CN117209161A - Preparation method of ash-resistant easy-to-clean glass - Google Patents
Preparation method of ash-resistant easy-to-clean glass Download PDFInfo
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- CN117209161A CN117209161A CN202310966132.9A CN202310966132A CN117209161A CN 117209161 A CN117209161 A CN 117209161A CN 202310966132 A CN202310966132 A CN 202310966132A CN 117209161 A CN117209161 A CN 117209161A
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- easy
- coating material
- glass
- ash
- clean glass
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- 239000011521 glass Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 230000003670 easy-to-clean Effects 0.000 title claims abstract description 18
- 239000011248 coating agent Substances 0.000 claims abstract description 56
- 238000000576 coating method Methods 0.000 claims abstract description 56
- 239000000463 material Substances 0.000 claims abstract description 41
- 238000004140 cleaning Methods 0.000 claims abstract description 27
- 239000000758 substrate Substances 0.000 claims abstract description 22
- UQZIWOQVLUASCR-UHFFFAOYSA-N alumane;titanium Chemical compound [AlH3].[Ti] UQZIWOQVLUASCR-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002131 composite material Substances 0.000 claims abstract description 19
- 239000007822 coupling agent Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 11
- 230000003301 hydrolyzing effect Effects 0.000 claims abstract description 7
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 41
- 239000000203 mixture Substances 0.000 claims description 23
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 17
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 claims description 17
- 230000002209 hydrophobic effect Effects 0.000 claims description 12
- 230000004048 modification Effects 0.000 claims description 11
- 238000012986 modification Methods 0.000 claims description 11
- 239000004071 soot Substances 0.000 claims description 10
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 229910052710 silicon Inorganic materials 0.000 claims description 8
- 239000010703 silicon Substances 0.000 claims description 8
- 229920003209 poly(hydridosilsesquioxane) Polymers 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 238000006555 catalytic reaction Methods 0.000 claims description 4
- -1 cyclic siloxane Chemical class 0.000 claims description 4
- 238000009832 plasma treatment Methods 0.000 claims description 3
- 229920001296 polysiloxane Polymers 0.000 claims description 3
- 238000013329 compounding Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 13
- 239000002245 particle Substances 0.000 description 10
- 229910002706 AlOOH Inorganic materials 0.000 description 7
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 7
- 229910010275 TiOOH Inorganic materials 0.000 description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- 230000003373 anti-fouling effect Effects 0.000 description 6
- 230000007062 hydrolysis Effects 0.000 description 6
- 238000006460 hydrolysis reaction Methods 0.000 description 6
- 239000000428 dust Substances 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 238000005299 abrasion Methods 0.000 description 4
- 229910010413 TiO 2 Inorganic materials 0.000 description 3
- 239000002052 molecular layer Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000006258 conductive agent Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- DBGSRZSKGVSXRK-UHFFFAOYSA-N 1-[2-[5-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]-1,3,4-oxadiazol-2-yl]acetyl]-3,6-dihydro-2H-pyridine-4-carboxylic acid Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C1=NN=C(O1)CC(=O)N1CCC(=CC1)C(=O)O DBGSRZSKGVSXRK-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention provides a preparation method of anti-ash easy-cleaning glass, which is prepared by hydrolyzing and hydrophobically modifying the existing aluminum-titanium composite coupling agent to prepare a coating material, coating the coating material on the surface of a glass substrate, and drying and curing. The process of directly applying the existing aluminum-titanium composite coupling agent to the coating material of the easy-to-clean glass after simple treatment can prepare the anti-ash easy-to-clean glass with coating stability, self-cleaning property and ash resistance only through a simple treatment process, and has the advantages of simplicity and high efficiency compared with the mode of preparing the coating material by compounding various raw materials in the prior art.
Description
Technical Field
The invention relates to the technical field of preparation methods of anti-ash easy-to-clean glass, in particular to a preparation method of anti-ash easy-to-clean glass.
Background
The easy-to-clean glass is characterized in that after a layer of special paint is coated on the surface of the glass, dust or dirty liquid is difficult to adhere to the surface of the glass, so that the surface of the glass can be kept clean, and the trouble of cleaning the surface of the glass is reduced.
