CN109437588A - A kind of preparation method of super-hydrophobic abrasion-resistance glass - Google Patents

A kind of preparation method of super-hydrophobic abrasion-resistance glass Download PDF

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Publication number
CN109437588A
CN109437588A CN201811287698.4A CN201811287698A CN109437588A CN 109437588 A CN109437588 A CN 109437588A CN 201811287698 A CN201811287698 A CN 201811287698A CN 109437588 A CN109437588 A CN 109437588A
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Prior art keywords
super
glass
5min
hydrophobic
impregnated
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CN201811287698.4A
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CN109437588B (en
Inventor
谷玉杰
吕剑
韩升
涂东怀
马辉
白彦波
王博
李凤仙
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Xian Modern Chemistry Research Institute
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Xian Modern Chemistry Research Institute
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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
    • C03C17/00Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/34Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
    • 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
    • C03C2217/00Coatings on glass
    • C03C2217/70Properties of coatings
    • C03C2217/78Coatings specially designed to be durable, e.g. scratch-resistant
    • 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
    • C03C2218/00Methods for coating glass
    • C03C2218/10Deposition methods
    • C03C2218/11Deposition methods from solutions or suspensions
    • C03C2218/111Deposition methods from solutions or suspensions by dipping, immersion

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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)
  • Surface Treatment Of Glass (AREA)
  • Glass Compositions (AREA)

Abstract

The invention discloses a kind of preparation methods of super-hydrophobic abrasion-resistance glass.The present invention comprises the following processes: (1) by glass mass percentage concentration be 1 ‰~2% Nano silica sol ethanol solution in impregnate 5min, in 300 DEG C~650 DEG C 1~5h of roasting, cleaning, drying;(2) containing 5min is impregnated in Nano diamond fluorine-containing organic silicon hydrophobing agent, 15 DEG C~100 DEG C are placed for 24 hours, and super-hydrophobic abrasion-resistance glass is obtained.Present invention is mainly used for a kind of preparations of super-hydrophobic abrasion-resistance glass.

