CN111621229A - Modified AF (aluminum fluoride) coating material, preparation method thereof and coating method - Google Patents
Modified AF (aluminum fluoride) coating material, preparation method thereof and coating method Download PDFInfo
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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
- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
- C09D187/005—Block or graft polymers not provided for in groups C09D101/00 - C09D185/04
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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
- 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
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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
- 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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- C08G83/00—Macromolecular compounds not provided for in groups C08G2/00 - C08G81/00
- C08G83/001—Macromolecular compounds containing organic and inorganic sequences, e.g. organic polymers grafted onto silica
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- 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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention relates to the technical field of glass manufacturing, in particular to a modified AF (AF) coating material, a preparation method and a coating method thereof, wherein the modified AF coating material comprises the following components in parts by weight: 69-100 parts of modified fluorosilicone resin; 19-32 parts of micro wax powder; the modified fluorosilicone resin is prepared by mixing and reacting the following components in parts by weight: 23-39 parts of a fluorine-containing silane compound; 72-105 parts of orthosilicate; 40-88 parts of FVT; the coating method comprises the steps of putting the treated glass and the modified AF coating material into spraying equipment, and carrying out spraying and baking. The invention provides a modified AF coating material, which has the effect that an AF film formed on the surface of glass has high adhesion with the glass so as to be difficult to fall off.
Description
Technical Field
The invention relates to the technical field of glass manufacturing, in particular to a modified AF (AF) coating material, a preparation method and a coating method thereof.
Background
The touch screen is an induction type liquid crystal display device capable of receiving input signals of a contact and the like, is the simplest, convenient and natural man-machine interaction medium at present, gives a brand-new appearance to multimedia, and is brand-new multimedia interaction equipment with great attraction. Because the touch screen surface is often touched with the finger and is operated, the filth on the finger especially greasy dirt is easily attached to the touch screen surface to leave the fingerprint, influence visual effect.
In view of the above problems, in the glass processing production applied to the touch screen, an AF coating process (AF is fingerprint resistance) is generally performed on the surface of the touch screen glass. The conventional AF coating process comprises spray coating, vacuum evaporation, vacuum sputtering and the like, wherein in the spray coating process, spray coating liquid made of an AF coating material is used, the spray coating liquid made of the AF coating material is sprayed on the surface of glass through a spraying device, and an AF film is formed on the surface of the glass through solidification. The AF coating material is plated on the surface of the glass in the mode and forms an AF film, so that the surface of the touch screen glass has the fingerprint resistance. The AF film is a hydrophobic and oleophobic film layer which is mainly made of organic fluorine materials, and the organic fluorine materials have excellent hydrophobic and oleophobic properties, so that after the AF film is formed on the surface of the touch screen glass, the touch screen glass has the performance that fingerprints are not easy to leave on the surface.
However, the organic fluorine material is difficult to bond to the glass surface due to its water and oil repellency, so the AF film attached to the glass surface of the touch panel is often easily peeled off, and the touch panel surface is frequently touched, and is not resistant to rubbing for a long period of time.
Disclosure of Invention
The first object of the present invention is to provide a modified AF plating material, which has a high adhesion between an AF film formed on a glass surface and the glass, and which has an effect of preventing the AF film from falling off.
The second purpose of the invention is to provide a preparation method of the modified AF coating material, and the prepared modified AF coating material has good storage stability so as to ensure the effect that the modified AF coating material is not easy to fall off after being sprayed on the surface of glass.
The third purpose of the invention is to provide a coating method of the modified AF coating material, which has the advantage of improving the adhesion of the AF film and the touch screen glass.
In order to achieve the first object, the invention provides the following technical scheme: a modified AF plating material comprises the following components in parts by weight:
69-100 parts of modified fluorosilicone resin;
19-32 parts of micro wax powder;
the modified fluorosilicone resin is prepared by mixing and reacting the following components in parts by weight:
23-39 parts of a fluorine-containing silane compound;
72-105 parts of orthosilicate;
40-88 parts of FVT (alkoxy modified fluorine-containing polysiloxane).
The present invention in a preferred example may be further configured to: the modified AF plating layer material comprises the following components in parts by weight:
80 parts of modified fluorosilicone resin;
20 parts of micro wax powder.
