CN109678359B - Preparation method and application of self-cleaning glass hydrophobic agent - Google Patents
Preparation method and application of self-cleaning glass hydrophobic agent Download PDFInfo
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- CN109678359B CN109678359B CN201910028051.8A CN201910028051A CN109678359B CN 109678359 B CN109678359 B CN 109678359B CN 201910028051 A CN201910028051 A CN 201910028051A CN 109678359 B CN109678359 B CN 109678359B
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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
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/007—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
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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
- C03C17/006—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character
- C03C17/008—Surface treatment of glass, not in the form of fibres or filaments, by coating with materials of composite character comprising a mixture of materials covered by two or more of the groups C03C17/02, C03C17/06, C03C17/22 and C03C17/28
- C03C17/009—Mixtures of organic and inorganic materials, e.g. ormosils and ormocers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
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Abstract
The invention belongs to the technical field of glass surface treatment, and particularly relates to a preparation method and application of a self-cleaning glass hydrophobic agent, which comprises the following steps of S1, preparing a component A, carrying out polymerization reaction on methyl cyclosiloxane, methyl phenyl siloxane and a silane coupling agent under certain conditions to obtain ternary polymerization siloxane, and filtering after reacting with a surfactant and a solvent to obtain the component A; and S2, preparing a component B, carrying out polymerization reaction on dimethyl cyclosiloxane, methyl phenyl siloxane and a silane coupling agent under a certain condition to obtain ternary polymerization siloxane, reacting with a surfactant and a solvent, and filtering to obtain the component B. The preparation method is simple, the quantitative production requirement is low, after the prepared product acts on the surface of the glass, water drops can form water drops on the surface of the glass, the contact angle can reach up to 125 degrees, and the automatic rolling without marks can be realized.
Description
Technical Field
The invention belongs to the technical field of glass surface treatment, and particularly relates to a preparation method and application of a self-cleaning glass hydrophobic agent.
Background
The surface of common glass is a hydrophilic surface, when water drops spread on the glass, the light transmittance of the glass is deteriorated, and the blurs of a windshield, a side windshield and front and rear view mirrors of an automobile are important causes of traffic accidents. In the case of rain or high humidity, the surface of the automobile glass forms attached liquid drops to influence the sight.
Disclosure of Invention
The invention aims to solve the problems and provides a preparation method of a self-cleaning glass hydrophobic agent, which has simple process and low quantitative production requirement, and after the prepared product acts on the surface of glass, water drops can form water drops on the surface of the glass, the contact angle can reach up to 125 degrees, and the automatic rolling can be realized without leaving traces.
The invention is realized by adopting the following technical scheme:
a preparation method of a self-cleaning glass hydrophobic agent comprises the following steps:
s1, preparing the component A, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to a proportion, mixing and stirring uniformly, and heating to obtain a hot material; adding an alkaline catalyst into the hot materials, carrying out polymerization reaction under certain conditions to obtain ternary copolymerized siloxane, cooling to room temperature, adding a surfactant, mixing uniformly, adding a solvent for emulsification, and filtering to obtain the component A.
S2, preparing the component B, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to the proportion, mixing and stirring uniformly, and heating to obtain a hot material; adding an alkaline catalyst into the hot materials, carrying out polymerization reaction under certain conditions to obtain ternary copolymerized siloxane, cooling to room temperature, adding a surfactant, mixing uniformly, adding a solvent for emulsification, and filtering to obtain a component B.
Preferably, in the step S1, the heating is carried out to 80-90 ℃ to obtain the hot material.
In a preferred embodiment, in step S1 and step S2, the polymerization conditions are: the reaction is carried out under the condition of stirring, the temperature is 125-150 ℃, and the reaction time is 3-5 h.
Preferably, the stirring speed is 30-60 rpm.
Preferably, in steps S1 and S2, the basic catalyst is tetramethylammonium hydroxide. The tetramethylammonium hydroxide is decomposed into trimethylamine and dimethyl ether at 135-140 ℃, and the tetramethylammonium hydroxide plays an important role as an alkaline catalyst for polymerization reaction. Acid neutralization is not needed, and no waste water is generated.
Preferably, in step S1, the hot material further includes nanoparticles, and the nanoparticles are one or more of nano-silica and nano-zinc oxide.
