CN106746747A - A kind of preparation method of superhydrophobic hollow glass microballoon - Google Patents
A kind of preparation method of superhydrophobic hollow glass microballoon Download PDFInfo
- Publication number
- CN106746747A CN106746747A CN201611190278.5A CN201611190278A CN106746747A CN 106746747 A CN106746747 A CN 106746747A CN 201611190278 A CN201611190278 A CN 201611190278A CN 106746747 A CN106746747 A CN 106746747A
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- China
- Prior art keywords
- hollow glass
- preparation
- decorations
- glass microballoon
- acid
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
- C03C23/0075—Cleaning of glass
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C15/00—Surface treatment of glass, not in the form of fibres or filaments, by etching
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL 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
- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/28—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material
- C03C17/30—Surface treatment of glass, not in the form of fibres or filaments, by coating with organic material with silicon-containing compounds
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
- Glass Compositions (AREA)
Abstract
The present invention provides a kind of preparation method of superhydrophobic hollow glass microballoon, it is characterised in that it is comprised the following steps：Hollow glass micropearl is put into mixed solution and is washed, then drying carries out quarter decorations in placing into acid decorations liquid, finally prepares a layered low-surface energy material on hollow glass micropearl surface.The present invention is simple and convenient to operate with preparation, workable, it is easy to accomplish the advantages of commercial application.
Description
Technical field：
Specifically it is exactly a kind of preparation side of superhydrophobic hollow glass microballoon the present invention relates to super-hydrophobic class field of new
Method.
Background technology：
Hollow glass micropearl is a kind of widely used, excellent performance new material developed in recent years, the master of the product
It is borosilicate, the hollow ball that granularity is 10-250 microns, wall thickness is 1-2 microns to want composition.The product has light weight, low leads
The advantages of heat, intensity chemical stability high and good, is widely used in the composites such as fiberglass, artificial marble, artificial agate
In, mitigate weight and sound-insulating effect with obvious, enable product that there is good crack resistance and cycling processability.
The fields such as Aeronautics and Astronautics, novel high-speed train, luxury yacht, insulating moulding coating, bowling are used widely, and are served solely
Special good action.However, because bead surface has substantial amounts of hydroxyl bond, making its easy moisture absorption and luming, stream is had a strong impact on
Dynamic performance, so that influence it to apply the performance in every field, therefore, it is necessary to the hollow glass micropearl to producing is carried out
Super-hydrophobicization treatment.
According to hydrophobic mechanism, mode and effect to the surface-hydrophobicized treatment of hollow glass micropearl are also not quite similar.It is open
Number a kind of method modified to disclose hollow glass micropearl surface hydrophobicity in CN101284712A, uniformly coats in bead surface
Functional membrane and outer functional membrane in one layer, interior functional membrane is the organosilicon material with good combination power, and outer membrane is with hydrophobic
The organosilicon material of performance, it is compound to have obtained the hollow glass micropearl with general hydrophobic performance, super-hydrophobic performance is not reached,
The complex process, relatively costly simultaneously.The present invention will solve the defect that prior art is present, there is provided a kind of process is simple, cost
Low, superior performance the super-hydrophobic treatment technology of hollow glass micropearl.
The present invention provides following technical scheme：
A kind of preparation method of superhydrophobic hollow glass microballoon, it is characterised in that it is comprised the following steps：By hollow glass micropearl
It is put into the mixed solution being made up of ultra-pure water, ethanol, acetone and is washed；Then dried up with nitrogen；It is put into acid and adorns to enter in liquid
Row carves decorations；It is last to prepare a layered low-surface energy coating on hollow glass micropearl surface.
On the basis of above-mentioned technical proposal, there can also be technical scheme further below：
Ultra-pure water, ethanol, the content of acetone are 1 in described mixed solution：1：1.
Described washing is ultrasonic washing, and the time is 10 ~ 50 minutes.
Contain 10 ~ 50% fluosilicic acid, 0.5 ~ 2.3% silica, 0.3 ~ 1.5% boric acid, 46.2 in described acid decorations liquid
~ 89.2% aqueous solvent.
Described low surface energy coat is silicon fluoride class hydrophobic coating.
Invention advantage：
（1）Hollow glass micropearl after present invention treatment has superior hydrophobic performance, and water contact angle is more than 150 °, reaches super thin
Water effect；
（2）Low cost of the present invention, cost performance is high.The raw materials used wide material sources of the present invention, price is relatively low, and present invention process letter
It is single, it is workable, it is easy to accomplish commercial application.
Specific embodiment:
Embodiment 1：
First, it is 1 hollow glass micropearl to be put into by content：1：Enter in the mixed solution that 1 ultra-pure water, ethanol, acetone are made
Row ultrasonic washing 30 minutes, to remove the impurity and pollutant on hollow glass micropearl surface.Then dried up with nitrogen hollow
Glass microballoon.