By adopting the technical scheme, C in the modified fluorine-silicon resin2H5-SiO3H (orthosilicate) + H2O→C2H5OH+H2SiO3，H2SiO3＝SiO2+H2Hydrolyzing O, orthosilicate step by utilizing a sol-gel method to obtain SiO2Sol, and simultaneously carrying out condensation reaction on the SiO2 sol and FVT to prepare a fluorosilicone resin prepolymer with hydroxyl groups on the surface, and continuously condensing the prepolymer with a fluorine-containing silane compound to obtain colorless and transparent modified fluorosilicone resin; the fluorosilicone resin prepolymer with hydroxyl groups on the surface can control SiO2The particles are agglomerated and the fluorine-containing silane compound can be grafted to SiO2The particle surface, therefore, the prepared modified fluorosilicone resin simultaneously has an organic part and an inorganic rough part, wherein the organic part is a group with hydrophobic and oleophobic properties, the inorganic rough part is a Si-OH group, when the modified AF coating material is sprayed on the glass surface and baked, the Si-OH group has stronger bonding force with the hydroxyl on the glass, and the Si-OH group is arranged and distributed on the glass surface and finally bonded with the glass in a chemical bond mode, so that the modified AF coating material is bonded with the glass in a way of chemical bondThe adhesive force between the material and the glass surface is obviously improved.
The modified AF plating material is also mixed with the micro-wax powder, the micro-wax powder is good in dispersion compatibility in liquid resin and has certain viscosity, and the whole resin can be uniformly and stably stored for a long time. Because the micro-wax powder has the characteristics of scratch resistance, adhesion resistance, friction resistance, smooth hand feeling improvement and the like, the micro-wax powder is added into the modified AF plating layer material, so that the integral rigidity of the modified AF plating layer material can be enhanced, the friction resistance of the modified AF plating layer material is improved, in addition, the characteristic of smooth hand feeling can be endowed to the modified AF plating layer material, and the user experience feeling can be greatly improved.
The present invention in a preferred example may be further configured to: the particle size of the micro wax powder is less than or equal to 5 mu m.
By adopting the technical scheme, the isolation and hydrophobicity of the product can be influenced by the overlarge particle size of the micro-wax powder, and even the combination of the modified fluorosilicone resin and the glass surface can be influenced.
The present invention in a preferred example may be further configured to: the fluorine-containing silane compound is POTS (perfluorooctyltrimethoxysilane).
By adopting the technical scheme, the POTS is a silane compound containing fluoroalkyl functional groups, and has the advantages of high heat resistance, high chemical stability, low surface free energy and the like.
The present invention in a preferred example may be further configured to: the FVT is prepared by mixing and reacting the following components in parts by weight: the mass ratio of FVSA (trifluoropropylvinyl silicone oil) to TMS (trimethoxyhydrosilane) is (1.7-2.5) to (0.7-1.4).
By adopting the technical scheme, the FVSA and the TMS are subjected to hydrosilylation reaction to obtain the FVT.
In order to achieve the second object, the invention provides the following technical scheme:
a preparation method of a modified AF (AF) coating material comprises the following steps:
(1) preparing modified fluorosilicone resin: weighing 100-125 parts of alcohol solution, 72-105 parts of orthosilicate, 40-88 parts of FVT and 23-39 parts of POTS according to parts by weight, mixing and reacting step by step, and removing the solvent by reduced pressure distillation to obtain modified fluorosilicone resin fluid;
(2) preparing a modified AF plating material: and (2) weighing 19-32 parts of micro-wax powder, adding the micro-wax powder into the modified fluorosilicone resin fluid prepared in the step (1), uniformly stirring, drying and curing, and performing air cooling and grain cutting to obtain solid modified AF plating layer material particles.
The present invention in a preferred example may be further configured to: in the step (1), the step-by-step mixing reaction specifically comprises the following steps: taking orthosilicate, distilled water and POTS as reactants, averagely dividing the reactants into 3 parts, firstly, adding 2 parts of the reactants into a system for reaction, slowly dripping the rest 1 part of the reactants into the system after the system is heated to 55-70 ℃, adjusting the pH value to 4-5 by hydrochloric acid, reacting for 2-3h, and carrying out cohydrolysis and polycondensation for 6-7 h.