Preferably, in the step S2, the surfactant and the nano titanium oxide are added, wherein the particle size of the nano titanium oxide is 20-5 nm.
The self-cleaning glass hydrophobic agent comprises a component A and a component B, wherein the component A and the component B are prepared by the method.
The application of the self-cleaning glass hydrophobic agent comprises the steps of spraying the component A prepared by the method on the surface of glass, drying to form a reference film, spraying the component B prepared by the method on the reference film, and drying to form a hydrophobic film.
Preferably, the component B prepared by the method is sprayed on a hydrophobic membrane to form new hydrophobicity.
The invention has the beneficial effects that:
1. the preparation method has simple process and low quantitative production requirement, and after the prepared product acts on the surface of the glass, water drops can form water drops on the surface of the glass, the contact angle can reach up to 125 degrees, and the product can automatically roll off without leaving traces.
2. The self-cleaning glass hydrophobic agent disclosed by the invention has better hydrophobicity and weather resistance, is effective for a long time after being used, has the advantages of wear resistance, washing resistance and the like, and keeps the attractiveness of glass without influencing the transmittance of the glass.
3. After the component A is sprayed on the surface of the glass, the nano particles can fill up microscopic pores on the surface of the glass, and because the nano particles have high specific surface area and act on the surface of the glass together with the terpolymer, the terpolymer forms a strong bonding effect with the nano particles and the surface of the glass, so that the surface of the glass has a layer of long-term effective, wear-resistant and washing-resistant reference film.
4. The component B forms a transparent hydrophobic film after being used, the nano titanium oxide in the hydrophobic film has a photocatalytic effect, and can decompose organic pollutants attached to the hydrophobic film under the irradiation of sunlight, so that the cleaning performance is obtained, the attachment amount of the organic pollutants is small, and C-F bonds in organic fluorides have high stability and slow decomposition speed, so that the hydrophobic film can keep the hydrophobic effect for a long time, and when the rainy day comes, rainwater can quickly take away inorganic matters on the surface of the hydrophobic film, so that the glass is bright as new.
5. The component B can be used as a cleaning agent diluted by 50 times with water, and because the copolymer exists in the component B, when the cleaning agent is used for cleaning, water can purchase dust on the surface of a hydrophobic membrane, and when the solvent damages the surface of the hydrophobic membrane, the copolymer, titanium oxide and other substances in the component B can be attached to the surface of the original hydrophobic membrane, so that a new hydrophobic layer can be formed on the surface of the hydrophobic membrane after the solvent is volatilized, the service life of the hydrophobic membrane is prolonged, and the self-cleaning effect is improved.
6. The tetramethylammonium hydroxide is decomposed into trimethylamine and dimethyl ether at 135-140 ℃, and the tetramethylammonium hydroxide plays an important role as an alkaline catalyst for polymerization reaction. Acid neutralization is not needed, and no waste water is generated.
Detailed Description
The technical solutions in the examples will be clearly and completely described below. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Example 1
A self-cleaning glass hydrophobic agent is prepared by the following steps:
s1, preparing the component A, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to a proportion, mixing and stirring uniformly, and heating to 80 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 3 hours at the temperature of 140-145 ℃ and the stirring speed of 30-60 rpm, carrying out polymerization reaction to obtain ternary copolysiloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component A;
the substances and the contents of the raw materials in the component A are shown in the table 1, and the unit of the content of each component is g;
the dimethyl cyclosiloxane is octamethylcyclotetrasiloxane;
the phenyl-containing siloxane comprises octaphenylcyclotetrasiloxane, tetramethyltetraphenylcyclotetrasiloxane, short-chain dimethyl diphenyl siloxane and short-chain methyl phenyl siloxane in a weight ratio of 1: 2: 1: 3;
the silane coupling agent is N-beta- (aminoethyl) -gamma-aminopropyl methyl trimethoxy silane;
tetramethyl ammonium hydroxide as basic catalyst;
the surfactant comprises nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether, and the weight ratio is 2: 1: 3;
the solvent is ethanol;
the nano particles are nano silicon dioxide;
s2, preparing the component B, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to the proportion, mixing and stirring uniformly, and heating to 80 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 3 hours at the temperature of 140-145 ℃ and the stirring speed of 30rpm, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component B;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the organic fluoride is tridecafluorooctyltriethoxysilane; the types of the silane coupling agent, the dimethyl cyclosiloxane, the methyl phenyl siloxane, the alkaline catalyst and the solvent are consistent with the component A, and the particle size of the nano titanium oxide is 20-50 nm;
the surfactant is F4432 nonionic fluorine-containing compound surfactant;
in steps S1 and S2, the polymerization conditions are as follows: the stirring speed is 60rpm, the temperature is 135-150 ℃, and the reaction time is 3 h.
