CN108395108A - A kind of glass microballoon and preparation method thereof - Google Patents

A kind of glass microballoon and preparation method thereof Download PDF

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Publication number
CN108395108A
CN108395108A CN201810476762.7A CN201810476762A CN108395108A CN 108395108 A CN108395108 A CN 108395108A CN 201810476762 A CN201810476762 A CN 201810476762A CN 108395108 A CN108395108 A CN 108395108A
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China
Prior art keywords
parts
glass microballoon
raw material
preparation
drying
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CN201810476762.7A
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CN108395108B (en
Inventor
窦明岳
张宏生
王光
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Guangdong Datong Datong Environmental Protection Technology Co Ltd
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Guangdong Datong Datong Environmental Protection Technology Co Ltd
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Priority to CN201810476762.7A priority Critical patent/CN108395108B/en
Publication of CN108395108A publication Critical patent/CN108395108A/en
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03CCHEMICAL 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
    • C03C12/00Powdered glass; Bead compositions
    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B19/00Other methods of shaping glass
    • C03B19/10Forming beads
    • C03B19/107Forming hollow beads

Abstract

The invention discloses a kind of glass microballoon, raw material includes by weight:75 90 parts of flyash and cullet, 5 12 parts of binder, 38 parts of sintering aid, 25 parts of colorant.The invention also discloses the preparation methods of the glass microballoon, include the following steps:Ball milling:Add the raw material into ball milling in ball-grinding machine;Mixing granulation:Raw material after ball milling is weighed in parts by weight, is then added in granulator by initial stage, mid-term, three stirring-granulating stages of latter stage, and water is added in the mid-term stirring-granulating stage, stirring-granulating terminates and filters out pellet;Drying:Obtained pellet is dried in drying equipment;Sintering:By the pellet after drying and processing through oversintering, last Temperature fall obtains glass microballoon.The glass microballoon sphericity higher that raw material proportioning and preparation method are prepared through the invention, while cost is lower as glass microballoon made of raw material compared with using pure glass micro mist, moreover it is possible to the glass microballoon of different color is made as needed.

