CN112830665A - Preparation method of glass beads through secondary beading - Google Patents

Preparation method of glass beads through secondary beading Download PDF

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Publication number
CN112830665A
CN112830665A CN202110224851.4A CN202110224851A CN112830665A CN 112830665 A CN112830665 A CN 112830665A CN 202110224851 A CN202110224851 A CN 202110224851A CN 112830665 A CN112830665 A CN 112830665A
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China
Prior art keywords
microbeads
beading
screening
powder
batch
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Inventor
应展杰
金俊嵩
胡源发
胡新艳
胡敏敏
潘向阳
原露能
原小向
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Shanxi Yemingzhu Technology Co ltd
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Shanxi Yemingzhu Technology Co ltd
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Priority to CN202110224851.4A priority Critical patent/CN112830665A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/10Forming beads
    • C03B19/1005Forming solid beads
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B1/00Preparing the batches
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00Technologies relating to the processing of minerals
    • Y02P40/50Glass production, e.g. reusing waste heat during processing or shaping
    • Y02P40/57Improving the yield, e-g- reduction of reject rates

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Glass Compositions (AREA)

Abstract

The invention provides a preparation method of secondary beading of glass beads, and relates to the technical field of glass bead manufacturing. The preparation method comprises the following steps: (1) pretreating the raw materials to obtain a sand material, crushing and screening the sand material for the first time to obtain powder, and performing first beading and spheroidizing on the powder to obtain a first batch of microbeads; (2) and screening the microbeads of the first batch for the second time, screening the microbeads with different grain sizes for the second balling and spheroidizing to obtain microbeads of the second batch. The preparation method reduces the devitrification rate and improves the retroreflection coefficient, the particle size distribution is uniform, and the product quality of the prepared glass beads is improved; the quality problem of the product can be controlled at any time, equipment is not required to be cleaned and maintained frequently, and the yield is improved quickly.