Example 2
A self-cleaning glass hydrophobic agent is prepared by the following steps:
s1, preparing the component A, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to a proportion, mixing and stirring uniformly, and heating to 90 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 5 hours at 135-150 ℃ and at a stirring speed of 60rpm, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component A;
the substances and the contents of the raw materials in the component A are shown in the table 1, and the unit of the content of each component is g;
the dimethyl cyclosiloxane comprises octamethylcyclotetrasiloxane and dimethyl cyclosiloxane in a weight ratio of 1: 1;
the phenyl-containing siloxane comprises octaphenylcyclotetrasiloxane, tetramethyltetraphenylcyclotetrasiloxane, short-chain dimethyl diphenyl siloxane and short-chain methyl phenyl siloxane in a weight ratio of 2: 3: 1: 1;
the silane coupling agent is N-beta- (aminoethyl) -gamma-aminopropyl methyl trimethoxy silane;
tetramethyl ammonium hydroxide as basic catalyst;
the surfactant is nonylphenol polyoxyethylene ether;
the solvent is methanol, ethanol and isopropanol, and the weight ratio is 1: 1: 1;
the nano particles are nano zinc oxide;
s2, preparing the component B, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to the proportion, mixing and stirring uniformly, and heating to 90 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 5 hours at 135-145 ℃ and at a stirring speed of 60rpm, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component B;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the organic fluoride is triethyl- (trifluorovinyl) silane; the types of the silane coupling agent, the dimethyl cyclosiloxane, the phenyl siloxane, the alkaline catalyst and the solvent are consistent with the component A, and the particle size of the nano titanium oxide is 20-50 nm;
the surfactant is F4432 nonionic fluorine-containing compound surfactant;
in steps S1 and S2, the polymerization conditions are as follows: the stirring speed is 30rpm, the temperature is 125-145 ℃, and the reaction time is 5 hours.
Example 3
A self-cleaning glass hydrophobic agent is prepared by the following steps:
s1, preparing the component A, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to a proportion, mixing and stirring uniformly, and heating to 85 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 4 hours at the temperature of 125-140 ℃ and the stirring speed of 45rpm, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component A.
The substances and the contents of the raw materials in the component A are shown in the table 1, and the unit of the content of each component is g;
the dimethyl cyclosiloxane comprises octamethylcyclotetrasiloxane and dimethyl cyclosiloxane in a weight ratio of 1: 4;
the phenyl-containing siloxane comprises octaphenylcyclotetrasiloxane, tetramethyltetraphenylcyclotetrasiloxane, short-chain dimethyl diphenyl siloxane and short-chain methyl phenyl siloxane, and the weight ratio of the octaphenylcyclotetrasiloxane to the tetramethyltetraphenylcyclotetrasiloxane is 4: 4: 1: 1;
the silane coupling agent is N-beta- (aminoethyl) -gamma-aminopropyl methyl trimethoxy silane;
tetramethyl ammonium hydroxide as basic catalyst;
the surfactant comprises nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether, and the weight ratio is 1: 1: 1;
the solvent comprises acetonitrile and acetone, and the weight ratio is 1: 1;
the nano particles are nano silicon dioxide and nano zinc oxide, and the weight ratio is 1: 1;
s2, preparing the component B, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to the proportion, mixing and stirring uniformly, and heating to 85 ℃ to obtain a hot material; continuously adding an alkaline catalyst into the hot material within 4 hours at the temperature of 125-140 ℃ and the stirring speed of 45rpm, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component B;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the organic fluoride comprises tridecafluorooctyltriethoxysilane, 4-methyl-tridecafluorodecyltriethoxysilane, heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltriisopropoxysilane, heptadecafluorodecyltripropoxysilane, triethyl- (trifluorovinyl) silane, nonafluorohexyldimethylchlorosilane in a weight ratio of 1: 2: 3: 1: 2: 3: 1; the types of the silane coupling agent, the dimethyl cyclosiloxane, the phenyl siloxane, the alkaline catalyst and the solvent are consistent with the component A, and the particle size of the nano titanium oxide is 20-50 nm;
the surfactant is F4432 nonionic fluorine-containing compound surfactant;
in steps S1 and S2, the polymerization conditions are as follows: the stirring speed is 45rpm, the temperature is 130-145 ℃, and the reaction time is 4 hours.