By adopting the technical scheme, as C2H5-SiO3H (orthosilicate) + H2O→C2H5OH+H2SiO3，H2SiO3＝SiO2+H2Hydrolyzing O, orthosilicate step by utilizing a sol-gel method to obtain SiO2Sol of SiO2The sol and FVT condensation reaction can prepare fluorosilicone resin prepolymer with hydroxyl groups on the surface, and the fluorosilicone resin prepolymer is continuously condensed with the fluorine-containing silane compound to obtain colorless and transparent modified fluorosilicone resin; wherein the purpose of the step-by-step reaction is to hydrolyze orthosilicate in the system step by step to obtain SiO2Sol of SiO2The sol and FVT condensation reaction can prepare fluorosilicone resin prepolymer with hydroxyl groups on the surface, so that the prepolymer of fluorosilicone resin with hydroxyl groups on the surface can be fully grafted with POTS.
The micro-wax powder is directly added into the modified fluorosilicone resin fluid, and can be uniformly dispersed in the modified fluorosilicone resin fluid under full stirring because the micro-wax powder has good dispersion compatibility in liquid resin.
In the step (2), the modified fluorosilicone resin fluid prepared by the sol-gel method is dried and cured, so that modified AF plating material particles with a nano structure can be obtained. In addition, the modified AF coating material is prepared into solid particles, and compared with the traditional fluid AF coating material, the solid modified AF coating material particles have the characteristics of long storage time, difficult drying and good substance stability, so that the modified AF coating material is not easy to lose efficacy.
In order to achieve the third object, the invention provides the following technical solutions:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 20-40min, and oven drying;
(2) feeding glass: mounting the glass on a spraying appliance, and then sending the glass into a spraying chamber;
(3) pretreatment of modified AF plating material: adding the modified AF coating material into an organic solvent and preparing into a spraying liquid;
(4) spraying: spraying a spraying liquid prepared from the modified AF coating material on the surface of the glass;
(5) baking: and (5) baking the glass.
The present invention in a preferred example may be further configured to: in the step (3), the specific preparation method of the spraying liquid comprises the following steps: and taking 4.5-6g of solid modified AF plating material particles, adding 42-50g of a mixed organic solvent of a fluoroether solvent and 30-35g of butyl acrylate, stirring for 20-30min, and performing ultrasonic dispersion for 30-35min to obtain the fluid modified AF plating material.
By adopting the technical scheme, the modified AF coating material particles stored in a solid state are dissolved by using an organic solvent before spraying, so that the modified AF coating material particles are suitable for the subsequent spraying step. The fluid modified AF coating material is sprayed on the surface of the glass by using spraying equipment, and a layer of AF film can be formed on the surface of the glass after baking.
The baking is to accelerate the volatilization of the solvent and the reaction between the resins, attach the resins on the surface of the glass to form nuclei and grow into a solid film, finally form a continuous film by the contact and combination of adjacent stable nuclei, solidify the modified AF coating material on the surface of the glass and dry the AF film
The present invention in a preferred example may be further configured to: the baking temperature in step (5) is set at 120-180 ℃.
By adopting the technical scheme, the butyl acrylate solvent and the fluoroether solvent begin to volatilize at 120 ℃, the baking temperature is higher than 120 ℃ so as to volatilize the butyl acrylate solvent and the fluoroether solvent and leave the active ingredients of the modified AF coating material on the surface of the glass, and the baking temperature is controlled below 180 ℃ so as to prevent the active ingredients of the modified AF coating material from being decomposed and losing efficacy.
The present invention in a preferred example may be further configured to: the baking temperature in the step (5) is set at 140-150 ℃.
By adopting the technical scheme, the baking temperature is set within the range of 140-150 ℃, so that the butyl acrylate solvent and the fluoroether solvent can be volatilized, the effective components of the modified AF coating material can not be decomposed, and the baking and curing efficiency and the film forming quality of the AF film can be improved.
In conclusion, the invention has the following beneficial effects:
firstly, in the formula of the modified AF coating material, SiO is added on the basis of fluorine-containing silane compound2Inorganic substance to allow the fluorine-containing silane compound to pass through SiO2The adhesion degree of the structure and the glass surface is larger so as to achieve the effect that the AF film is not easy to fall off.
Secondly, in the preparation method of the modified AF coating material, the modified AF coating material is prepared into solid particles, so that the modified AF coating material has the characteristics of long storage period and stable substance, and the effect that the modified AF coating material is not easy to fall off after being sprayed on the surface of glass is ensured.
