CN111662017A - Preparation method of hydrophobic chemical group modified waterproof glass - Google Patents
Preparation method of hydrophobic chemical group modified waterproof glass Download PDFInfo
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- CN111662017A CN111662017A CN201910877397.5A CN201910877397A CN111662017A CN 111662017 A CN111662017 A CN 111662017A CN 201910877397 A CN201910877397 A CN 201910877397A CN 111662017 A CN111662017 A CN 111662017A
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- 239000011521 glass Substances 0.000 title claims abstract description 74
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 13
- 125000003636 chemical group Chemical group 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 43
- 238000004140 cleaning Methods 0.000 claims abstract description 22
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000006557 surface reaction Methods 0.000 claims abstract description 13
- 239000010410 layer Substances 0.000 claims abstract description 9
- GZGREZWGCWVAEE-UHFFFAOYSA-N chloro-dimethyl-octadecylsilane Chemical compound CCCCCCCCCCCCCCCCCC[Si](C)(C)Cl GZGREZWGCWVAEE-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000002052 molecular layer Substances 0.000 claims abstract description 6
- 239000002356 single layer Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 5
- 230000001590 oxidative effect Effects 0.000 claims abstract description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000008367 deionised water Substances 0.000 claims description 15
- 229910021641 deionized water Inorganic materials 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 15
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 229910052757 nitrogen Inorganic materials 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- AZUXXYCNTKYZJB-UHFFFAOYSA-N chloro(octadecyl)silane Chemical compound CCCCCCCCCCCCCCCCCC[SiH2]Cl AZUXXYCNTKYZJB-UHFFFAOYSA-N 0.000 claims description 2
- 239000000443 aerosol Substances 0.000 claims 2
- 230000005661 hydrophobic surface Effects 0.000 abstract description 4
- 230000003068 static effect Effects 0.000 abstract description 3
- 230000007797 corrosion Effects 0.000 abstract description 2
- 238000005260 corrosion Methods 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 230000003647 oxidation Effects 0.000 abstract description 2
- 238000007254 oxidation reaction Methods 0.000 abstract description 2
- 230000002265 prevention Effects 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 description 6
- 239000003795 chemical substances by application Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000001514 detection method Methods 0.000 description 3
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 3
- 230000003075 superhydrophobic effect Effects 0.000 description 3
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 description 1
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000009120 camo Nutrition 0.000 description 1
- 235000005607 chanvre indien Nutrition 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000011487 hemp Substances 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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Classifications
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- 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
- C03C23/0095—Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous 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
- C03C23/00—Other surface treatment of glass not in the form of fibres or filaments
Landscapes
- 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)
- Surface Treatment Of Glass (AREA)
Abstract
The invention relates to a preparation method of hydrophobic chemical group modified waterproof glass, which comprises the following steps: (1) preparation of a Pirahan solution: by means of H2O2And concentrated H2SO4Preparing a strong oxidizing Pirahan solution; (2) CH (CH)3Preparation of monolayer surface reaction solution: preparing CH by using dimethyl octadecyl chlorosilane and n-hexane solution3A monomolecular layer surface reaction solution; (3) preparation of self-assembled molecular layer: clean glass is sequentially dipped in the solution to prepare the glass with rich CH on the surface3The glass surface of (1). The advantages are that: 1) the static water contact angle of the glass surface is improved from 45 degrees to 110 degrees, and a strong hydrophobic surface is formed, so that the glass surface has the remarkable advantages of water resistance, fog resistance, snow resistance, pollution resistance, adhesion resistance, oxidation resistance, corrosion resistance, self-cleaning, current conduction prevention and the like. 2) The method has the advantages of simple experimental steps, simple and convenient operation, high efficiency, good application value and wide application space, and has extremely wide application prospect in scientific research, production, life and other fields.
Description
Technical Field
The invention relates to a preparation method of hydrophobic chemical group modified waterproof glass, belonging to the technical field of engineering materials.