Then, then by hollow glass micropearl fluosilicic acid, 1.5% silica, 0.7% boron that mass fraction is 28% are put into
Adoring at the quarter that acid, 69% aqueous solvent are made carries out sour decorations in liquid, acid 52 DEG C of temperature of decorations, 26 minutes sour decorations time.By carving decorations liquid
Acid decorations, by eroding for the selectivity such as the sodium oxide molybdena of bead surface, calcium oxide, retain silica skeleton, form surface crater micro-
Structure, increases its specific surface area.
The hollow glass micropearl surface for having surface micro-structure after acid decorations is finally coated with one layer of ten ethoxy of trifluoro octyl group three
The low surface energy coat of base silane.So as to remove the hydrophilic hydroxyl groups on hollow glass micropearl surface, one layer of fluorine silicon is formed on its surface
The hydrophobic coating of alkanes.
After testing, the hollow glass micropearl water contact angle of preparation is 156 °, reaches super-hydrophobic effect.
Embodiment 2：
First, it is 1 hollow glass micropearl to be put into by content：1：Enter in the mixed solution that 1 ultra-pure water, ethanol, acetone are made
Row ultrasonic washing 10 minutes, to remove the impurity and pollutant on hollow glass micropearl surface.Then dried up with nitrogen hollow
Glass microballoon.
Then, then by hollow glass micropearl fluosilicic acid, 0.5% silica, 0.3% boron that mass fraction is 11% are put into
Adoring at the quarter of sour, 88.2% aqueous solvent carries out sour decorations in liquid, acid 41 DEG C of temperature of decorations, 35 minutes sour decorations time.By the acid for carving decorations liquid
Decorations, by eroding for the selectivity such as the sodium oxide molybdena of bead surface, calcium oxide, retain silica skeleton, form the micro- knot of surface crater
Structure, increases its specific surface area.
The hollow glass micropearl surface for having surface micro-structure after acid decorations is finally coated with one layer of 17 fluorine decyl triethoxysilicane
The low surface energy coat of alkane.So as to remove the hydrophilic hydroxyl groups on hollow glass micropearl surface, one layer of silicon fluoride class is formed on its surface
Hydrophobic coating.
After testing, the hollow glass micropearl water contact angle of preparation is 161 °, reaches super-hydrophobic effect.
Embodiment 3：
First, it is 1 hollow glass micropearl to be put into by content：1：Enter in the mixed solution that 1 ultra-pure water, ethanol, acetone are made
Row ultrasonic washing 49 minutes, to remove the impurity and pollutant on hollow glass micropearl surface.Then dried up with nitrogen hollow
Glass microballoon.
Then, then by hollow glass micropearl fluosilicic acid, 2.3% silica, 1.5% boron that mass fraction is 49% are put into
Adoring at the quarter of sour, 47.2% aqueous solvent carries out sour decorations in liquid, acid decorations temperature 70 C, 10 minutes sour decorations time.By the acid for carving decorations liquid
Decorations, by eroding for the selectivity such as the sodium oxide molybdena of bead surface, calcium oxide, retain silica skeleton, form the micro- knot of surface crater
Structure, increases its specific surface area.
The hollow glass micropearl surface for having surface micro-structure after acid decorations is finally coated with one layer of perfluoro hexyl trichlorosilane.
So as to remove the hydrophilic hydroxyl groups on hollow glass micropearl surface, one layer of hydrophobic coating of silicon fluoride class is formed on its surface.
After testing, the hollow glass micropearl water contact angle of preparation is 153 °, reaches super-hydrophobic effect.
The above, is only presently preferred embodiments of the present invention, and any formal limitation is not made to the present invention；Appoint
What those of ordinary skill in the art, in the case where technical solution of the present invention ambit is not departed from, all using the side of the disclosure above
Method and technology contents make many possible variations and modification, or the equivalent reality for being revised as equivalent variations to technical solution of the present invention
Apply example.Therefore, every content without departing from technical solution of the present invention, is done according to technical spirit of the invention to above example
Any simple modification, equivalent, equivalence changes and modification, still fall within the range of technical solution of the present invention protection.
Claims (5)
1. a kind of preparation method of superhydrophobic hollow glass microballoon, it is characterised in that it is comprised the following steps：Hollow glass is micro-
Pearl is washed in being put into the mixed solution being made up of ultra-pure water, ethanol, acetone；Then dried up with nitrogen；It is put into acid decorations liquid
Carry out quarter decorations；It is last to prepare a layered low-surface energy coating on hollow glass micropearl surface.
2. the preparation method of a kind of superhydrophobic hollow glass microballoon according to claim 1, it is characterised in that it includes
Following steps：Ultra-pure water, ethanol, the content of acetone are 1 in described mixed solution：1：1.
3. the preparation method of a kind of superhydrophobic hollow glass microballoon according to claim 1, it is characterised in that it includes
Following steps：Described washing is ultrasonic washing, and the time is 10 ~ 50 minutes.