In the prior art, the application number is CN202010743993.7, the publication date is 2020, and the application number is 27, namely a long-acting self-cleaning composition for glass surface is provided in the patent application document, which utilizes 0.5-5 parts of nano titanium dioxide, 1-10 parts of nano silicon dioxide mixture, 0.1-5 parts of inorganic sol, 0.001-0.01 part of conductive agent, 0.01-0.1 part of metal salt, 0.01-2 parts of catalyst, 0.01-1 part of acid and 80-99 parts of solvent to be compounded, the self-cleaning capability of the composition is endowed by adding the conductive agent and titanium dioxide, and the defect of light dependence when the titanium dioxide is used as a self-cleaning coating in the prior art is overcome. However, the composition for self-cleaning in the above technical scheme has the defects of complex composition and difficult control of the manufacturing process.
In view of the foregoing, there is a need for an improved method for preparing an ash resistant easy-to-clean glass.
Disclosure of Invention
The invention aims to provide a preparation method of ash-resistant easy-to-clean glass.
In order to achieve the aim, the invention provides a preparation method of the anti-ash easy-cleaning glass, which is prepared by coating a coating material on the surface of a glass substrate and drying and curing the coating material;
the preparation of the coating material comprises the following steps:
s1, under the catalysis of ammonia water, hydrolyzing an aluminum-titanium composite coupling agent in an isopropanol solution to obtain a mixture of aluminum hydroxide sol and titanium hydroxide sol;
s2, adding organic silicon into the mixture obtained in the step S1 to carry out hydrophobic modification on the mixture, thereby obtaining the coating material.
Preferably, in step S1, the concentration of the isopropyl alcohol solution is 5-30%, and the addition amount of the isopropyl alcohol solution is 5-50%.
Preferably, in step S2, the organosilicon is an organohydrogen cyclic siloxane.
Preferably, the silicone is a methyl-hydrogen-cyclic siloxane or a hydrogen silsesquioxane.
Preferably, the methyl-hydrogen-cyclic siloxane is added in an amount of 1 to 3 times the volume of the aluminum-titanium composite coupling agent.
Preferably, the hydrogen silsesquioxane is added in an amount of 15-30%.
Preferably, the curing temperature is 200-300 ℃.
Preferably, the surface of the glass substrate is pre-treated before the coating material is applied to the surface of the glass substrate.
Preferably, the pretreatment is a plasma treatment.
The beneficial effects of the invention are as follows:
1. the preparation method of the anti-ash easy-cleaning glass comprises the steps of preparing a coating material by hydrolyzing and hydrophobically modifying the existing aluminum-titanium composite coupling agent, coating the coating material on the surface of a glass substrate, and drying and solidifying the coating material; in the process, the mixture of the aluminum hydroxide sol and the titanium hydroxide sol containing the nano AlOOH/TiOOH particles can be obtained through hydrolysis, and the nano AlOOH/TiOOH particles are combined with active hydroxyl groups on the surface of the glass matrix, and are dehydrated to form Al in the curing process of drying and curing 2 O 3 /TiO 2 The particle layer can block pores on the surface of the glass and form a compact nano layer on the surface of the glass, so that the glass substrate is endowed with excellent antifouling property and self-cleaning capability; and secondly, the organic silicon introduced during hydrophobic modification can chemically react with active hydroxyl groups on the surfaces of the nano AlOOH/TiOOH particles at high temperature to form firm chemical covalent bonds, so that the bonding force between the coating and glass is effectively enhanced, the stability of the coating is ensured, and meanwhile, the hydrophobic silane groups are introduced, so that the coating material has hydrophobicity, and the anti-fouling capability of a glass substrate is improved.
2. The preparation method of the anti-ash easy-cleaning glass provided by the invention has the advantages that the existing aluminum-titanium composite coupling agent is directly applied to the coating material of the easy-cleaning glass after being simply treated, and the anti-ash easy-cleaning glass with coating stability, self-cleaning property and anti-ash property can be prepared only through a simple treatment process, so that the preparation method has the advantages of simplicity and high efficiency compared with the mode of preparing the coating material by compounding various raw materials in the prior art.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to specific embodiments.