Thirdly, in the coating method of the modified AF coating material, the modified AF coating material is sprayed on the surface of the glass, and an AF film with strong adhesion with the surface of the glass and good wear resistance can be formed on the surface of the glass.
Detailed Description
The present invention will be described in further detail with reference to examples.
The reagents used in the following examples and comparative examples are preferably those manufactured by the following manufacturers, and it should be noted that the technical skill in the art can select the reagents manufactured by any manufacturers according to the teachings of the present invention, and the reagents are within the protection scope of the present invention.
Tetraethoxysilane was purchased from chemical reagents ltd of miou europe, department of tianjin; POTS produced by Hangzhou Anjiarui scientific and technological limited is selected as POTS; FVSA is purchased from Jingyi glass, Inc. of Shenzhen; TMS was purchased from Trifluoropropylmethylsiloxane, a vinyl-terminated fluorosilicone oil, produced by Shanghai silicon friend New materials science and technology, Inc.; the micro-wax powder is purchased from Shanghai Kayin chemical Co.
The alcohol solution described below may be one or more of methanol solution, ethanol solution, isobutanol, and isoamyl alcohol, and the alcohol solution in the present application is preferably an ethanol solution. The orthosilicate described below may be methyl orthosilicate or ethyl orthosilicate, and the orthosilicate in this application is preferably ethyl orthosilicate.
In all the following examples and comparative examples, the same production batch was used for the glass used.
Examples
Example 1:
a modified AF plating material is prepared by mixing modified fluorine-silicon resin and wax powder,
wherein, the FVT is prepared firstly for preparing the modified fluorosilicone resin.
The preparation method of the FVT comprises the following steps: mixing m (fvsa): m (tms) ═ 2: adding FVSA and TMS of 1 into a flask, adding a catalyst chloroplatinic acid when the temperature of the system is raised to 83 ℃, and reacting for 2 hours to obtain transparent viscous liquid.
(1) Preparing modified fluorosilicone resin: weighing 300 parts of distilled water, 100 parts of ethanol solution, 72 parts of ethyl orthosilicate, 40 parts of FVT and 23 parts of POTS according to parts by weight, taking the ethyl orthosilicate, the distilled water and the POTS as reactants, averagely dividing the reactants into 3 parts, firstly adding 2 parts of the reactants into a system, heating the system to 60 ℃, adjusting the pH value to 4 by hydrochloric acid (the mass fraction is 37%), reacting for 2h, slowly dripping the rest 1 part of the reactants into the system, carrying out cohydrolysis and polycondensation for 6h, and removing the solvent by reduced pressure distillation to obtain the modified fluorosilicone resin fluid.
(2) And weighing 20 parts of micro-wax powder, adding the micro-wax powder into 80 parts of modified fluorosilicone resin fluid, uniformly stirring, drying and curing, and performing air cooling and grain cutting to obtain solid modified AF plating layer material particles.
TABLE 1 component proportions of modified AF-coating materials in examples 1 to 5
| The components are added in | Modified fluorosilicone resin | Micro wax powder |
| Example 1 | 80 | 20 |
| Example 2 | 80 | 19 |
| Example 3 | 80 | 25 |
| Example 4 | 80 | 28 |
| Example 5 | 80 | 32 |
Examples 2 to 5:
a modified AF plating material is different from that of example 1 in the amount of the wax powder, which is shown in Table 1, and the rest is the same as that of example 1.
Examples 6 to 11:
a modified AF plating material is different from that of example 1 in the component amounts of the modified fluorosilicone resin, which are shown in Table 2, and the rest is the same as that of example 1.
TABLE 2 component proportions of modified fluorosilicone resins in modified AF-plated materials in examples 6 to 11
Example 12:
a modified AF plating material is different from that in example 1 in that FOTS (perfluorooctyltrichlorosilane) is selected as a fluorine-containing silane compound, wherein FOTS is selected from FOTS produced by Shanghai Germing Biotech limited.
Example 13:
a modified AF plating material is different from that in example 2 in that FOTS is selected as the fluorine-containing silane compound, wherein FOTS is selected from FOTS produced by Shanghai sprouted Biotech limited.
Application example 1:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(3) Pretreatment of modified AF plating material: adding the modified AF plating material particles prepared in the example 1 into an organic solvent and preparing a spraying liquid; the preparation method of the spraying liquid comprises the following steps: taking 4.5g of solid modified AF plating material particles, adding 42g of a mixed organic solvent of a fluoroether solvent and 30g of butyl acrylate, stirring for 20min, and performing ultrasonic dispersion for 30 min.
