitrogen flow is 0.02-0.05 m3Min, the air pressure at the nozzle is 0.1 MPa.
8. The method for spray granulation of aluminum-sealed phosphate glass powder according to claim 1, wherein the powder prepared in S4 is spherical particles, the particle size distribution range is 100-150 μm, the angle of repose is 22-26 degrees, and the bulk density is 0.70-0.81 g/cm3The tap density is 0.83 to 1.04g/cm3。
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| CN202111281096.XA CN114014527B (en) | 2021-11-01 | 2021-11-01 | Spray granulation method for aluminum-sealed phosphate glass powder |
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| CN202111281096.XA CN114014527B (en) | 2021-11-01 | 2021-11-01 | Spray granulation method for aluminum-sealed phosphate glass powder |
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| CN114014527A true CN114014527A (en) | 2022-02-08 |
| CN114014527B CN114014527B (en) | 2023-07-14 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116768484A (en) * | 2023-06-27 | 2023-09-19 | 江西盛富莱光学科技股份有限公司 | Method for preparing high-refractive-index reflective glass beads from glass dust removal powder |
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| JP2018020947A (en) * | 2016-07-20 | 2018-02-08 | 株式会社ノリタケカンパニーリミテド | Green sheet for encapsulation |
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| CN113200744A (en) * | 2021-04-25 | 2021-08-03 | 湖南省美程陶瓷科技有限公司 | Lead-free piezoelectric ceramic sensor material and preparation method thereof |
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2021
- 2021-11-01 CN CN202111281096.XA patent/CN114014527B/en active Active
Patent Citations (6)
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| JP2018020947A (en) * | 2016-07-20 | 2018-02-08 | 株式会社ノリタケカンパニーリミテド | Green sheet for encapsulation |
| CN112551902A (en) * | 2019-09-25 | 2021-03-26 | 中国科学院上海硅酸盐研究所 | Low-melting-point glass powder containing alkaline earth metal and preparation method and application thereof |
| CN111499417A (en) * | 2020-04-24 | 2020-08-07 | 湖南省美程陶瓷科技有限公司 | Insulating ring for microwave magnetron and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116768484A (en) * | 2023-06-27 | 2023-09-19 | 江西盛富莱光学科技股份有限公司 | Method for preparing high-refractive-index reflective glass beads from glass dust removal powder |
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| CN114014527B (en) | 2023-07-14 |
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