It should also be noted herein that the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention provides a preparation method of anti-ash easy-cleaning glass, which is prepared by coating a coating material on a glass substrate, and drying and curing at 200-300 ℃; in order to make the bonding force between the glass substrate and the coating material stronger, the glass substrate needs to be pretreated by plasma treatment and other modes before coating so as to lead the surface of the glass substrate to carry active hydroxyl groups.
Specifically, the preparation of the coating material comprises the following steps:
s1, under the catalysis of ammonia water, hydrolyzing an aluminum-titanium composite coupling agent in an isopropanol solution to obtain a mixture of aluminum hydroxide sol and titanium hydroxide sol;
s2, adding organic silicon into the mixture of the aluminum hydroxide sol and the titanium hydroxide sol obtained in the step S1 to carry out hydrophobic modification on the mixture, thereby obtaining the coating material.
Preferably, in the step S1, the concentration of the isopropanol solution is 5-30%, the addition amount is 5-50%, and the addition amount is the percentage of the added isopropanol solution in the whole system, and the effective components in the isopropanol solution can determine the content of the aluminum hydroxide sol and the titanium hydroxide sol obtained after the hydrolysis of the aluminum-titanium composite coupling agent; the content of the aluminum hydroxide sol and the titanium hydroxide sol in the mixture of the aluminum hydroxide sol and the titanium hydroxide sol is 35-55%, and the sum of the content of the aluminum hydroxide sol and the titanium hydroxide sol is 100%.
Preferably, in step S2, the organosilicon is an organohydrogen cyclic siloxane, in particular a methyl-hydrogen-cyclic siloxane or a hydrogen silsesquioxane; the organosilicon is methyl-hydrogen-cyclic siloxane, and the addition amount is 1-3 times of the volume of the aluminum-titanium composite coupling agent; when the organosilicon is hydrogen silsesquioxane, the addition amount is 15-30%, and the addition amount is the percentage of the organosilicon in the whole system; the aluminum-titanium composite coupling agent in the scheme is a commercially available product, and the model is LT-1.
The preparation method of the ash-resistant easy-to-clean glass of the invention is further described below with reference to specific examples:
example 1
The anti-ash easy-cleaning glass is prepared by coating a coating material on the surface of a glass substrate and drying and curing at 100-300 ℃.
Further, the preparation of the coating material comprises the following steps:
s1, under the catalysis of ammonia water, hydrolyzing an aluminum-titanium composite coupling agent in an isopropanol solution to obtain a mixture of aluminum hydroxide sol and titanium hydroxide sol; wherein, the concentration of the isopropanol solution is 30 percent, and the addition amount is 50 percent;
s2, adding 70% of the aluminum hydroxide sol and titanium hydroxide sol mixture in the step S1. To hydrophobically modify the above mixture to obtain a coating material.
In order to explore the performance of the anti-ash easy-cleaning glass prepared by the embodiment, the following method is adopted for testing, and the specific testing method is as follows: after wiping the surface of the glass with lint for 5000 times, comparing the retention degree of the coating material on the surface of the glass after wiping to evaluate the abrasion resistance of the glass; coating colored articles such as a mark pen, a lipstick and the like on the surface of the glass, and wiping stains on the surface of the glass after drying at room temperature so as to evaluate the self-cleaning property of the glass; to evaluate the glass's resistance to ash, the glass was placed in a dust-containing environment and the dust on the surface of the glass was wiped over time, and the glass's resistance to ash was evaluated for ease of wiping, and each performance was distinguished by excellent, good, general, and poor grades.