(4) Spraying: and (4) spraying the spraying liquid in the step (3) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 145 ℃.
Application example 2:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 2.
Application example 3:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 3.
Application example 4:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 4.
Application example 5:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 5.
Application example 6:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 6.
Application example 7:
a modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 7.
Application example 8:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 8.
Application example 9:
a modified AF coating material, which is different from the first application example in that the modified AF coating material was prepared in example 9.
Application example 10:
the modified AF coating material is different from the first application example in that the modified AF coating material is prepared by adopting the first application example 10.
Application example 11:
a modified AF coating material, which is different from the first application example in that the modified AF coating material was obtained in example 11.
Application example 12:
a modified AF coating material, which is different from the first application example in that the modified AF coating material was prepared in example 12.
Application example 13:
a modified AF coating material, which is different from the first application example in that the modified AF coating material was obtained in example 13.
Application example 14:
a coating method of a modified AF coating material comprises the following steps:
(1) pretreatment of modified AF plating material: after being left for 3 months, the modified AF plating material particles prepared in the example 1 are added into an organic solvent to be prepared into a spraying liquid, wherein the specific preparation method of the spraying liquid comprises the following steps: taking 4.5g of solid modified AF plating material particles, adding 42g of a mixed organic solvent of a fluoroether solvent and 30g of butyl acrylate, stirring for 20min, and performing ultrasonic dispersion for 30 min.
(2) Glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(3) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(4) Spraying: and (3) spraying the spraying liquid in the step (1) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 145 ℃.
Application examples 15 to 17:
a modified AF plating material is different from that of the first application example in the baking temperature in the step (5), specifically shown in Table 3, and the rest is the same as that of the first application example.
TABLE 3 baking temperature settings for step (5) of application examples 15-17
| Baking temperature/. degree.C | |
| Application example 15 | 148 |
| Application example 16 | 130 |
| Application example 17 | 160 |
Application example 18:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) Feeding glass: the glass was mounted on a spray applicator and then fed into a spray booth.
(3) Pretreatment of modified AF plating material: adding the modified AF plating material prepared in the example 1 into an organic solvent and preparing a spraying liquid; the preparation method of the spraying liquid comprises the following steps: taking 6g of solid modified AF plating material particles, adding 50g of a mixed organic solvent of a fluoroether solvent and 35g of butyl acrylate, stirring for 30min, and performing ultrasonic dispersion for 35 min.
(4) Spraying: and (4) spraying the spraying liquid in the step (3) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 145 ℃.
Comparative example 1:
a modified AF plating material is different from that of example 1 in that no wax powder is added.
Comparative example 2:
a modified AF plating material was distinguished from example 1 in that 10 parts of a wax powder was added.
Comparative example 3:
a modified AF plating material is different from that of embodiment 1 in that the modified AF plating material is prepared by mixing fluorine-silicon resin and micro-wax powder, wherein the fluorine-silicon resin is not modified and POTS produced by Hangzhou AnjiaRui technology limited is directly selected.
And (3) weighing 20 parts of micro-wax powder, adding the micro-wax powder into 80 parts of POTS, uniformly stirring, drying and curing, and performing air cooling and dicing to obtain solid modified AF (AF) coating material particles.
Comparative example 4:
a modified AF plating material is prepared by mixing modified fluorosilicone resin and micro wax powder, wherein FVT is prepared respectively for preparing the modified fluorosilicone resin.
The preparation method of the FVT comprises the following steps: mixing m (fvsa): m (tms) ═ 2: adding FVSA and TMS of 1 into a flask, adding a catalyst chloroplatinic acid when the temperature of the system is raised to 83 ℃, and reacting for 2 hours to obtain transparent viscous liquid.
(1) Preparing modified fluorosilicone resin: weighing 300 parts of distilled water, 100 parts of ethanol solution, 72 parts of ethyl orthosilicate, 40 parts of FVT and 23 parts of POTS (plain old telephone), adding the reactants into the system at one time, heating the system to 60 ℃, adjusting the pH value to 4 by hydrochloric acid (mass fraction is 37%), reacting for 2 hours, slowly dripping the rest 1 part of reactants into the system, cohydrolyzing and polycondensing for 6 hours, and removing the solvent by reduced pressure distillation to obtain the modified fluorosilicone resin fluid.