Description

A kind of glass microballoon and preparation method thereof
Technical field
The invention belongs to glass microballoon technical field, a kind of glass microballoon and preparation method thereof is related particularly to.
Background technology
The preparation method of glass microballoon mainly uses glass micro mist at present, disperses by equipment or chemicals, then burns Knot obtains, and is mainly used in the fields such as electronics, traffic, navigation, is the manufacture raw material of the products such as high reflective original paper, high reflective membrane. Such as patent " high-brightness glass micro-bead and its preparation process " (application number 200810107355.5), a kind of " production of glass microballoon Method " (application number 00110639.2), " a kind of production method and its device of high roundness glass microballoon " (application number 201610926955.9) a kind of, " preparation method of porous glass beads " (application number 201310678782.X), a kind of " utilization Glass micro mist is all made of in the method that cullet prepares fine-celled foam glass " (application number 201310529973.X) as main former Material, preparation method cause the manufacturing cost of glass microballoon relatively high, spend larger.Therefore it provides a kind of manufacturing cost Relatively low and simple and direct preparation process glass microballoon and preparation method thereof is this field technical problem urgently to be resolved hurrily.
Invention content
The object of the present invention is to provide a kind of higher glass microballoon of sphericity and the lower glass microballoons of manufacturing cost Preparation method.
To achieve the above object, the technical scheme is that:
A kind of glass microballoon, raw material include in parts by weight:75-90 parts of flyash and cullet, 5-12 parts viscous Tie agent, 3-8 parts of sintering aid, 2-5 parts of colorant.
Further, the parts by weight of flyash are 25-50 parts.
Preferably, binder is one or more of bentonite, kaolin, waterglass.
Preferably, sintering aid is one or both of miberal powder, perlite.
A kind of preparation method of glass microballoon, includes the following steps:
(1) ball milling:It adds the raw material into ball-grinding machine ball milling 1-3 hours;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight, be then added in granulator by initial stage, Mid-term, three stirring-granulating stages of latter stage, and water is added in the mid-term stirring-granulating stage, after stirring-granulating and filter out Pellet;
(3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, last Temperature fall obtains glass Glass microballon.
Further, in step (2) rotating speed of initial stage stirring-granulating be 750-1500r/min, mixing time 1- 3min;The rotating speed of mid-term stirring-granulating is 3000-4500r/min, mixing time 4-8min;The rotating speed of latter stage stirring-granulating is 1000-2000r/min, mixing time 0.5-2min.
Further, mid-term stirring-granulating stage amount of water is 13-20 parts in step (2).
Further, the grain size of the pellet filtered out in step (2) is 20-100 mesh.
Further, drying temperature is 70-150 DEG C in step (3), drying time 1-5h.
Further, sintering processes process is in step (4):First 400 are warming up to 10-25 DEG C/min heating rates~ 600 DEG C, then 650~850 DEG C are warming up to 1-8 DEG C/min heating rates, and keep the temperature 10-30min.
Compared with prior art, it is an advantage of the invention that:
1, the present invention substitutes segment glass micro mist using flyash as primary raw material, and the additive amount of flyash is by weight Number calculates between 25-50 parts, can reduce the cost of whole raw material.
2, the present invention uses non-slurry pelletizing, and the mixing granulation " single step " in granulator of each raw material after weighing is completed, section Water is energy saving.Mixing in the present invention is carried out with granulation in granulator, and initial stage is under low speed (rotating speed 750-1500r/min) The mixing and granulation of raw material are carried out, mid-term is promoted to high speed (rotating speed 3000-4500r/min) and is granulated and is added water, shape At solid close sphere, the later stage repairs pellet surface under low speed (rotating speed 1000-2000r/min), improves ball Shape degree.Due to using non-slurry pelletizing, water content is low when raw material mixing granulation, and drying time is short, and the pellet after drying has certain Mechanical strength, it is non-breakable, convenient for sintering.Sintering process heating rate early period is very fast (first with 10-25 DEG C/min heating rates It is warming up to 400~600 DEG C), later stage high temperature section heating rate slows down (is warming up to 650~850 with 1-8 DEG C/min heating rates again DEG C), the extraneous temperature difference with pellet interior is advantageously reduced, the generation of defect is reduced.
3, the glass microballoon sphericity higher that middle raw material proportioning and preparation method are prepared through the invention, by mixed It is full particle to close the particle that is formed after being granulated, and sphericity can reach 70% or more, sintered glass microsphere sphericity higher, 95% or more can be reached.Cost is lower as glass microballoon made of raw material compared with using pure glass micro mist simultaneously, and as needed also The glass microballoon of different color can be made.The entire preparation method of the present invention is simple and direct, and production efficiency is high, is suitble to industry metaplasia Production.
Specific implementation mode
Technical solution in the embodiment of the present invention is subjected to clear, complete description below, it is clear that described implementation Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common All other embodiment for being obtained without making creative work of technical staff, belong to the guarantor of the present invention Protect range.
Embodiment 1
A kind of preparation method of glass microballoon, includes the following steps:
(1) ball milling:Add the raw material into ball milling 3 hours in ball-grinding machine;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight --- 25 parts of flyash, 50 parts of cullet are swollen 7 parts of profit soil, 5 parts of waterglass, 8 parts of miberal powder, 5 parts of red stain is then added in granulator and is stirred granulations, initial stage elder generation with The rotating speed of 750r/min stirs 1min, and rotating speed is promoted to 3000r/min and 20 parts of water is added by mid-term, stirs 4min, latter stage Rotating speed is reduced to 1000r/min, stirs 0.5min;After stirring-granulating and filter out the pellet that grain size is 20-100 mesh; (3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment, wherein drying temperature is 70 DEG C, is dried The dry time is 5h;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, first heated up with 10 DEG C/min fast Degree is warming up to 400 DEG C, then is warming up to 650 DEG C with 1 DEG C/min heating rates, and keeps the temperature 30min;Last Temperature fall, obtains glass Glass microballon.
Embodiment 2
A kind of preparation method of glass microballoon, includes the following steps:
(1) ball milling:Add the raw material into ball milling 1 hour in ball-grinding machine;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight --- 50 parts of flyash, 40 parts of cullet are high 5 parts of ridge soil, 3 parts of perlite, 2 parts of yellow material is then added in granulator and is stirred granulation, and initial stage is first with 1500r/min Rotating speed stir 3min, rotating speed is promoted to 4500r/min and 13 parts of water is added by mid-term, stirs 8min, rotating speed drops in latter stage Down to 2000r/min, 2min is stirred;After stirring-granulating and filter out the pellet that grain size is 20-100 mesh;
(3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment, wherein drying temperature is 150 DEG C, drying time 1h;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, first heated up with 25 DEG C/min fast Degree is warming up to 600 DEG C, then is warming up to 850 DEG C with 8 DEG C/min heating rates, and keeps the temperature 10min;Last Temperature fall, obtains glass Glass microballon.
Embodiment 3
A kind of preparation method of glass microballoon, includes the following steps:
(1) ball milling:Add the raw material into ball milling 2 hours in ball-grinding machine;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight --- 30 parts of flyash, 55 parts of cullet are high 1 part of ridge soil, 5 parts of bentonite, 3 parts of miberal powder, 3 parts of perlite, 3 parts of green material are then added in granulator and are stirred granulation, Initial stage first stirs 2min with the rotating speed of 1200r/min, and rotating speed is promoted to 4000r/min and 17 parts of water is added by mid-term, stirring Rotating speed is reduced to 1500r/min by 6min, latter stage, stirs 1min;After stirring-granulating and grain size is filtered out as 20-100 mesh Pellet;
(3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment, wherein drying temperature is 120 DEG C, drying time 3h;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, first heated up with 15 DEG C/min fast Degree is warming up to 500 DEG C, then is warming up to 750 DEG C with 4 DEG C/min heating rates, and keeps the temperature 20min;Last Temperature fall, obtains glass Glass microballon.
Embodiment 4
A kind of preparation method of glass microballoon, includes the following steps:
(1) ball milling:Add the raw material into ball milling 2 hours in ball-grinding machine;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight --- 40 parts of flyash, 45 parts of cullet are high 2 parts of ridge soil, 3 parts of waterglass, 5 parts of miberal powder, 5 parts of blue is then added in granulator and is stirred granulations, initial stage elder generation with The rotating speed of 1000r/min stirs 2min, and rotating speed is promoted to 3500r/min and 15 parts of water is added by mid-term, stirs 5min, latter stage Rotating speed is reduced to 1800r/min, stirs 1min;After stirring-granulating and filter out the pellet that grain size is 20-100 mesh;
(3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment, wherein drying temperature is 100 DEG C, drying time 4h;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, first heated up with 20 DEG C/min fast Degree is warming up to 550 DEG C, then is warming up to 700 DEG C with 6 DEG C/min heating rates, and keeps the temperature 25min;Last Temperature fall, obtains glass Glass microballon.
The glass microballoon that embodiment 1-4 is prepared carries out sphericity test, test result is as follows table:
As seen from the above table, through the invention in the sphericity of glass microballoon that is prepared of method be all higher than 95%, and The sphericity of the glass microballoon of commercial type is about 80% at present, it can be seen that, through the invention in method be prepared into The more commercially available glass microballoon of glass microballoon arrived has higher sphericity, illustrates the glass microballoon being prepared closer to ball Shape.Since the mixing in preparation method of the present invention is carried out with granulation in granulator, initial stage is in low speed (rotating speed 750- The mixing and granulation of raw material are carried out under 1500r/min), mid-term is promoted to high speed (rotating speed 3000-4500r/min) and is granulated And addition water, solid close sphere is formed, the later stage carries out pellet surface under low speed (rotating speed 1000-2000r/min) Repairing, improves the sphericity of glass microballoon.
The glass microballoon that embodiment 1-4 is prepared carries out Mechanics Performance Testing, the glass microballoon sold more on the market Compression strength increase rate result such as following table:
Since the preparation method of the present invention uses non-slurry pelletizing, water content is low when raw material mixing granulation, and drying time is short, dries Pellet after dry has certain mechanical strength, non-breakable, convenient for sintering.Sintering process heating rate early period it is very fast (first with 10-25 DEG C/min heating rates are warming up to 400~600 DEG C), later stage high temperature section heating rate slows down (to be heated up with 1-8 DEG C/min again Speed is warming up to 650~850 DEG C), the extraneous temperature difference with pellet interior is advantageously reduced, the generation of defect is reduced.
Example the above is only the implementation of the present invention is not intended to limit the scope of the invention, every to utilize this hair Equivalent structure or equivalent flow shift made by bright description is applied directly or indirectly in other relevant technology necks Domain is included within the scope of the present invention.