Background
Waterproof glass is common in the market, but some problems still exist in the actual use process, firstly, a hydrophobic rainproof agent is prepared by coating a hydrophobic high polymer material on the surface of glass to form a high polymer coating, the water drops slide downwards by the aid of the self weight of the water drops to achieve a waterproof effect, but the water drops cannot slide off very small time, so that dense and hemp water drops are formed on the glass, the definition of the glass is reduced, and the glass is poor in stability and needs to be maintained repeatedly; secondly, the hydrophilic waterproof agent is easy to cause surface image deformation and influence the use effect due to the fact that a local water film is uneven; thirdly, the super-hydrophobic waterproof agent is composed of nano particles and high polymer materials, glass treated by the super-hydrophobic waterproof agent has high efficiency of water drop gliding and dropping, and can play a dustproof effect, but the surface firmness of the super-hydrophobic waterproof agent is not enough, the super-waterproof performance is lost by wiping with hands or a towel, the waterproof effect has timeliness, and the price is relatively high.
Disclosure of Invention
The invention provides a preparation method of hydrophobic chemical group modified waterproof glass, aiming at overcoming the defects of the existing waterproof glass, and introducing a strong hydrophobic chemical group-methyl (-CH 3) on the surface of a glass mirror by utilizing a material surface modification technology to prepare the glass mirror with a strong hydrophobic surface, so that the glass mirror has a good waterproof effect.
The technical solution of the invention is as follows: a preparation method of hydrophobic chemical group modified waterproof glass comprises the following steps:
(1) preparation of a Pirahan solution: measuring 700 ml of 30% H2O2Pouring into a clean beaker, standing the beaker in an ice bath environment, and measuring 300 ml of 98% H2SO4Slowly adding H2O2In solution, and continuously slowly stirred with a glass rod.
(2)CH3Preparation of monolayer surface reaction solution: 5 ml of dimethyloctadecylchlorosilane is dissolved in 500 ml of n-hexane solution to prepare a reaction solution with the volume ratio of 5%.
(3) Preparation of self-assembled molecular layer:
1) fully cleaning the glass with acetone, absolute ethyl alcohol and deionized water in sequence, and cleaning and drying each liquid in an ultrasonic cleaning machine to obtain blank and clean glass;
2) immersing the dried blank clean glass into a prepared Pirahan solution, treating for 55-65min under the condition of 75-85 ℃ water bath, taking out the glass, fully cleaning with deionized water, and drying with high-purity nitrogen to obtain OH surface glass;
3) and immersing the obtained OH surface glass into the reaction solution on the surface of the CH3 monomolecular layer one by one, reacting for 50-70h in a water bath at 50-60 ℃, fully cleaning with absolute ethyl alcohol and deionized water in sequence, and drying with high-purity nitrogen to obtain the CH3 surface waterproof glass.
The main reaction principle is as follows: in strongly oxidizing Pirahan solution (concentrated H)2SO4∶H2O2Volume ratio = 7: 3), the glass surface undergoes extreme hydroxylation to form a hydroxylated monomolecular film, on the basis of which the terminal group is CH3The octadecylchlorosilane is subjected to further self-assembly condensation reaction to form the product with the surface rich in CH3The glass mirror surface of (1).
The invention has the beneficial effects that:
1) the static water contact angle of the glass surface is improved from 45 degrees to 110 degrees, and a strong hydrophobic surface is formed, so that the glass surface has the remarkable advantages of water resistance, fog resistance, snow resistance, pollution resistance, adhesion resistance, oxidation resistance, corrosion resistance, self-cleaning, current conduction prevention and the like.
2) The method has the advantages of simple experimental steps, simple and convenient operation, high efficiency, good application value and wide application space, and has extremely wide application prospect in scientific research, production, life and other fields.
Drawings
FIG. 1 is CH3Full spectrum XPS detection of the surface.
FIG. 2 is CH3C spectrum XPS detection spectrum of the surface.
FIG. 3 is a photograph of the water contact angle of the glass surface.
Detailed Description
The technical scheme of the invention is further explained by combining the attached drawings
1. Preparation of reaction solution for related experiments
① Pirahan solution, measuring 700 ml of 30% H2O2Pouring into a clean beaker, and standing the beaker in an ice bath environment; 300 ml of 98% H is measured2SO4. Carefully add it slowly to H above2O2In the solution, continuously and slowly stirring by a glass rod;
surface reaction solution of CH3 monomolecular layer: 5 ml of dimethyloctadecylchlorosilane is dissolved in 500 ml of n-hexane solution to prepare a reaction solution with the volume ratio of 5%, and the reaction solution is placed in a ventilation kitchen for later use.