(2) And weighing 20 parts of micro-wax powder, adding the micro-wax powder into 80 parts of modified fluorosilicone resin fluid, uniformly stirring, drying and curing, and performing air cooling and grain cutting to obtain solid modified AF plating layer material particles.
Comparative example 5:
a modified AF plating material is prepared by mixing modified fluorosilicone resin and micro wax powder, wherein FVT is prepared respectively for preparing the modified fluorosilicone resin.
The preparation method of the FVT comprises the following steps: mixing m (fvsa): m (tms) ═ 2: adding FVSA and TMS of 1 into a flask, adding a catalyst chloroplatinic acid when the temperature of the system is raised to 83 ℃, and reacting for 2 hours to obtain transparent viscous liquid.
(1) Preparing modified fluorosilicone resin: weighing 300 parts of distilled water, 100 parts of ethanol solution, 72 parts of ethyl orthosilicate, 40 parts of FVT and 23 parts of POTS according to parts by weight, taking the ethyl orthosilicate, the distilled water and the POTS as reactants, averagely dividing the reactants into 3 parts, firstly adding 2 parts of the reactants into a system, heating the system to 60 ℃, adjusting the pH value to 4 by hydrochloric acid (the mass fraction is 37%), reacting for 2h, slowly dripping the rest 1 part of the reactants into the system, carrying out cohydrolysis and polycondensation for 6h, and removing the solvent by reduced pressure distillation to obtain the modified fluorosilicone resin fluid.
(2) And (2) adding the modified fluorosilicone resin fluid obtained in the step (1) into a fluoroether solvent, and performing ultrasonic dispersion to obtain a fluid-like modified AF plating material.
Comparative application example 1:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(3) Pretreatment of modified AF plating material: the modified AF plating material prepared in comparative example 1 was added to an organic solvent and formulated into a spray liquid.
(4) Spraying: and (4) spraying the spraying liquid in the step (3) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 145 ℃.
Comparative application example 2:
a coating method of a modified AF coating material, which is different from comparative application example 1 in that the modified AF coating material was prepared using comparative example 2.
Comparative application example 3:
a coating method of a modified AF coating material, which is different from comparative application example 1 in that the modified AF coating material was prepared using comparative example 3.
Comparative application example 4:
a coating method of a modified AF coating material is different from that of comparative application example 1 in that the modified AF coating material is prepared by using comparative example 4.
Comparative application example 5:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(3) Spraying: the fluid modified AF coating material prepared in comparative example 5 was sprayed onto the glass surface to a thickness of 0.1 mm.
(4) Baking: baking the glass at 145 ℃.
Comparative application example 6:
a coating method of a modified AF coating material comprises the following steps:
(1) pretreatment of modified AF plating material: the fluid modified AF-plated material prepared in comparative example 5 was left to stand for 3 months.
(2) Glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(3) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(4) Spraying: and (3) spraying the fluid modified AF coating material in the step (1) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 145 ℃.
Comparative application example 7:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(3) Pretreatment of modified AF plating material: the modified AF plating material prepared in example 1 was added to an organic solvent and formulated into a spray coating liquid.
(4) Spraying: and (4) spraying the spraying liquid in the step (3) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 100 ℃.
Comparative application example 8:
a coating method of a modified AF coating material comprises the following steps:
(1) glass coating pretreatment: ultrasonic cleaning for 30min, and oven drying.
(2) And (3) mounting glass: and (5) conveying the mixture into a spraying chamber.
(3) Pretreatment of modified AF plating material: the modified AF plating material prepared in example 1 was added to an organic solvent and formulated into a spray coating liquid.
(4) Spraying: and (4) spraying the spraying liquid in the step (3) on the surface of the glass, wherein the spraying thickness is 0.1 mm.
(5) Baking: baking the glass at 220 ℃.
Performance detection
The water and oil repellency of the AF film is expressed by the water drop angle of distilled water on the surface of glass; the hardness of the AF film is expressed by the scratching condition of a Mitsubishi 7H pencil on the surface of glass according to the GB/T6739-1996 standard; the rubbing resistance of the AF film was represented by the water drop angle after steel wool was rubbed 3000 times on the glass surface; the smoothness of the AF film is expressed by a wiping coefficient of the BEMCOT dust-free cloth wiping the glass surface; the chemical resistance of the AF film was expressed as the water drop angle after the glass was wrapped with dust-free cloth soaked with artificial sweat for 48 hours.