Example 4
The preparation steps of the self-cleaning glass hydrophobic agent are the same as those of the example 1.
The substances and the contents of the raw materials in the component A are shown in the table 1, and the unit of the content of each component is g;
the dimethyl cyclosiloxane comprises octamethylcyclotetrasiloxane and dimethyl cyclosiloxane in a weight ratio of 3: 1;
the phenyl-containing siloxane comprises octaphenylcyclotetrasiloxane, tetramethyltetraphenylcyclotetrasiloxane, short-chain dimethyl diphenyl siloxane and short-chain methyl phenyl siloxane in a weight ratio of 1: 1: 1: 1;
the silane coupling agent is N-beta- (aminoethyl) -gamma-aminopropyl methyl trimethoxy silane;
tetramethyl ammonium hydroxide as basic catalyst;
the surfactant is isomeric tridecanol polyoxyethylene ether;
the solvent is acetone;
the nano particles are nano silicon dioxide;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the organic fluoride comprises tridecafluorooctyltriethoxysilane, 4-methyl-tridecafluorodecyltriethoxysilane, heptadecafluorodecyltriethoxysilane, heptadecafluorodecyltriisopropoxysilane, heptadecafluorodecyltripropoxysilane, triethyl- (trifluorovinyl) silane, nonafluorohexyldimethylchlorosilane in a weight ratio of 1: 2: 3: 1: 2: 3: 1; the types of the silane coupling agent, the dimethyl cyclosiloxane, the phenyl siloxane, the alkaline catalyst and the solvent are consistent with the component A;
the surfactant is F4432 nonionic fluorine-containing compound surfactant;
the particle size of the nano titanium oxide is 20-50 nm.
Example 5
The preparation steps of the self-cleaning glass hydrophobic agent are the same as those in the embodiment 1;
the substances and the contents of the raw materials in the component A are shown in the table 1, and the unit of the content of each component is g; the difference from example 1 is that:
the silane coupling agent is 1, 2-bis (triethoxysilyl) ethane;
the alkaline catalyst is potassium hydroxide;
the surfactant comprises nonylphenol polyoxyethylene ether, perfluoro-1-butanesulfonic acid and isomeric tridecanol polyoxyethylene ether, and the weight ratio is 1: 2: 4;
no nanoparticles are contained;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the difference from example 1 is that:
the silane coupling agent is 1, 2-bis (triethoxysilyl) ethane;
the alkaline catalyst is potassium hydroxide;
the surfactant comprises nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and isomeric tridecanol polyoxyethylene ether, and the weight ratio is 1: 2: 1;
the particle size of the nano titanium oxide is 50-100 nm.
Example 6
The preparation procedure of a self-cleaning glass hydrophobing agent is the same as that of example 2.
The substances and the contents of the raw materials in the component A are shown in the table 1, the unit of the content of each component is g, and the difference from the example 2 is that:
the alkaline catalyst is potassium hydroxide;
the surfactant comprises nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene ether and perfluoro-1-butanesulfonic acid, and the weight ratio is 1: 2: 5;
no nanoparticles are contained;
the substances and the contents of the raw materials in the component B are shown in Table 2, and the unit of the content of each component is g; the difference from example 2 is that:
the silane coupling agent is 1, 2-bis (triethoxysilyl) ethane;
the alkaline catalyst is potassium hydroxide;
the surfactant is F4432 nonionic fluorine-containing compound surfactant;
does not contain nano titanium oxide.
