CN106675119A - Preparation method of automotive glass antifogging agent - Google Patents

Preparation method of automotive glass antifogging agent Download PDF

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Publication number
CN106675119A
CN106675119A CN201611157307.8A CN201611157307A CN106675119A CN 106675119 A CN106675119 A CN 106675119A CN 201611157307 A CN201611157307 A CN 201611157307A CN 106675119 A CN106675119 A CN 106675119A
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agent
preparation
wind
screen
initiator
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蒋建华
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1606—Antifouling paints; Underwater paints characterised by the anti-fouling agent
    • C09D5/1612—Non-macromolecular compounds
    • C09D5/1618—Non-macromolecular compounds inorganic
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16—Antifouling paints; Underwater paints
    • C09D5/1687—Use of special additives

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Surface Treatment Of Glass (AREA)
  • Application Of Or Painting With Fluid Materials (AREA)

Abstract

The invention relates to a preparation method of an automotive glass antifogging agent. The automotive glass antifogging agent comprises the following raw materials in percentage by mass: 50-99% of nano titanium dioxide hydrosol, 0.02-40% of lignin coupling agent, 0.001-30% of surfactant, 0.01-5% of initiator, 0.001-2% of dispersing agent, 0-10% of compatilizer and 0-10% of acid regulator. The preparation method comprises the following steps: stirring and mixing the nano titanium dioxide hydrosol, lignin coupling agent, initiator and dispersing agent, and sufficiently reacting; then adding a mixture of the surfactant and compatilizer, and stirring for 0.5-4 hours; and regulating the pH value with the pH regulator to obtain the nano antifogging agent having the pH value of 8-10. The antifogging agent has favorable antifogging effect; the addition of the lignin coupling agent and initiator realizes firm bonding and achieves a long-lasting effect; and meanwhile, the antifogging agent is simple in process, low in cost and convenient to use.