2. Preparation of self-assembled molecular layers
Fully cleaning glass with acetone, absolute ethyl alcohol and deionized water in sequence, cleaning each liquid in an ultrasonic cleaning machine for three times, and drying to obtain blank and clean glass;
immersing the dried blank clean glass into a prepared Pirahan solution, treating for 1 h under the condition of 80 ℃ water bath, taking out the glass, fully cleaning with deionized water, and drying with high-purity nitrogen to obtain OH surface glass;
③ the OH surface obtained was immersed in CH one by one3Reacting the surface reaction solution of the monomolecular layer for 1 hour under the water bath condition of 55 ℃, fully cleaning with absolute ethyl alcohol and deionized water in sequence, and drying with high-purity nitrogen to obtain CH3Surface slide;
as shown in attached figures 1 and 2, is CH3Full spectrum and C spectrum XPS detection spectra of the surface show that the surface of the glass mirror surface is successfully accessed with-CH3Radical density of 92%.
As shown in FIG. 3, which is a photograph of the water contact angle of the glass surface, the static water contact angle of the prepared water-repellent glass mirror surface is increased from 45 degrees to 110 degrees, which proves that a strong hydrophobic surface is formed.
Example 1
A preparation method of hydrophobic chemical group modified waterproof glass is characterized by comprising the following steps:
(1) preparation of a Pirahan solution: measuring and measuring700 ml 30% H2O2Pouring into a clean beaker, standing the beaker in an ice bath environment, and measuring 300 ml of 98% H2SO4Slowly adding H2O2In solution, and continuously slowly stirred with a glass rod.
(2)CH3Preparation of monolayer surface reaction solution: 5 ml of dimethyloctadecylchlorosilane is dissolved in 500 ml of n-hexane solution to prepare a reaction solution with the volume ratio of 5%.
(3) Preparation of self-assembled molecular layer:
1) fully cleaning the glass with acetone, absolute ethyl alcohol and deionized water in sequence, and cleaning and drying each liquid in an ultrasonic cleaning machine to obtain blank and clean glass;
2) immersing the dried blank clean glass into a prepared Pirahan solution, treating for 1 h under the condition of 80 ℃ water bath, taking out the glass, fully cleaning with deionized water, and drying with high-purity nitrogen to obtain OH surface glass;
3) the OH surface glass obtained is dipped in CH piece by piece3Reacting the surface reaction solution of the monomolecular layer for 1 hour under the water bath condition of 55 ℃, fully cleaning with absolute ethyl alcohol and deionized water in sequence, and drying with high-purity nitrogen to obtain CH3The surface is waterproof glass.
Example 2
A preparation method of hydrophobic chemical group modified waterproof glass is characterized by comprising the following steps:
(1) preparation of a Pirahan solution: measuring 700 ml of 30% H2O2Pouring into a clean beaker, standing the beaker in an ice bath environment, and measuring 300 ml of 98% H2SO4Slowly adding H2O2In solution, and continuously slowly stirred with a glass rod.
(2)CH3Preparation of monolayer surface reaction solution: 5 ml of dimethyloctadecylchlorosilane is dissolved in 500 ml of n-hexane solution to prepare a reaction solution with the volume ratio of 5%.
(3) Preparation of self-assembled molecular layer:
1) fully cleaning the glass with acetone, absolute ethyl alcohol and deionized water in sequence, and cleaning and drying each liquid in an ultrasonic cleaning machine to obtain blank and clean glass;
2) immersing the dried blank clean glass into a prepared Pirahan solution, treating for 55min under the condition of 82 ℃ water bath, taking out the glass, fully cleaning with deionized water, and drying with high-purity nitrogen to obtain OH surface glass;
3) the OH surface glass obtained is dipped in CH piece by piece3Reacting the surface reaction solution of the monomolecular layer for 65min under the condition of water bath at 53 ℃, fully cleaning with absolute ethyl alcohol and deionized water in sequence, and drying with high-purity nitrogen to obtain CH3The surface is waterproof glass.