TABLE 1 substances and amounts in component A
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Dimethylcyclosiloxane | 100 | 100 | 100 | 100 | 100 | 100 |
| Containing phenylsiloxane | 21 | 30 | 49 | 25 | 30 | 50 |
| Silane coupling agent | 5 | 7.5 | 10 | 6 | 8 | 9 |
| Basic catalyst | 1 | 0.8 | 0.5 | 1 | 0.3 | 0.1 |
| Surface active agent | 6 | 13 | 20 | 15 | 40 | 30 |
| Solvent(s) | 90 | 30 | 60 | 70 | 10 | 50 |
| Nanoparticles | 10 | 15 | 20 | 5 | 0 | 0 |
Table 2B Components, substances and amounts
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Organofluoro compounds | 80 | 80 | 80 | 80 | 80 | 80 |
| Silane coupling agent | 15 | 8 | 12 | 10 | 6 | 4 |
| Dimethylcyclosiloxane | 10 | 30 | 13 | 18 | 25 | 20 |
| Containing phenylsiloxane | 20 | 10 | 15 | 12 | 15 | 18 |
| Basic catalyst | 10 | 8 | 5 | 10 | 3 | 0.1 |
| Surface active agent | 6 | 13 | 20 | 15 | 40 | 30 |
| Solvent(s) | 90 | 30 | 60 | 70 | 10 | 50 |
| Nano titanium oxide | 15 | 20 | 5 | 10 | 1 | 0 |
Comparative example 1
The lotus leaf hydrophobing agent is purchased from Taida chemical Co., Ltd, Taida, Librarian ceramic county, and has the model of LC-808.
Comparative example 2
An automobile glass coating agent which is purchased from Henghui nano science and technology Limited and has the model of PV-30000.
Performance testing
The products prepared in examples 1 to 6 and the products of comparative examples 1 to 2 were subjected to the following tests:
experiment 1, contact angle test: glass sheets were prepared into 10 × 10cm standard blocks 1 to 8, which corresponded to examples 1, 2, 3, 4, 5, 6, 1 and 2 in this order, and after washing the glass with 1 part of 2% by mass hydrochloric acid, 30 parts of water were added to rinse it clean, and after drying, the contact angle before treatment was measured with reference to the GB/T31815-15 standard.
Experiment 2, samples 1 to 6 after the test were sprayed with 20ml of the component a corresponding to the components in examples 1, 2, 3, 4, 5 and 6 in this order, and after the spontaneous combustion drying, the samples 7 to 8 after the test were sprayed with 40ml of the component B corresponding to the products in comparative examples 1, 2, 3, 4, 5 and 6, and after the test, the contact angle was measured according to the GB/T31815-15 standard after drying the samples 1 to 8.
Experiment 3, impact 1-8 standard sample blocks with 100g of active clay with 300 meshes from a height of 30cm within 3min, wash with water, dry, and test the friction contact angle.
Experiment 4, samples 1 to 6 after the treatment of experiment 3 were spray-treated corresponding to the component B in examples 1, 2, 3, 4, 5 and 6, with a spray amount of 20ml, and samples 7 to 8 after the treatment of experiment 3 were spray-treated corresponding to examples 1 and 2, with a spray amount of 20ml, and the secondary treatment contact angles were measured with reference to the GB/T31815-15 standard.
Experiment 5, the visible light transmittance was tested with reference to GB/T2680-94 standard.
The test results are shown in table 3.
Table 3 results of performance testing
According to the experimental data, after the product prepared by the invention is used for treating the surface of glass, an effective hydrophobic layer can be formed on the surface of the glass, the contact angle can reach more than 125 degrees, and water drops can naturally fall off without being attached to the glass to influence the sight. The hydrophobic cleaning agent has strong resistance to dust and good dust resistance, can achieve good hydrophobic effect without special treatment after secondary use, can be directly used as a cleaning agent after primary film formation, and does not need special treatment.
Claims (2)
1. The application of the self-cleaning glass hydrophobic agent is characterized in that the preparation method of the self-cleaning glass hydrophobic agent comprises the following steps:
s1, preparing the component A, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to a proportion, mixing and stirring uniformly, and heating to 80-90 ℃ to obtain a heating material; the hot material also comprises nano particles, wherein the nano particles are one or two of nano silicon dioxide and nano zinc oxide; adding tetramethyl ammonium hydroxide serving as an alkaline catalyst into the hot material, stirring at the stirring speed of 30-60 rpm at the temperature of 125-150 ℃, reacting for 3-5 hours, carrying out polymerization reaction to obtain ternary polymerization siloxane, cooling to room temperature, adding a surfactant, uniformly mixing, adding a solvent, emulsifying, and filtering to obtain a component A;
s2, preparing the component B, weighing dimethyl cyclosiloxane, phenyl siloxane and a silane coupling agent according to the proportion, mixing and stirring uniformly, and heating to obtain a hot material; adding tetramethyl ammonium hydroxide serving as an alkaline catalyst into a hot material, stirring at the stirring speed of 30-60 rpm for 3-5 hours at the temperature of 125-150 ℃, carrying out polymerization reaction to obtain terpolymer siloxane, cooling to room temperature, adding a surfactant and nano titanium oxide, wherein the particle size of the nano titanium oxide is 20-50 nm, uniformly mixing, adding a solvent for emulsification, and filtering to obtain a component B;
spraying the prepared component A on the surface of glass, drying to form a reference film, spraying the prepared component B on the reference film, and drying to form a hydrophobic film;
the component B can be used as a cleaning agent after being diluted by 50 times with water.