Description

A kind of preparation method of anti-fog agent for wind-screen of automobile
Technical field
The present invention relates to a kind of for cleaning, the liquid of anti-fog function and preparation method thereof, and in particular to Yi Zhonghan There is the preparation method of the anti-fog agent for wind-screen of automobile of nano titanium oxide.
Background technology
The pollution of vehicle glass and atomization, bring many inconvenience, remove depollution, prevent the method being atomized from having many Kind, and antifoggant is a kind of method of relatively inexpensive material benefit, and energy consumption is low, and application prospect is very wide.
The ultimate principle of antifoggant is, with surfactant as main component, in substrate material surface one layer of hydrophilic film to be formed To prevent mist pearl from producing, the transmitance of light is kept.
At present the manufacture method of antifoggant has plenty of and directly surfactant is coated onto on matrix, and is more in matrix Upper coating polymeric membrane, it includes that esters of acrylic acid anti-fog coating, organopolysiloxane antifoggant, polyoxyethylene polyols class are antifog Agent etc., such as United States Patent (USP) US3212909 disclose a kind of antifoggant with Laurel sulfo group acid sodium as main component；United States Patent (USP) US5244935 disclose it is a kind of can be with antifog amine polymer preparation method Jing after ultra-violet curing；European patent EP 5244935 is disclosed It is a kind of to realize antifog method with hydroxy polymer activating agent is included；But, the antifog composition in said method lacks with matrix material Weary effective interaction, causes antifog effect duration short.Chinese patent CN03117059.5 introduces nanometer two in antifoggant Titanium oxide（TiO2）Particle, the photocatalytic activity in titanium dioxide can degrade the surface active ingredient in antifoggant, thus also be unfavorable for Improve the stability and persistency of antifoggant.Chinese patent 200810099062.7 discloses one kind with acidic nano-sized silica and four Alkoxy silane Si（OR）4 is component for improving hydrophilic silica dioxide coating preparation method, and the coating system is under acidity Anti-fog feature is just shown, simultaneously because slightly stronger acid promotes the hydrolytic-polymeric reaction of siloxanes key to accelerate, nanometer titanium dioxide silicon grain It is sub to be easy to reunite in the network structure for having gel to be inclined to for being formed, so as to cause stability to reduce, particularly four alkoxyl silicones Alkane is hydrolyzed under acid catalysiss, forms the silicon-oxygen polymer of chain branch, and chain silicon-oxygen polymer has with the interaction of matrix material Limit, and disappearance of the surface group on chain causes polymer lacking toughness and becomes fragile so that and the antifog effect duration of coating is short.
The content of the invention
In order to overcome the deficiencies in the prior art, the invention provides one kind vehicle glass surface energy self-cleaning, while The preparation method of the antifoggant containing nano-titania particle with anti-fog function.
For achieving the above object, the technical solution used in the present invention is：
A kind of preparation method of anti-fog agent for wind-screen of automobile, comprises the following steps：
（1）Following each component is weighed by following mass percent：
Nanometer Titanium Dioxide Hydrosol 50~99%
Lignin coupling agent 0.02~40%
Surfactant 0.001~30%
Initiator 0.01~5%
Dispersant 0.001~2%
Phase solvent 0~10%
PH regulators 0~10%；
（2）By Nanometer Titanium Dioxide Hydrosol, lignin coupling agent, initiator and dispersant stirring mixing 1 ~ 24 hour；
（3）Treat step（2）Surfactant is added to stir 0.5 ~ 4 hour with the mixture of phase solvent after reaction fully, with PH tune Section agent adjusts the nanometer anti-fog agent that pH is obtained pH 8~10.
The Nanometer Titanium Dioxide Hydrosol pH is 9~10.5, and contained TiO 2 particles size is 15~30 nanometers.
The surfactant is high fatty alcohol sulfuric acid ester, aliphatic sulfonic class, amino acidses, polyalcohols, fat Fatty alcohol class, fatty acid glycerine esters, the combination of one or more of lecithin apoplexy due to endogenous wind.
The initiator is the combination of one or more in benzyl dimethylamine, triethanolamine, tetrabutyl ammonium bromide.
The dispersant is the combination of one or more in sodium tripolyphosphate, sodium hexameta phosphate, triethyl group hexyl phosphoric acid.
The phase solvent is one or two the combination in isopropanol, ethylene glycol.
The PH regulators are the diluted acids such as dilute hydrochloric acid, spirit of vinegar, dust technology or the one or more combination in aminoacid.
After above-mentioned technical proposal, the beneficial effect that the present invention reaches is：
（1）Nano titanium oxide TiO2There is under light illumination Superhydrophilic and super permanent, even if the moisture or water in air Devaporation, condensed water will not also form single water droplet, but form moisture film and equably spread over surface, so surface will not be sent out The mist of third contact of a total solar or lunar eclipse scattering, when rain is broken through, also can spread rapidly in the rainwater of surface attachment becomes uniform moisture film, thus not The water droplet of dispersion sight line can be formed so that rearview mirror surface keeps original light, the safety of driving be improved, while using oxygen Change the light-catalyzed reaction of titanium just can be decomposed into CO the organic pollution adsorbed in titania surface2And O2, with remaining inorganic Thing together can be clean by rain drop erosion, so as to realize self-cleaning function.