The detection method comprises the following steps:
(1) detection method of initial water drop angle test: a water drop angle tester (SDC200) is adopted, distilled water is used as a probe, liquid is dropped on the surface of the glass, the size of the water drop is 5 mu L, and the water drop angle is not less than 110 degrees, so that the glass is qualified.
(2) The pencil hardness test detection method comprises the following steps: the glass is scratched by a Mitsubishi 7H pencil under the conditions of 1kg pressure, 5mm/s speed and 40mm stroke by adopting a pencil hardness tester, and the glass is qualified after no scratch is formed on the surface.
(3) The detection method of the friction resistance test comprises the following steps: a friction tester is adopted, a contact area of 10 x 10mm is taken, under the conditions that the pressure is 1kg, the friction speed is 60 times/min and the friction stroke is 40mm, steel wool is used for rubbing 3000 times on the surface of the glass, then a water drop angle test is carried out by adopting a detection method of an initial water drop angle test, and the water drop angle is not less than 105 degrees and is a qualified product.
(3) The detection method of the dynamic friction coefficient comprises the following steps: wiping the surface of the glass by using a dynamic friction tester and using BEMCOT dust-free cloth with the area of 10 x 10mm under the conditions of the load of 100g and the wiping speed of 500mm/min, wherein the wiping coefficient is less than 0.04, and the glass is qualified.
(4) The detection method for the artificial sweat resistance test comprises the following steps: an environment test box is adopted, under the conditions that the temperature is 45 ℃ and the humidity is 45%, the glass is wrapped by dust-free cloth soaked by artificial sweat, the glass is cleaned after being placed for 48 hours, then a water drop angle test is carried out by adopting a detection method of an initial water drop angle test, and the water drop angle is not less than 100 degrees and is a qualified product.
The results are shown in the following table:
as can be seen from the above table, the AF film formed by spraying the modified AF coating material prepared in each application example onto the glass surface exhibits good effects in terms of water and oil repellency, abrasion resistance, smoothness, sweat resistance, and the like, and thus it can be seen that the AF film formed on the glass surface by the modified AF coating material prepared in each application example can be well adhered to the glass surface.
In examples 1 to 5, the micro-wax powder is added to the modified fluorosilicone resin, and the overall rigidity of the modified AF coating material is enhanced by utilizing the characteristics of scratch resistance, adhesion resistance, abrasion resistance, smoothness improvement and the like of the micro-wax powder, so that the abrasion resistance of the modified AF coating material is improved, and as can be seen from the data of application examples 1 to 5 and comparative application examples 1 to 2, the micro-wax powder is added to the modified fluorosilicone resin, the overall hydrophobic and oleophobic performance of the modified AF coating material is not affected, and the dynamic friction coefficient test performance and the abrasion resistance performance are excellent, so that the obtained AF film can be better combined with glass, and under the condition that the micro-wax powder is not added, the performance of the AF film is reduced on a pencil hardness test and a dynamic friction coefficient test, and the smoothness of the corresponding AF film is proved to be insufficient.
Examples 6 to 11, the amounts of the respective components for preparing the modified fluorosilicone resin were changed, and according to the test results of application examples 6 to 11, it was found that the test results of application example 1 were comparable, and the differences from the test results of example 1 were not large among all the test items of the initial water drop angle test, the pencil hardness test, the rub resistance test, the coefficient of kinetic friction, and the artificial sweat resistance test.
Examples 12 to 13, in which the POTS having the advantages of high heat resistance, high chemical resistance, low surface free energy, etc., in the modified fluorosilicone resin was replaced with FOTS, the tests of pencil hardness and coefficient of dynamic friction were all performed with a certain reduction in other properties, and particularly the test results of the initial water drop angle were significantly different from those of the previous examples, which demonstrated that POTS was more prominent in the heat resistance, chemical resistance, and hydrophobicity in the reaction for preparing the modified fluorosilicone resin than FOTS, and that even when the modified AF plating material was prepared using the fluorine-containing silane compound such as POTS, an AF film having better adhesion to the glass surface was obtained.