2. Use of a hydrophobic agent for self-cleaning glass according to claim 1, wherein the component B according to claim 1 is sprayed onto the hydrophobic film to form a new hydrophobic layer.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1778749A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Glass hydrophobic film coating liuqid |
| DE102005013857A1 (en) * | 2005-03-24 | 2006-09-28 | Schott Ag | Antibacterial coating article, process for its preparation and its use |
| JP2007076940A (en) * | 2005-09-13 | 2007-03-29 | Ishizuka Glass Co Ltd | Water-repellent glass material and its manufacturing method |
| CN101148325A (en) * | 2007-09-06 | 2008-03-26 | 北京首创纳米科技有限公司 | Nano protecting liquid used for glass and preparation method thereof |
| CN101333078A (en) * | 2008-08-05 | 2008-12-31 | 广州市白云化工实业有限公司 | Fluorosilicate self-cleaning glass nanophase material and producing method thereof |
| CN102950843A (en) * | 2012-11-29 | 2013-03-06 | 大连创达技术交易市场有限公司 | Automotive glass with anti-fog and self-cleaning functions |
| CN105347693A (en) * | 2014-08-22 | 2016-02-24 | 北京易净星科技有限公司 | Long-acting glass hydrophobic agent and preparation and application method thereof |
| CN105524279A (en) * | 2015-11-26 | 2016-04-27 | 杭州师范大学 | Preparation method for heat-conducting methylphenyl silicone oil |
| CN106380588A (en) * | 2016-08-31 | 2017-02-08 | 湖北新四海化工股份有限公司 | Oil-displacement organosilicon surfactant and preparation method thereof |
| CN106398523A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | Organosilicon coating agent and preparation method thereof |
-
2019
- 2019-01-11 CN CN201910028051.8A patent/CN109678359B/en active Active
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE102005013857A1 (en) * | 2005-03-24 | 2006-09-28 | Schott Ag | Antibacterial coating article, process for its preparation and its use |
| JP2007076940A (en) * | 2005-09-13 | 2007-03-29 | Ishizuka Glass Co Ltd | Water-repellent glass material and its manufacturing method |
| CN1778749A (en) * | 2005-10-14 | 2006-05-31 | 浙江大学 | Glass hydrophobic film coating liuqid |
| CN101148325A (en) * | 2007-09-06 | 2008-03-26 | 北京首创纳米科技有限公司 | Nano protecting liquid used for glass and preparation method thereof |
| CN101333078A (en) * | 2008-08-05 | 2008-12-31 | 广州市白云化工实业有限公司 | Fluorosilicate self-cleaning glass nanophase material and producing method thereof |
| CN102950843A (en) * | 2012-11-29 | 2013-03-06 | 大连创达技术交易市场有限公司 | Automotive glass with anti-fog and self-cleaning functions |
| CN105347693A (en) * | 2014-08-22 | 2016-02-24 | 北京易净星科技有限公司 | Long-acting glass hydrophobic agent and preparation and application method thereof |
| CN105524279A (en) * | 2015-11-26 | 2016-04-27 | 杭州师范大学 | Preparation method for heat-conducting methylphenyl silicone oil |
| CN106380588A (en) * | 2016-08-31 | 2017-02-08 | 湖北新四海化工股份有限公司 | Oil-displacement organosilicon surfactant and preparation method thereof |
| CN106398523A (en) * | 2016-08-31 | 2017-02-15 | 湖北新四海化工股份有限公司 | Organosilicon coating agent and preparation method thereof |
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