4. the preparation method of a kind of superhydrophobic hollow glass microballoon according to claim 1, it is characterised in that it includes
Following steps：In described acid decorations liquid containing 10 ~ 50% fluosilicic acid, 0.5 ~ 2.3% silica, 0.3 ~ 1.5% boric acid,
46.2 ~ 89.2% aqueous solvent.
5. the preparation method of a kind of superhydrophobic hollow glass microballoon according to claim 1, it is characterised in that it includes
Following steps：Described low surface energy coat is silicon fluoride class hydrophobic coating.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190278.5A CN106746747A (en) | 2016-12-21 | 2016-12-21 | A kind of preparation method of superhydrophobic hollow glass microballoon |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190278.5A CN106746747A (en) | 2016-12-21 | 2016-12-21 | A kind of preparation method of superhydrophobic hollow glass microballoon |
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| CN106746747A true CN106746747A (en) | 2017-05-31 |
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| CN201611190278.5A Pending CN106746747A (en) | 2016-12-21 | 2016-12-21 | A kind of preparation method of superhydrophobic hollow glass microballoon |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107235639A (en) * | 2017-07-18 | 2017-10-10 | 合肥鼎亮光学科技有限公司 | A kind of preparation method of hydrophobicity reflective glass beads |
| CN107382086A (en) * | 2017-09-06 | 2017-11-24 | 安徽凯盛基础材料科技有限公司 | Hollow glass micropearl surface reinforcing method and surface peening hollow glass micropearl |
| CN107555808A (en) * | 2017-09-06 | 2018-01-09 | 安徽凯盛基础材料科技有限公司 | A kind of method of hollow glass micropearl surface hydrophobic processing |
| CN115584189A (en) * | 2022-09-16 | 2023-01-10 | 国家能源集团新能源技术研究院有限公司 | Super-hydrophobic glass bead and preparation method thereof, and super-hydrophobic coating and preparation method thereof |
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| CN102219391A (en) * | 2011-03-28 | 2011-10-19 | 华南理工大学 | Method for forming super-hydrophobic coating on glass matrix |
| CN102674697A (en) * | 2011-03-18 | 2012-09-19 | 北京市太阳能研究所有限公司 | Method for preparing minus reflection antireflection glass through etching |
| CN102950099A (en) * | 2011-08-21 | 2013-03-06 | 比亚迪股份有限公司 | Super-hydrophobic material and preparation method thereof |
| CN104130597A (en) * | 2014-07-08 | 2014-11-05 | 上海海事大学 | Hollow glass micro-spheres surface modification method |
| CN106009791A (en) * | 2016-05-16 | 2016-10-12 | 东南大学 | Super-hydrophilic particle hybridized super-hydrophobic coating and preparation method thereof |
-
2016
- 2016-12-21 CN CN201611190278.5A patent/CN106746747A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102674697A (en) * | 2011-03-18 | 2012-09-19 | 北京市太阳能研究所有限公司 | Method for preparing minus reflection antireflection glass through etching |
| CN102219391A (en) * | 2011-03-28 | 2011-10-19 | 华南理工大学 | Method for forming super-hydrophobic coating on glass matrix |
| CN102950099A (en) * | 2011-08-21 | 2013-03-06 | 比亚迪股份有限公司 | Super-hydrophobic material and preparation method thereof |
| CN104130597A (en) * | 2014-07-08 | 2014-11-05 | 上海海事大学 | Hollow glass micro-spheres surface modification method |
| CN106009791A (en) * | 2016-05-16 | 2016-10-12 | 东南大学 | Super-hydrophilic particle hybridized super-hydrophobic coating and preparation method thereof |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107235639A (en) * | 2017-07-18 | 2017-10-10 | 合肥鼎亮光学科技有限公司 | A kind of preparation method of hydrophobicity reflective glass beads |
| CN107382086A (en) * | 2017-09-06 | 2017-11-24 | 安徽凯盛基础材料科技有限公司 | Hollow glass micropearl surface reinforcing method and surface peening hollow glass micropearl |
| CN107555808A (en) * | 2017-09-06 | 2018-01-09 | 安徽凯盛基础材料科技有限公司 | A kind of method of hollow glass micropearl surface hydrophobic processing |
| CN115584189A (en) * | 2022-09-16 | 2023-01-10 | 国家能源集团新能源技术研究院有限公司 | Super-hydrophobic glass bead and preparation method thereof, and super-hydrophobic coating and preparation method thereof |
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| CB02 | Change of applicant information |
Address after: 751 No. 233010 Anhui province Bengbu Longzihu East Avenue Applicant after: Anhui Kasen basic Mstar Technology Ltd Applicant after: Bengbu design Institute of Glass Industry Address before: Tu Shan Lu Yuhui District 233010 Anhui city of Bengbu Province, No. 1047 Applicant before: Anhui Kasen basic Mstar Technology Ltd Applicant before: Bengbu design Institute of Glass Industry |
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Application publication date: 20170531 |
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| RJ01 | Rejection of invention patent application after publication |