（2）Using lignin coupling agent, and it is used in conjunction with phase solvent, strengthens the company of nano-particle and matrix material Connect, in substrate material surface the framing structure of porous is formed, increase surface energy, the strength and stability of coating is improved, while right TiO 2 particles are produced and are modified, and at utmost reduce the interaction between nano-titania particle, make nanometer titanium dioxide Titanium particle is easier to spread more evenly across, adheres to the matrix body surface such as glass face；
（3）The present invention can advantageously promote nanometer using surfactants such as high fatty alcohol sulfuric acid ester, aliphatic sulfonic classes The dispersion of TiO 2 particles, while the control for passing through addition, strengthen particle-stabilised performance, more importantly activating agent Hydrophilic group interacts with the hydrone in air so as to sprawl into moisture film in substrate material surface, so as to prevent mist pearl from producing Raw, anti-fog effect is more longlasting；
（4）Using benzyl dimethylamine, triethanolamine, tetrabutyl ammonium bromide etc. as initiator, coated polymeric speed can be accelerated, be carried The degree of cross linking of high coating, shortens hardening time, so as to improve the durability of coating, and significantly improve the matrix of brushing antifoggant Adhesion strength；
（5）The present invention, as dispersant, improves electric double layer using sodium tripolyphosphate, sodium hexameta phosphate, triethyl group hexyl phosphoric acid Thickness, makes nano-particle stability in the solution be weakened by surface electric double layer thickness effect, so as to greatly improve antifoggant Kept for the life-span.
To sum up, prepared by the present invention the self-cleaning antifoggant self-cleaning function of vehicle glass is strong, antifog excellent effect, lignin idol Connection agent and initiator strengthen adhesive attraction of the antifoggant to substrate material surface, realization self-cleaning at any time, antifog Effect is more than 30 days, while preparation process is simple, low cost is easy to use.
Specific embodiment
The present invention is described in further detail with reference to embodiment.
Embodiment 1
（1）Following raw materials are weighed in proportion：
Nanometer Titanium Dioxide Hydrosol, contained nano titanium oxide mass percent concentration is 30%, and pH value is 9.5, titanium dioxide Particle size is 15~30 nanometers：5㎏；
Lignin coupling agent：0.5㎏；
Sodium lauryl sulphate：0.1㎏；
Benzyl dimethylamine：0.2㎏；
Sodium tripolyphosphate：0.001㎏；
Isopropanol：0.209㎏；
0.1N aminoacid：0.050kg；
（2）After lignin coupling agent, benzyl dimethylamine, Nanometer Titanium Dioxide Hydrosol and sodium tripolyphosphate are stirred 18 hours, Add sodium lauryl sulphate to mix 2 hours with the mixed liquor stirring of isopropanol, and add 0.1N amino acid for adjusting pH value to obtain PH is 9 antifoggant；
（3）Detection test：Take a small amount of antifoggant to be applied on vehicle glass piece, after 100 DEG C of drying, be put in the glass for filling boiled water At the about 10cm of glass cup top and the one of antifoggant will be scribbled facing to glass inner side, the antifog effect observed under vapor after 5 seconds Really：The sheet glass that film is crossed understands transparent, fogless pearl generation, with good anti-fog effect；The sheet glass humidity be 80%, Temperature be place 30 days in 25 DEG C of climatic chamber after, with water-vapo(u)r test, still transparent fogless pearl produces, and surface cleaning is antifog Work well.
Embodiment 2
（1）Following raw materials are weighed in proportion：
Nanometer Titanium Dioxide Hydrosol, contained nano titanium oxide mass percent concentration is 35%, and pH value is 10, titanium dioxide Particle size is 15~30 nanometers：9.9㎏；
Lignin coupling agent：0.002㎏；
Dioctyl succinate disulfonate acid：0.0001㎏；
Triethanolamine：0.001㎏；
Sodium hexameta phosphate：0.0001㎏；
Ethylene glycol：0.03㎏；
The ㎏ of 0.01N dilute hydrochloric acid 0.0668；
（2）After lignin coupling agent, triethanolamine, Nanometer Titanium Dioxide Hydrosol and sodium hexameta phosphate are stirred 24 hours, plus Enter the dioctyl succinate disulfonate acid of spent glycol dilution, stirring mixes 30 minutes, and gained reactant liquor adjusts pH value with dilute hydrochloric acid, Prepared pH is 9.5 antifoggant；
（3）Detection test：Take a small amount of antifoggant to be applied on vehicle glass piece, be 75%, temperature in humidity after 110 DEG C of drying After placing 35 days in 24 DEG C of climatic chambers, with water-vapo(u)r test, still transparent fogless pearl produces, clean surface light, without dirt Dye thing, antifog to work well, its antifog effect persistence was more than 30 days.
Embodiment 3
（1）Following raw materials are weighed in proportion：
Nanometer Titanium Dioxide Hydrosol, contained nano titanium oxide mass percent concentration is 35%, and pH value is 10.5, titanium dioxide Titanium particle size is 5~30 nanometers：5㎏；
Lignin coupling agent：4㎏；
Aliphatic alcohol ester：0.0001㎏；
Tetrabutyl ammonium bromide：0.001㎏；
Triethyl group hexyl phosphoric acid：0.0001㎏；
Ethylene glycol：0.548㎏；
0.1N acetic acid：0.45kg；
（2）The stirring 18 of lignin coupling agent, tetrabutyl ammonium bromide, Nanometer Titanium Dioxide Hydrosol and triethyl group hexyl phosphoric acid is little Shi Hou, the mixed liquor for adding aliphatic alcohol ester and ethylene glycol is stirred and mixed 2 hours, and adds 0.1N vinegar acid for adjusting pH value to obtain pH to be 8 antifoggant；
（3）Detection test：Take a small amount of antifoggant to be applied on sheet glass, after 90 DEG C of drying, be put in the glass for filling boiled water At the about 10cm of top and the one of antifoggant will be scribbled facing to glass inner side, after 5 seconds, the anti-fog effect observed under vapor： The sheet glass that film is crossed understands transparent, fogless pearl generation, with good anti-fog effect；The sheet glass is 70%, temperature in humidity After placing 28 days in 24 DEG C of climatic chambers, with water-vapo(u)r test, still transparent fogless pearl produces, antifog to work well.