Description

Preparation method of glass beads through secondary beading
Technical Field
The invention relates to the technical field of glass bead manufacturing, in particular to a preparation method of secondary beading of glass beads.
Background
The glass beads are solid or hollow glass beads having a diameter of several micrometers to several millimeters, and are generally referred to as fine beads having a diameter of 0.8mm or more and beads having a diameter of 0.8mm or less. The glass microspheres have the characteristics of transparency, adjustable refractive index, directional retro-reflection, stable chemical property, high heat resistance, high mechanical strength and the like, are mainly used for retro-reflecting glass microspheres for roads, are commonly used in the fields of roads such as road signboards, license plates, advertising films and the like, aerospace and the like, and have large market demand.
At present, a powder method is usually adopted for preparing glass beads, and the basic principle of the powder method is that glass is crushed into required particles, the particles pass through a uniform heating area at a certain temperature after being screened, so that the glass particles are melted, and the beads are formed under the action of surface tension. However, the glass bead products in the current market adopt a water bath beading (powder method), the productivity is low, the devitrification rate is high, and the quality is unstable.
Therefore, it is urgently needed to develop a method for preparing glass beads, which can improve and stabilize the product quality and improve the production performance.
Disclosure of Invention
The invention provides a preparation method of secondary beading of glass beads, which comprises the following steps:
(1) pretreating the raw materials to obtain a sand material, crushing and screening the sand material for the first time to obtain powder, and performing first beading and spheroidizing on the powder to obtain a first batch of microbeads;
(2) and screening the microbeads of the first batch for the second time, screening the microbeads with different grain sizes for the second balling and spheroidizing to obtain microbeads of the second batch.
In the invention, the raw materials for preparing the glass beads are pretreated and crushed and then are subjected to beading and spheroidizing twice. The preparation method of the secondary beading is an innovative improvement on the basis of the original water bath beading. The original water bath beading process included: proportioning raw materials, melting, water cooling, drying, air flow crushing, coarse screening (grading), balling (balling) powder, cooling the balling glass beads by water, drying the collected water-carrying glass beads by fire after being transported to post-treatment, fine screening (grading), (unqualified inspection and beading again), proportioning after mixing, treating foreign matters, packaging and warehousing. As such, water bath beading has the following disadvantages: the drying consumes manpower, the product quality is not good, the control is not good (the devitrification rate is high, the quality is unstable), the bead-forming cooling spray head is frequently cleaned (at least once per week), and the productivity is not rapidly improved.
The secondary beading process flow of the invention comprises the following steps: proportioning raw materials, melting, water cooling, drying, air flow crushing, coarse screening (primary screening and grading), performing primary beading (spheroidizing) on powder, screening (secondary screening and grading), performing secondary beading (air cooling and spray water cooling are used for cooling, the finished product just dries the moisture) on the first batch of microbeads with the same size, performing fine screening (grading), checking unqualified beading again, mixing, proportioning after mixing, treating foreign matters, packaging and warehousing. Therefore, the secondary beading process of the invention has the following advantages: the second batch of microbead products obtained by secondary beading can be directly subjected to fine screening (grading) for a dry material, the quality problem of the products can be controlled at any time, equipment is not required to be cleaned and maintained frequently, and the yield is increased quickly.
Further, on the basis of the technical scheme provided by the invention, the raw materials comprise at least two of titanium dioxide, calcium carbonate, barium carbonate, zinc oxide, quartz sand, zircon sand and soda ash.
Further, the pretreatment of the raw materials comprises melting, cooling and drying. Wherein, the melting process can be carried out 1300-1350 ℃ high-temperature melting treatment after the materials are proportioned according to the respective metering and batching systems of the smelting furnaces. The cooling can be preferably carried out by air cooling or spray water cooling, for example, the water gun is used for atomizing water to achieve the effect of cooling, so that the devitrification rate of the glass beads can be reduced; drying may preferably be by elevated temperature drying, such as fire drying.
Further, on the basis of the technical scheme provided by the invention, the grain size of the sand material is 1-4 mm; and/or the particle size of the powder is 38-75 μm.
The grit size may typically, but not exclusively, be 1mm, 2mm, 3mm, 4 mm.
The particle size of the powder may typically, but not exclusively, be 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 32 μm, 38 μm, 40 μm, 43 μm, 45 μm, 48 μm, 50 μm, 53 μm, 55 μm, 58 μm, 60 μm, 62 μm, 66 μm, 68 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm.
The method of pulverizing the sand is not particularly limited, and jet milling may be preferable. The grain diameters of the sand material and the powder material are optimized, so that the powder material is conveniently beaded and spheroidized, the product quality of the prepared glass beads can be improved, the product with proper grain diameter can be prepared more easily,
further, on the basis of the technical scheme provided by the invention, the temperature for the first beading is 850-870 ℃, and preferably 870 ℃.