Claims (4)
1. A preparation method of hydrophobic chemical group modified waterproof glass is characterized by comprising the following steps:
(1) preparation of a Pirahan solution: by means of H2O2And concentrated H2SO4Preparing a strong oxidizing Pirahan solution;
(2)CH3preparation of monolayer surface reaction solution: preparing CH by using dimethyl octadecyl chlorosilane and n-hexane solution3A monomolecular layer surface reaction solution;
(3) preparation of self-assembled molecular layer: clean glass is sequentially dipped in the solution to prepare the glass with rich CH on the surface3The glass surface of (1).
2. The method for preparing hydrophobic chemical group modified water-proof glass according to claim 1, wherein the step (1) of preparing the Pirahan solution comprises the following steps: measuring 700 ml of 30% H2O2Pouring into a clean beaker, standing the beaker in an ice bath environment, and measuring 300 ml of 98% H2SO4Slowly adding H2O2In solution, and continuously slowly stirred with a glass rod.
3. The automatic dispensing device for medicinal metered dose aerosol according to claim 1, wherein said step (2) CH3Preparation of monolayer surface reaction solution: taking 5 ml of dimethylDissolving octadecylchlorosilane in 500 ml of n-hexane solution to prepare a reaction solution with the volume ratio of 5%.
4. The automatic dispensing device of medicinal metered dose aerosol as claimed in claim 1, wherein the step (3) of preparing the self-assembled molecular layer comprises the following process steps:
1) fully cleaning the glass with acetone, absolute ethyl alcohol and deionized water in sequence, and cleaning and drying each liquid in an ultrasonic cleaning machine to obtain blank and clean glass;
2) immersing the dried blank clean glass into a prepared Pirahan solution, treating for 55-65min under the condition of 75-85 ℃ water bath, taking out the glass, fully cleaning with deionized water, and drying with high-purity nitrogen to obtain OH surface glass;
3) the OH surface glass obtained is dipped in CH piece by piece3Reacting the surface reaction solution of the monomolecular layer for 50-70h in a water bath at 50-60 ℃, fully cleaning with absolute ethyl alcohol and deionized water in sequence, and drying with high-purity nitrogen to obtain CH3The surface is waterproof glass.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910877397.5A CN111662017A (en) | 2019-09-17 | 2019-09-17 | Preparation method of hydrophobic chemical group modified waterproof glass |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910877397.5A CN111662017A (en) | 2019-09-17 | 2019-09-17 | Preparation method of hydrophobic chemical group modified waterproof glass |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2752834A1 (en) * | 1996-08-30 | 1998-03-06 | Corning Inc | Hydrophobic surface treatment of siliceous material |
| CN1275927A (en) * | 1997-08-14 | 2000-12-06 | 丹尼尔·萨梅因 | Solid material treatment methods for rendering solid materials hydrophobic, resulting materials and applications |
| CN104176944A (en) * | 2014-09-05 | 2014-12-03 | 北京航空航天大学 | Method for modifying OTS self-assembled film on glass substrate |
| CN104276765A (en) * | 2013-07-08 | 2015-01-14 | 重庆绿色智能技术研究院 | Preparation method of super-hydrophobic transparent glass |
| CN106495498A (en) * | 2016-10-11 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of glass antifogging coating |
-
2019
- 2019-09-17 CN CN201910877397.5A patent/CN111662017A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2752834A1 (en) * | 1996-08-30 | 1998-03-06 | Corning Inc | Hydrophobic surface treatment of siliceous material |
| CN1275927A (en) * | 1997-08-14 | 2000-12-06 | 丹尼尔·萨梅因 | Solid material treatment methods for rendering solid materials hydrophobic, resulting materials and applications |
| CN104276765A (en) * | 2013-07-08 | 2015-01-14 | 重庆绿色智能技术研究院 | Preparation method of super-hydrophobic transparent glass |
| CN104176944A (en) * | 2014-09-05 | 2014-12-03 | 北京航空航天大学 | Method for modifying OTS self-assembled film on glass substrate |
| CN106495498A (en) * | 2016-10-11 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of glass antifogging coating |
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