Description

A kind of preparation method of super-hydrophobic abrasion-resistance glass
Technical field
The present invention relates to a kind of preparation methods of super-hydrophobic abrasion-resistance glass, belong to hydrophobic material preparation field.
Background technique
The free energy of the surface of solids is lower, and adhesive force is with regard to smaller, so that solid is bigger with Liquid contact angle.However, Even if the smooth surface with minimum surface energy, also there was only 119 ° to the contact angle of water.Contain long chain fluorine-containing group siloxanes It is the very low substance of a kind of surface free energy, is disclosed in US6395331 with long-chain fluorocarbons and fluorine carbon self assembly Monofilm is to the contact angle of water less than 120 °, and in the case where contact angle is less than 120 °, the surface of solids has hydrophobic ability, but water Or spot is easy in remained on surface, self-cleaning effect is poor.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiency of background technique and shortcoming, micro- knot is received in smooth surface building The rough surface of structure uses the hydrophobing agent of low-surface-energy to be surface modified again, obtains a kind of super-hydrophobic abrasion-resistance glass.
For the contact angle for improving smooth surface film, the present invention passes through the coarse table in smooth surface building nano-micro structure The contact angle of surface coating and water is improved in face.The present invention provides a kind of preparation method of super-hydrophobic abrasion-resistance glass, including it is as follows Step: (1) by glass mass percentage concentration be 1 ‰~5% Nano silica sol ethanol solution in impregnate 5min, 300 DEG C~650 DEG C of 1~5h of roasting, cleaning, drying;(2) containing impregnating 5min in Nano diamond fluorine-containing organic silicon hydrophobing agent, 15 DEG C~100 DEG C place for 24 hours, obtain super-hydrophobic abrasion-resistance glass.
The preparation method of the super-hydrophobic abrasion-resistance glass, it is characterised in that Nano silica sol is acidic silicasol or alkalinity Silica solution.
The preparation method of the super-hydrophobic abrasion-resistance glass, it is characterised in that Nano silica sol solid particle be 5~ 500nm。
The preparation method of the super-hydrophobic abrasion-resistance glass, it is characterised in that include the following steps: (1) by glass in quality 5min is impregnated in the ethanol solution for the Nano silica sol that percentage concentration is 1 ‰~3%, in 400 DEG C~600 DEG C 1~4h of roasting, clearly Wash drying;(2) containing 5min is impregnated in Nano diamond fluorine-containing organic silicon hydrophobing agent, 20 DEG C~80 DEG C are placed for 24 hours, are surpassed Hydrophobic abrasion-resistance glass.
Compared with prior art, beneficial effects of the present invention: constructing the rough surface of nano-micro structure by simple procedure, then It is modified using the hydrophobing agent of low-surface-energy, obtains super-hydrophobic glass contact angle up to 168.1 °.Furthermore the present invention is due to receiving The addition of rice diamond or derivatives thereof significantly improves its wearability, and wearability test is tested contact angle and reduced less than 6 °;This Kind method preparation obtains super-hydrophobic glass visible transmission ratio up to 90%.
Specific embodiment
Invention is further described in detail combined with specific embodiments below, but protection scope of the present invention is not limited to This.
Preparation containing Nano diamond fluorine-containing organic silicon hydrophobing agent: being stirred at room temperature down, and solvent C FC113a99.8g is added Enter in reaction flask, n-octadecane ethyl triethoxy silicane alkane 0.08g, (ten seven fluoro- 1,1,2,2- tetrahydro decyl) methyl dimethoxy is added The Nano diamond 0.06g that oxysilane hydrolysate 0.10g, n-hexadecyl triethoxysilane are modified, fluorochemical polyether (molecule Amount 2000~2800) 0.01g, continues to stir 0.5h after adding.
Contact angle test: contact angle instrument, Shanghai Zhongchen digital technology equipment Co., Ltd, JC2000D type, deionization 5 μ L of water.
Wearability test: straight line abrasion instrument, outing cloth, loading 9.8N/cm2,40 round-trip/min, round-trip distance 12 ± 2cm, round-trip 10000 times, contact angle is surveyed in test front and back.
Embodiment 1
(1) glass is impregnated into 5min in 1 ‰ acidity nanometer silica solution (5~100nm of solid particle), at 500 DEG C Roasting temperature 5h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 25 DEG C are placed for 24 hours, and initial contact angle is 168.1 °, 163.8 ° of contact angle after wearability test, it is seen that luminous transmittance 89%.
Comparative example 1
At room temperature, by test plate containing 5min is impregnated in Nano diamond fluorine-containing organic silicon hydrophobing agent, 25 DEG C are placed For 24 hours, initial contact angle is 119.0 °, 116.6 ° of contact angle after wearability test, it is seen that luminous transmittance 86%.
Embodiment 2
(1) glass is impregnated into 5min in 5 ‰ acidity nanometer silica solution (100~200nm of solid particle), at 400 DEG C Roasting temperature 4h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 35 DEG C are placed for 24 hours, and initial contact angle is 145.9 °, 140.2 ° of contact angle after wearability test, it is seen that luminous transmittance 90%.
Embodiment 3
(1) glass is impregnated into 5min in 1% acidity nanometer silica solution (400~500nm of solid particle), at 300 DEG C Roasting temperature 3h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 15 DEG C are placed for 24 hours, and initial contact angle is 125.7 °, 123.3 ° of contact angle after wearability test, it is seen that luminous transmittance 83%.
Embodiment 4
(1) glass is impregnated into 5min in 5% acidity nanometer silica solution (200~300nm of solid particle), at 600 DEG C Roasting temperature 2h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 50 DEG C are placed for 24 hours, and initial contact angle is 161.8 °, 156.4 ° of contact angle after wearability test, it is seen that luminous transmittance 86%.
Embodiment 5
(1) glass is impregnated into 5min in 5% alkaline nano silica solution (300~400nm of solid particle), at 650 DEG C Roasting temperature 1h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 75 DEG C are placed for 24 hours, and initial contact angle is 124.3 °, 118.6 ° of contact angle after wearability test, it is seen that luminous transmittance 80%.
Embodiment 6
(1) glass is impregnated into 5min in 2% alkaline nano silica solution (100~200nm of solid particle), at 550 DEG C Roasting temperature 3h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 25 DEG C are placed for 24 hours, and initial contact angle is 151.5 °, 146.8 ° of contact angle after wearability test, it is seen that luminous transmittance 84%.
Embodiment 7
(1) glass is impregnated into 5min in 1 ‰ alkaline nano silica solution (400~500nm of solid particle), at 500 DEG C Roasting temperature 4h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 30 DEG C are placed for 24 hours, and initial contact angle is 139.7 °, 135.6 ° of contact angle after wearability test, it is seen that luminous transmittance 88%.
Embodiment 8
(1) glass is impregnated into 5min in 5 ‰ acidity nanometer silica solution (5~100nm of solid particle), at 650 DEG C Roasting temperature 4h, cleaning, drying;
(2) at room temperature, (1) made test plate is impregnated in containing Nano diamond fluorine-containing organic silicon hydrophobing agent 5min, 30 DEG C are placed for 24 hours, and initial contact angle is 162.4 °, 157.8 ° of contact angle after wearability test, it is seen that luminous transmittance 90%.