Preferably, the first balling temperature is about 870 ℃, and the powder (powder) with different shapes is instantaneously balling into round microbeads. The primary purpose of the first beading is to make the powder spherical and to make the glass beads preliminarily shaped.
Further, on the basis of the technical scheme provided by the invention, microbeads with the particle sizes of 5-32 μm, 32-38 μm, 38-45 μm, 45-53 μm, 53-63 μm, 63-75 μm and 75-90 μm are screened out by a second screening, and microbeads with the same particle size range are beaded for the second time.
After the first batch of microbeads are obtained, different particle sizes are screened, and then the microbeads with the same particle size range are subjected to secondary beading in a beading furnace, for example, the glass microbeads with different particle sizes can be divided once, so that the particle size difference of the finished glass microbeads is reduced, secondary beading is facilitated, and the quality of beaded products is controlled.
Further, on the basis of the technical scheme provided by the invention, the temperature of the second beading is 850-950 ℃, and preferably 900 ℃.
Further, the flow rate of the second beading was controlled at 10 to 20 g/6 sec.
The temperature and the flow rate of the second balling are controlled, so that the obtained second batch of microbeads can be directly subjected to fine screening (classification) as the dry materials, and the product quality of the prepared glass microbeads is improved.
Further, on the basis of the technical scheme provided by the invention, oxygen is added for combustion supporting in the second beading, and the gas flow is 17-25m3H, air flow rate of 70-80m3H, oxygen flow of 7-14m3/h。
The sizes of fuel gas, air and oxygen are adjusted according to the product quality, oxygen is added for combustion supporting in the second beading process, the fuel gas achieves the effect of complete combustion, and the secondary beading process is carried out more smoothly.
Further, on the basis of the technical scheme provided by the invention, the secondary beading preparation method of the glass beads comprises the following steps:
(1) melting, cooling and drying the raw materials to obtain a sand material;
(2) grinding and screening the sand material for the first time to obtain powder, and performing first beading and spheroidizing on the powder to obtain a first batch of microbeads;
(3) carrying out the second screening after the first balling and spheroidizing to screen out microbeads with different particle sizes;
(4) microbeads of the same particle size range are beaded a second time to obtain a second batch of microbeads.
In a preferred embodiment of the present invention, the method for preparing the glass beads by secondary beading comprises the following steps:
(1) the raw materials are subjected to melting, cooling and drying pretreatment to obtain sand materials, wherein the grain diameter of the sand materials is 1-4 mm;
(2) crushing and screening the sand material for the first time to obtain powder (the particle size of the powder is 38-75 mu m), and performing primary balling and spheroidizing on the powder in a balling furnace at the temperature of 850-;
(3) carrying out secondary screening after the first beading and spheroidizing to screen out microbeads with different particle sizes of 5-32 μm, 32-38 μm, 38-45 μm, 45-53 μm, 53-63 μm, 63-75 μm and 75-90 μm;
(4) the microbeads with the same particle size range are beaded for the second time in a beading furnace at the temperature of 900-1000 ℃, the flow rate is controlled at 10-20 g/6 s and the gas flow rate is 20-22m3H, air flow rate of 70-74m3H, oxygen flow rate of 10-14m3/h,A second batch of microbeads was obtained.
The invention provides the glass beads obtained by the secondary beading preparation method of the glass beads in the second aspect.
The glass microspheres prepared by the preparation method have the advantages of low devitrification rate, high retroreflection coefficient and the like.
The invention adopts the technical scheme and has the following beneficial effects:
(1) the preparation method of the glass beads by secondary beading reduces the devitrification rate, improves the retroreflection coefficient, has uniform particle size distribution, and improves the product quality of the prepared glass beads
(2) According to the preparation method of the glass beads through secondary beading, the quality problem of the product can be controlled at any time, equipment does not need to be cleaned and maintained frequently, and the productivity is improved quickly.
Detailed Description
Unless defined otherwise, all scientific and technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The invention is described in detail below with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Example 1
A secondary beading preparation method of glass beads comprises the following steps:
(1) the raw materials are subjected to melting, cooling and drying pretreatment to obtain sand materials, wherein the particle size range of the sand materials is 1-4 mm;
(2) grinding and screening the sand material for the first time to obtain powder (the particle size range of the powder is 38-75 mu m), and performing first balling and spheroidizing on the powder in a balling furnace at the temperature of 850 ℃ to obtain a first batch of microbeads;
(3) carrying out secondary screening after the first beading and spheroidizing to screen out microbeads with different particle sizes of 5-32 μm, 32-38 μm, 38-45 μm, 45-53 μm, 53-63 μm, 63-75 μm and 75-90 μm;
(4) the microbeads with the same particle size range are beaded for the second time in a beading furnace at 900 ℃, the flow rate is controlled to be 10-20 g/6 s, and the fuel gas flow rate is 21m3Flow rate of air/h 72m3H, oxygen flow rate 11m3H, obtaining a second batch of microbeads.
Example 2
A secondary beading preparation method of glass beads comprises the following steps:
(1) the raw materials are subjected to melting, cooling and drying pretreatment to obtain sand materials, wherein the particle size range of the sand materials is 1-4 mm;