Claims (10)

1. a kind of glass microballoon, which is characterized in that its raw material includes in parts by weight:75-90 parts of flyash and cullet, 5- 12 parts of binder, 3-8 parts of sintering aid, 2-5 parts of colorant.
2. glass microballoon according to claim 1, which is characterized in that the parts by weight of the flyash are 25-50 parts.
3. glass microballoon according to claim 1, which is characterized in that the binder is bentonite, kaolin, waterglass One or more of.
4. glass microballoon according to claim 1, which is characterized in that the sintering aid is one in miberal powder, perlite Kind or two kinds.
5. the preparation method of the glass microballoon described in any one of claim 1-4 claims, which is characterized in that including walking as follows Suddenly:
(1) ball milling:It adds the raw material into ball-grinding machine ball milling 1-3 hours;
(2) mixing granulation:Raw material after ball milling is weighed in parts by weight, be then added in granulator by initial stage, mid-term, Three stirring-granulating stages of latter stage, and water is added in the mid-term stirring-granulating stage, after stirring-granulating and filter out pellet;
(3) it dries:The pellet obtained in step (2) is subjected to drying and processing in drying equipment;
(4) it is sintered:Sintering processes will be passed through by the pellet after step (3) drying and processing, it is micro- to obtain glass for last Temperature fall Pearl.
6. the preparation method of glass microballoon according to claim 5, which is characterized in that initial stage stirs in the step (2) The rotating speed of granulation is 750-1500r/min, mixing time 1-3min;The rotating speed of mid-term stirring-granulating is 3000-4500r/ Min, mixing time 4-8min;The rotating speed of latter stage stirring-granulating is 1000-2000r/min, mixing time 0.5-2min.
7. the preparation method of glass microballoon according to claim 6, which is characterized in that mid-term stirs in the step (2) Pelletization stage amount of water is 13-20 parts.
8. the preparation method of glass microballoon according to claim 7, which is characterized in that filtered out in the step (2) The grain size of pellet is 20-100 mesh.
9. the preparation method of glass microballoon according to claim 5, which is characterized in that drying temperature in the step (3) It is 70-150 DEG C, drying time 1-5h.
10. the preparation method of glass microballoon according to claim 5, which is characterized in that sintering processes in the step (4) Process is:400~600 DEG C first are warming up to 10-25 DEG C/min heating rates, then 650 are warming up to 1-8 DEG C/min heating rates ~850 DEG C, and keep the temperature 10-30min.
CN201810476762.7A 2018-05-18 2018-05-18 Glass bead and preparation method thereof Active CN108395108B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115093122A (en) * 2022-07-15 2022-09-23 中钢集团马鞍山矿山研究总院股份有限公司 Preparation method of high-strength and low-density hollow glass microspheres

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4081259A (en) * 1976-09-23 1978-03-28 Maryland Environmental Service Method for forming coated cellular glass pellets
CN102910820A (en) * 2011-08-06 2013-02-06 闫井民 Flyash glass and preparation method thereof
CN105621891A (en) * 2015-12-30 2016-06-01 成都汇华英建筑材料有限公司 Vitrification foam glass particle and preparation method thereof
CN105800945A (en) * 2016-02-05 2016-07-27 北京大学 Foamed heat insulation material and preparation method thereof
EP2708517B1 (en) * 2012-09-13 2017-06-28 Binder + Co Aktiengesellschaft Method for the preparation of foamed glass
CN107555767A (en) * 2017-09-06 2018-01-09 安徽凯盛基础材料科技有限公司 The method that hollow glass micropearl is prepared using high-boron-silicon glass waste material

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4081259A (en) * 1976-09-23 1978-03-28 Maryland Environmental Service Method for forming coated cellular glass pellets
CN102910820A (en) * 2011-08-06 2013-02-06 闫井民 Flyash glass and preparation method thereof
EP2708517B1 (en) * 2012-09-13 2017-06-28 Binder + Co Aktiengesellschaft Method for the preparation of foamed glass
CN105621891A (en) * 2015-12-30 2016-06-01 成都汇华英建筑材料有限公司 Vitrification foam glass particle and preparation method thereof
CN105800945A (en) * 2016-02-05 2016-07-27 北京大学 Foamed heat insulation material and preparation method thereof
CN107555767A (en) * 2017-09-06 2018-01-09 安徽凯盛基础材料科技有限公司 The method that hollow glass micropearl is prepared using high-boron-silicon glass waste material

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115093122A (en) * 2022-07-15 2022-09-23 中钢集团马鞍山矿山研究总院股份有限公司 Preparation method of high-strength and low-density hollow glass microspheres

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