Claims (7)

1. a kind of preparation method of anti-fog agent for wind-screen of automobile, it is characterised in that comprise the following steps：
（1）Following each component is weighed by following mass percent：
Nanometer Titanium Dioxide Hydrosol 50~99%
Lignin coupling agent 0.02~40%
Surfactant 0.001~30%
Initiator 0.01~5%
Dispersant 0.001~2%
Phase solvent 0~10%
PH regulators 0~10%；
（2）By Nanometer Titanium Dioxide Hydrosol, lignin coupling agent, initiator and dispersant stirring mixing 1 ~ 24 hour；
（3）Treat step（2）Surfactant is added to stir 0.5 ~ 4 hour with the mixture of phase solvent after reaction fully, with PH tune Section agent adjusts the nanometer anti-fog agent that pH is obtained pH 8~10.
2. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The nano-silica It is 9~10.5 to change titanium hydrosol pH, and contained TiO 2 particles size is 15~30 nanometers.
3. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The surface activity Agent is high fatty alcohol sulfuric acid ester, aliphatic sulfonic class, amino acidses, polyalcohols, fatty alcohol esters, fatty glyceride The combination of one or more of class, lecithin apoplexy due to endogenous wind.
4. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The initiator is The combination of one or more in benzyl dimethylamine, triethanolamine, tetrabutyl ammonium bromide.
5. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The dispersant is The combination of one or more in sodium tripolyphosphate, sodium hexameta phosphate, triethyl group hexyl phosphoric acid.
6. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The phase solvent is One or two combination in isopropanol, ethylene glycol.
7. the preparation method of a kind of anti-fog agent for wind-screen of automobile according to claim 1, it is characterised in that：The PH regulators For the diluted acids such as dilute hydrochloric acid, spirit of vinegar, dust technology or the one or more combination in aminoacid.
CN201611157307.8A 2016-12-15 2016-12-15 Preparation method of automotive glass antifogging agent Pending CN106675119A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109370519A (en) * 2018-09-30 2019-02-22 江苏耀兴安全玻璃有限公司 A kind of glass antidimmer and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1696063A (en) * 2004-05-14 2005-11-16 泉耀科技股份有限公司 Method for synthesizing sol of Nano powder of titanium dioxide in visible light type
CN103013198A (en) * 2012-12-19 2013-04-03 江苏博斯腾纳米涂层有限公司 Nano anti-fogging agent and preparation method thereof
CN103013197A (en) * 2012-12-19 2013-04-03 江苏博斯腾纳米涂层有限公司 Preparation method of nano anti-fogging agent

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1696063A (en) * 2004-05-14 2005-11-16 泉耀科技股份有限公司 Method for synthesizing sol of Nano powder of titanium dioxide in visible light type
CN103013198A (en) * 2012-12-19 2013-04-03 江苏博斯腾纳米涂层有限公司 Nano anti-fogging agent and preparation method thereof
CN103013197A (en) * 2012-12-19 2013-04-03 江苏博斯腾纳米涂层有限公司 Preparation method of nano anti-fogging agent

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109370519A (en) * 2018-09-30 2019-02-22 江苏耀兴安全玻璃有限公司 A kind of glass antidimmer and preparation method thereof

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Application publication date: 20170517