Claims (4)

1. a kind of preparation method of super-hydrophobic abrasion-resistance glass, include the following steps: that glass is 1 ‰ in mass percentage concentration by (1) 5min is impregnated in the ethanol solution of~5% Nano silica sol, in 300 DEG C~650 DEG C 1~5h of roasting, cleaning, drying;(2) exist Containing 5min is impregnated in Nano diamond fluorine-containing organic silicon hydrophobing agent, 15 DEG C~100 DEG C are placed for 24 hours, obtain super-hydrophobic wear-resisting glass Glass.
2. the preparation method of super-hydrophobic abrasion-resistance glass according to claim 1, it is characterised in that Nano silica sol is acidity Silica solution or alkaline silica sol.
3. the preparation method of super-hydrophobic abrasion-resistance glass according to claim 1, it is characterised in that Nano silica sol solid Grain is 5~500nm.
4. the preparation method of super-hydrophobic abrasion-resistance glass according to claim 1, it is characterised in that include the following steps: (1) By glass mass percentage concentration be 1 ‰~3% Nano silica sol ethanol solution in impregnate 5min, at 400 DEG C~600 DEG C Roast 1~4h, cleaning, drying;(2) containing 5min is impregnated in Nano diamond fluorine-containing organic silicon hydrophobing agent, 20 DEG C~80 DEG C are put It sets for 24 hours, obtains super-hydrophobic abrasion-resistance glass.
CN201811287698.4A 2018-10-31 2018-10-31 Preparation method of super-hydrophobic wear-resistant glass Active CN109437588B (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102677132A (en) * 2012-05-28 2012-09-19 大连理工大学 Method for preparing super-hydrophobic coating of metallic matrix
CN104150785A (en) * 2014-07-29 2014-11-19 奇瑞汽车股份有限公司 Preparation method of hydrophobic glass
CN105419450A (en) * 2015-11-30 2016-03-23 东南大学 Highly-wear-resistant super-hydrophobic composite coating and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102677132A (en) * 2012-05-28 2012-09-19 大连理工大学 Method for preparing super-hydrophobic coating of metallic matrix
CN104150785A (en) * 2014-07-29 2014-11-19 奇瑞汽车股份有限公司 Preparation method of hydrophobic glass
CN105419450A (en) * 2015-11-30 2016-03-23 东南大学 Highly-wear-resistant super-hydrophobic composite coating and preparation method thereof

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