Examples 2 to 5
Examples 2 to 5 differ from example 1 only in that: in the preparation process of the coating material, the concentration and the addition amount of the isopropanol solution are different, and other steps are basically the same as those of the embodiment 1, and are not repeated here. The settings of the concentration and addition amount of the isopropyl alcohol solution and the properties of the ash-resistant easy-to-clean glass produced under the corresponding conditions in examples 1 to 5 are shown in table 1, and it can be seen from the data in the table that when the concentration of isopropyl alcohol is 30%, the produced ash-resistant easy-to-clean glass can exhibit excellent abrasion resistance, self-cleaning property and ash absorption resistance because: when isopropanol solution with proper concentration is added, the product obtained by hydrolysis of the aluminum-titanium composite coupling agent can be ensured to contain enough aluminum hydroxide sol and titanium hydroxide sol, so that the glass substrate and the coating material are combined together by utilizing the acting force of the aluminum hydroxide sol and the titanium hydroxide sol and the surface of the glass substrate after subsequent hydrophobic modification.
TABLE 1 setting of concentration and addition amount of isopropyl alcohol solution in examples 1 to 5 and Properties of anti-Gray and easy-to-clean glass produced under corresponding conditions
Examples 6 to 7
Examples 6 to 7 differ from example 1 only in that: in step S1, the amount of the organosilicon added in the hydrophobic modification process is different from that in example 1, and other steps are substantially the same as those in example 1, and will not be described here. The addition of the organic silicon in examples 1 and 6 to 7 and the properties of the anti-dust easy-cleaning glass prepared under the corresponding conditions are shown in table 2, and it can be seen from the data in the table that the addition of a proper amount of organic silicon can endow the mixture of aluminum hydroxide sol and titanium hydroxide sol with certain hydrophobicity, so that the coating material has the anti-dust and self-cleaning properties.
TABLE 2 Properties of the Ash resistant easy-to-clean glass obtained under the corresponding conditions in example 1 and examples 6 to 7 in which the amount of the organic silicon added
Project | Organosilicon addition (%) | Abrasion resistance | Self-cleaning property | Resistance to ash |
Example 1 | 30 | Excellent and excellent properties | Excellent and excellent properties | Excellent and excellent properties |
Example 6 | 15 | In general | Good (good) | Good (good) |
Example 7 | 20 | Good (good) | Good (good) | Good (good) |
Comparative example 1
Comparative example 1 differs from example 1 in that: the aluminum-titanium composite coupling agent is directly used as a coating material without hydrolysis and hydrophobic modification treatment, and other steps are basically the same as those of the embodiment 1, and are not repeated here.
Comparative example 2
Comparative example 2 differs from example 1 in that: only the aluminum-titanium composite coupling agent is subjected to hydrolysis treatment, but not hydrophobic modification treatment, and other steps are basically the same as those of example 1, and are not repeated here.
Comparative example 3
Comparative example 3 differs from example 1 in that: the coating material is not prepared by using the aluminum-titanium composite coupling agent, but the directly prepared mixture of the aluminum hydroxide sol and the titanium hydroxide sol is subjected to hydrophobic modification to be used as the coating material, the content of the aluminum hydroxide sol and the titanium hydroxide sol in the coating material in the comparative example is the same as that in the example 1, other steps are basically the same as that in the example 1, and no repeated description is provided. The properties of the anti-soot easy-clean glasses prepared in example 1 and comparative examples 1 to 3 are shown in Table 3, and it can be seen from the data in the table that the anti-soot easy-clean glass prepared by the method of the present invention has more excellent properties because: in the coating material prepared by the method of hydrolyzing and hydrophobically modifying the aluminum-titanium composite coupling agent, nano AlOOH or TiOOH particles in sol of the mixture obtained by hydrolysis are combined with glass surface active hydroxyl groups, and are dehydrated to form Al in the process of drying and curing 2 O 3 Or TiO 2 The particle layer can effectively block capillary pores on the surface of the glass and form a compact nano layer on the surface of the glass, so that the glass is endowed with anti-fouling and easy-cleaning properties, and is effectively mildew-proof and anti-fouling; on the other hand, in the drying and curing process, hydrogen-containing cyclic siloxane and active hydroxyl on the surfaces of the nano particles are subjected to chemical reaction to form very firm chemical covalent bonds, so that the binding force between the glass substrate and the coating material is effectively enhanced, and the stability between the coating material and the glass substrate is ensured; in contrast, in comparative examples 1 to 3, the above-mentioned several effects were not present, and the coating material was merely deposited on the surface of the glass substrate and bonded together by electrostatic adsorption therebetween, so that the stability was inferior to that of example 1.