(2) grinding and screening the sand material for the first time to obtain powder (the particle size of the powder is 38-75 mu m), and performing first balling and spheroidizing on the powder in a balling furnace at the temperature of 870 ℃ to obtain a first batch of microbeads;
(3) carrying out secondary screening after the first beading and spheroidizing to screen out microbeads with different particle sizes of 5-32 μm, 32-38 μm, 38-45 μm, 45-53 μm, 53-63 μm, 63-75 μm and 75-90 μm;
(4) the microbeads with the same particle size range are beaded for the second time in a beading furnace at 850 ℃, the flow rate is controlled to be 10-20 g/6 s, and the gas flow rate is 17m3Flow rate of air/h 70m3H, oxygen flow 7m3H, obtaining a second batch of microbeads.
Example 3
A secondary beading preparation method of glass beads comprises the following steps:
(1) the raw materials are subjected to melting, cooling and drying pretreatment to obtain sand materials, wherein the particle size range of the sand materials is 1-4 mm;
(2) grinding and screening the sand material for the first time to obtain powder (the particle size of the powder is 38-75 mu m), and performing first balling and spheroidizing on the powder in a balling furnace at the temperature of 870 ℃ to obtain a first batch of microbeads;
(3) carrying out secondary screening after the first beading and spheroidizing to screen out microbeads with different particle sizes of 5-32 μm, 32-38 μm, 38-45 μm, 45-53 μm, 53-63 μm, 63-75 μm and 75-90 μm;
(4) the microbeads with the same particle size range are beaded for the second time in a beading furnace, the temperature is 950 ℃, the flow rate is controlled to be 10-20 g/6 s, and the gas flow rate is 25m3Flow rate of air/h 80m3H, oxygen flow 14m3H, obtaining a second batch of microbeads.
Example 4
The difference between the preparation method of the glass bead by secondary beading and the example 1 is that the grain size of the sand material is 5-6 mm.
Example 5
A method for preparing glass beads by secondary beading is different from that of example 1 in that the particle size of the powder is in the range of 90 to 100 μm.
Example 6
A method for preparing glass beads by secondary beading is different from that of example 1 in that the flow rate is controlled to 22 to 25 g/6 sec.
Comparative example 1
A secondary beading preparation method of glass beads comprises the following steps:
(1) the raw materials are subjected to melting, cooling and drying pretreatment to obtain sand materials, wherein the particle size range of the sand materials is 1-4 mm;
(2) grinding sand and screening for the first time to obtain powder (the particle size of the powder is 38-75 μm), balling the powder in a balling furnace at 870 deg.C for 10-20 g/6 s and gas flow of 21m3Flow rate of air/h 72m3H, oxygen flow rate 11m3H, obtaining the micro-beads;
(3) cooling the spheroidized glass beads by water, and conveying the collected water-carrying glass beads to post-treatment for drying by fire.
Comparative example 2
A method for preparing glass beads by secondary beading is different from the method in example 1 in that microbeads with different grain sizes of 38-53 mu m and 53-75 mu m are screened in step (3).
Comparative example 3
The preparation method of the glass beads by secondary beading is different from the example 1 in that oxygen is not added for combustion supporting in the step (4).
Comparative example 4
A method for preparing glass beads by secondary beading is different from the method in example 1 in that the oxygen flow in the step (4) is 5m3/h。
The raw materials used in the above examples and comparative examples were titanium dioxide, calcium carbonate, barium carbonate, zinc oxide, quartz sand, zircon sand, and soda ash.
Testing of glass Microbead Performance
The glass beads obtained in examples 1 to 6 and comparative examples 1 to 4 were finely sieved, and glass beads having a particle size in the range of 32 to 45 μm were respectively finely sieved for use.
The appearance, the refractive index, the devitrification rate and the retroreflection coefficient of the glass microspheres are tested according to the test label in transport industry standard JT/T1035.1-2016 of Ministry of transportation of the people's republic of China, and the specific test result is shown in Table 1.
TABLE 1
Figure DEST_PATH_IMAGE002
As can be seen from the results in table 1, in the method for preparing the glass microspheres by secondary beading according to the present invention, the particle size ranges of the selected sand and powder, the flow rate in the beading furnace, and the factors of increasing oxygen combustion supporting and beading again with the particle size during the secondary beading process all affect some properties of the finally obtained glass microspheres, such as devitrification rate and retroreflection coefficient.
In addition, the experimental data of comparative example 1 show that the secondary beading process of the present invention significantly improves the performance of glass beads, such as reducing devitrification rate and increasing retroreflective factor, compared to the conventional water bath beading.
In summary, the method for preparing the glass beads by secondary beading not only needs the factors such as the particle size of the raw materials and the reaction conditions to meet the requirements, but also needs continuous matching use among the reaction steps to improve the performance of the glass beads, so that the quality of the glass beads is more stable, the productivity is improved, and the market demand is better met.
The glass beads having particle diameters of 32 to 38 μm, 38 to 45 μm, 45 to 53 μm, 53 to 63 μm, and 63 to 75 μm obtained in example 1 were respectively tested for brightness, and the test results are shown in Table 2.
TABLE 2 Brightness of glass beads (Brightness before plating aluminum)
Glass particle diameter (mum) Brightness of light
32-38 1.7-2.1
38-45 2.4-3.1
45-53 3.2-3.9
53-63 3.4-4.1
63-75 3.9-4.6
From the results of table 2, it is understood that the glass particles prepared in example 1 of the present invention have excellent appearance with good brightness in each particle size range.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and the like that are within the spirit and principle of the present invention are included in the present invention.