According to the data of comparative application example 3 and application example 1, POTS was directly used as the fluorosilicone resin in comparative application example 3 without SiO2POTS was modified to perform poorly in the initial water drop angle test, rub resistance test, and artificial sweat resistance test, i.e., SiO2The AF membrane prepared by the POTS modification method can improve the hydrophobic and oleophobic properties, the friction resistance and the chemical resistance stability.
According to the detection results of application example 1 and application example 14, the prepared solid modified AF coating material particles are sprayed on glass for AF film coating after 3 months of storage time, and the obtained glass has little difference in various performances; the detection results of comparative application examples 5-6 are combined, it can be seen that the freshly prepared fluid AF coating material is sprayed on the glass, the performance of the obtained glass is not much different from that of application example 1 in all detection performances, but the fluid AF coating material is sprayed on the glass to be coated with the AF film after being placed for 3 months, and the obtained glass has a phenomenon of great reduction in all detection performances, so that the solid modified AF coating material particles are proved to be better than the fluid modified AF coating material in long-term storage.
According to the test results of application examples 15 to 17 and comparative application examples 7 to 8, the baking temperature is too high or too low, which has a certain influence on the performance of the modified AF coating material, wherein the pencil hardness test and the coefficient of dynamic friction test have no influence, i.e. the AF film has consistent performance in both rigidity and smoothness, but the AF film has greatly reduced performance in the initial water drop angle test, the friction resistance test and the artificial sweat resistance test, i.e. the AF film has poor hydrophobic and oleophobic performance, friction resistance and chemical stability.
The present embodiment is only for explaining the present invention, and it is not limited to the present invention, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present invention.
Claims (9)
1. The modified AF plating material is characterized by comprising the following components in parts by weight:
69-100 parts of modified fluorosilicone resin;
19-32 parts of micro wax powder;
the modified fluorosilicone resin is prepared by mixing and reacting the following components in parts by weight:
23-39 parts of a fluorine-containing silane compound;
72-105 parts of orthosilicate;
40-88 parts of FVT.
2. The modified AF coating material of claim 1, comprising the following components in parts by weight:
80 parts of modified fluorosilicone resin;
20 parts of micro wax powder.
3. A modified AF coating material as claimed in claim 1, wherein the fluorine-containing silane compound is POTS.
4. The modified AF coating material of claim 1, wherein the FVT is obtained by mixing and reacting the following components in parts by weight: the mass ratio of FVSA to TMS is (1.7-2.5) to (0.7-1.4).
5. A method for preparing a modified AF-coating material as claimed in any one of claims 1 to 4, characterized in that it comprises the following steps:
(1) modified fluorosilicone resin: weighing 100-125 parts of alcohol solution, 250-360 parts of distilled water, 72-105 parts of orthosilicate, 40-88 parts of FVT and 23-39 parts of POTS according to parts by weight, mixing and reacting step by step, and removing the solvent by reduced pressure distillation to obtain modified fluorosilicone fluid;
(2) and (2) weighing 19-32 parts of micro-wax powder, adding the micro-wax powder into the modified fluorosilicone resin fluid prepared in the step (1), uniformly stirring, drying and curing, and performing air cooling and grain cutting to obtain solid modified AF plating layer material particles.
6. The preparation method of the modified AF coating material as claimed in claim 5, wherein in the step (1), the step-by-step mixing reaction is specifically as follows: taking orthosilicate, distilled water and POTS as reactants, averagely dividing the reactants into 3 parts, firstly adding 2 parts of the reactants into a system, heating the system to 55-70 ℃, adjusting the pH value to be =4-5 by hydrochloric acid, reacting for 2-3h, then slowly dripping the rest 1 part of the reactants into the system, and carrying out cohydrolysis and polycondensation for 6-7 h.
7. A coating method using the modified AF coating material described in any one of claims 1 to 4, characterized by comprising the steps of:
(1) glass coating pretreatment: ultrasonic cleaning for 20-40min, and oven drying;
(2) and (3) mounting glass: sending into a spraying chamber;
(3) pretreatment of modified AF plating material: adding the modified AF coating material into an organic solvent and preparing into a spraying liquid;
(4) spraying: spraying a spraying liquid prepared from the modified AF coating material on the surface of the glass;
(5) baking: and (5) baking the glass.
8. The coating method of a modified AF coating material as claimed in claim 7, wherein the baking temperature in step (5) is set at 120-180 ℃.
9. The coating method of a modified AF coating material as claimed in claim 7, wherein the baking temperature in step (5) is set at 140-150 ℃.
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