TABLE 3 Properties of the anti-Gray easy-to-clean glasses prepared in example 1 and comparative examples 1 to 3
Project | Abrasion resistance | Self-cleaning property | Resistance to ash |
Example 1 | Excellent and excellent properties | Excellent and excellent properties | Excellent and excellent properties |
Comparative example 1 | Difference of difference | Difference of difference | Difference of difference |
Comparative example 2 | Difference of difference | Difference of difference | Difference of difference |
Comparative example 3 | Difference of difference | Difference of difference | Difference of difference |
In conclusion, the preparation method of the ash-resistant easy-to-clean glass provided by the invention can obtain the nano AlOOH/TiOOH particles through hydrolysisThe mixture of aluminium hydroxide sol and titanium hydroxide sol is combined with active hydroxyl on the surface of glass matrix by nanometer AlOOH/TiOOH particles, and is dehydrated to form Al in the solidification process of drying and solidification 2 O 3 /TiO 2 The particle layer can block pores on the surface of the glass and form a compact nano layer on the surface of the glass, so that the glass substrate is endowed with excellent antifouling property and self-cleaning capability; secondly, the organic silicon introduced during hydrophobic modification can chemically react with active hydroxyl groups on the surfaces of the nano AlOOH/TiOOH particles at high temperature to form firm chemical covalent bonds, so that the bonding force between the coating and glass is effectively enhanced, the stability of the coating is ensured, and meanwhile, hydrophobic silane groups are introduced, so that the coating material has hydrophobicity, and the anti-fouling capability of a glass substrate is improved; the coating material directly applied to the easy-to-clean glass after simple treatment of the existing aluminum-titanium composite coupling agent has the advantages of simplicity and high efficiency compared with the mode of preparing the coating material by compounding various raw materials in the prior art.
The above embodiments are only for illustrating the technical solution of the present invention and not for limiting the same, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications and equivalents may be made thereto without departing from the spirit and scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the anti-ash easy-cleaning glass is characterized in that the anti-ash easy-cleaning glass is prepared by coating a coating material on the surface of a glass substrate and then drying and curing;
the preparation of the coating material comprises the following steps:
s1, under the catalysis of ammonia water, hydrolyzing an aluminum-titanium composite coupling agent in an isopropanol solution to obtain a mixture of aluminum hydroxide sol and titanium hydroxide sol;
s2, adding organic silicon into the mixture obtained in the step S1 to carry out hydrophobic modification on the mixture, thereby obtaining the coating material.
2. The method for producing an anti-soot easy-clean glass according to claim 1, wherein in the step S1, the concentration of the isopropyl alcohol solution is 5 to 30%, and the addition amount of the isopropyl alcohol solution is 5 to 50%.
3. The method for producing an anti-soot easy-clean glass according to claim 1, wherein in step S2, the silicone is an organohydrogen cyclic siloxane.
4. A method of making an anti-soot easy-clean glass as in claim 3, wherein the silicone is a methyl-hydrogen-cyclic siloxane or a hydrogen silsesquioxane.
5. The method for producing an anti-soot easy-clean glass according to claim 4, wherein the addition amount of the methyl-hydrogen-cyclic siloxane is 1 to 3 times the volume of the aluminum-titanium composite coupling agent.
6. The method for producing an anti-soot easy-to-clean glass according to claim 4, wherein the hydrogen silsesquioxane is added in an amount of 15 to 30%.
7. The method for producing an anti-soot easy-clean glass according to claim 1, wherein the curing temperature is 200 to 300 ℃.
8. The method of producing an anti-soot easy-clean glass according to claim 1, wherein the surface of the glass substrate is subjected to pretreatment before the coating material is applied to the surface of the glass substrate.
9. The method for producing an anti-soot easy-clean glass according to claim 8, wherein the pretreatment is a plasma treatment.
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