Claims (10)

1. The preparation method of the glass beads through secondary beading is characterized by comprising the following steps:
(1) pretreating the raw materials to obtain a sand material, crushing and screening the sand material for the first time to obtain powder, and performing first beading and spheroidizing on the powder to obtain a first batch of microbeads;
(2) and screening the microbeads of the first batch for the second time, screening the microbeads with different grain sizes for the second balling and spheroidizing to obtain microbeads of the second batch.
2. The preparation method according to claim 1, wherein the raw materials comprise at least two of titanium dioxide, calcium carbonate, barium carbonate, zinc oxide, quartz sand, zircon sand and soda;
preferably, the pretreatment of the raw material comprises melting, cooling and drying.
3. The method according to claim 1, wherein the sand material has a particle size of 1-4 mm; and/or the particle size of the powder is 38-75 μm.
4. The method according to any one of claims 1 to 3, wherein the temperature for the first beading is 850 ℃ and 870 ℃, preferably 870 ℃.
5. The method according to claim 1, wherein microbeads having a particle size of 5 to 32 μm, 32 to 38 μm, 38 to 45 μm, 45 to 53 μm, 53 to 63 μm, 63 to 75 μm and 75 to 90 μm are sieved out by the second sieving, and microbeads having the same particle size range are beaded for the second time.
6. The method according to claim 5, wherein the second beading temperature is 850-.
7. The method of claim 5, wherein the flow rate of the second beading is controlled at 10 to 20 g/6 sec.
8. The preparation method according to any one of claims 5 to 7, wherein oxygen is added for combustion supporting in the second beading, and the fuel gas flow is 17 to 25m3H, air flow rate of 70-80m3H, oxygen flow of 7-14m3/h。
9. The method of claim 1, comprising the steps of:
(1) melting, cooling and drying the raw materials to obtain a sand material;
(2) grinding and screening the sand material for the first time to obtain powder, and performing first beading and spheroidizing on the powder to obtain a first batch of microbeads;
(3) carrying out the second screening after the first balling and spheroidizing to screen out microbeads with different particle sizes;
(4) microbeads of the same particle size range are beaded a second time to obtain a second batch of microbeads.
10. Glass microspheres produced by the production method according to any one of claims 1 to 9.
CN202110224851.4A 2021-03-01 2021-03-01 Preparation method of glass beads through secondary beading Pending CN112830665A (en)

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CN107673606A (en) * 2017-11-02 2018-02-09 江西盛汇光学科技协同创新有限公司 Utilize the unrecovered method and device for preparing glass microballoon of waste glass powder
CN208449855U (en) * 2018-05-29 2019-02-01 山西夜明珠科技有限公司 A kind of glass micro-bead screening apparatus
CN110963699A (en) * 2019-12-30 2020-04-07 兴化市红阳玻璃制品有限公司 Method and equipment for improving refractive index of glass beads
CN111499206A (en) * 2020-06-04 2020-08-07 石家庄东昊化工研究院有限公司 Method for preparing hollow glass microspheres by using silico slag containing fluosilicic acid

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1292358A (en) * 1999-06-24 2001-04-25 中国科学院光电技术研究所 Leadless high-refractivity microbead glass
CN101638291A (en) * 2008-07-30 2010-02-03 中国建材国际工程有限公司 Method and device for balling hollow glass microballoons through oxygen-enriched combustion
CN101638295A (en) * 2008-07-30 2010-02-03 中国建材国际工程有限公司 Hollow glass microballoons and production method thereof
CN102086087A (en) * 2009-12-08 2011-06-08 沈阳临德陶瓷研发有限公司 Method for preparing glass microspheres with high refractive index
US9016090B2 (en) * 2013-06-12 2015-04-28 Hamid Hojaji Glass microspheres comprising sulfide, and methods of producing glass microspheres
CN105271647A (en) * 2015-11-05 2016-01-27 中国建材国际工程集团有限公司 Method for preparing hollow glass beads through waste glass
CN107586043A (en) * 2017-09-06 2018-01-16 安徽凯盛基础材料科技有限公司 Quan Haishen hollow glass micropearls and preparation method thereof
CN107673606A (en) * 2017-11-02 2018-02-09 江西盛汇光学科技协同创新有限公司 Utilize the unrecovered method and device for preparing glass microballoon of waste glass powder
CN208449855U (en) * 2018-05-29 2019-02-01 山西夜明珠科技有限公司 A kind of glass micro-bead screening apparatus
CN110963699A (en) * 2019-12-30 2020-04-07 兴化市红阳玻璃制品有限公司 Method and equipment for improving refractive index of glass beads
CN111499206A (en) * 2020-06-04 2020-08-07 石家庄东昊化工研究院有限公司 Method for preparing hollow glass microspheres by using silico slag containing fluosilicic acid

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Application publication date: 20210525