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CN111662017A - Preparation method of hydrophobic chemical group modified waterproof glass - Google Patents

Preparation method of hydrophobic chemical group modified waterproof glass Download PDF

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Publication number
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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China
Prior art keywords
glass
solution
preparation
resistance
reaction solution
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CN201910877397.5A
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Chinese (zh)
Inventor
李岩
赵佳婧
黄岩
刘明源
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Taizhou Polytechnic College
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Taizhou Polytechnic College
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Priority to CN201910877397.5A priority Critical patent/CN111662017A/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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments
    • C03C23/0095Solution impregnating; Solution doping; Molecular stuffing, e.g. of porous glass
    • 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
    • C03C23/00Other surface treatment of glass not in the form of fibres or filaments

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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)

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

Preparation method of hydrophobic chemical group modified waterproof glass
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.
CN201910877397.5A 2019-09-17 2019-09-17 Preparation method of hydrophobic chemical group modified waterproof glass Pending CN111662017A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
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

Patent Citations (5)

* Cited by examiner, † Cited by third party
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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Application publication date: 20200915

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