Polysiloxane organic silicon elastic glass coating and preparation process thereof

Abstract

The invention discloses a polysiloxane organic silicon elastic glass coating and a preparation process thereof, and belongs to the technical field of organic silicon coatings. The preparation process of the glass coating comprises the following steps: uniformly mixing polysiloxane, organic silicon modified resin, a composite filler, a crosslinking aid, a catalyst, a coalescing agent and a solvent according to a raw material formula to obtain a film forming solution; and coating the film forming liquid on a glass substrate, curing and cooling to obtain the film. Wherein the organic silicon modified resin is prepared by carrying out a reaction on dicyclohexylmethane-4, 4 '-diisocyanate, polytetrahydrofuran ether glycol, polysilsesquioxane grafted hydroxypropyl silicone oil and a quaternary ammonium polymer containing a hydroxyl group; the composite filler is a mixture of molybdenum disulfide and aluminum oxide. The glass coating prepared by the invention not only has excellent adhesive force, salt fog resistance and stain resistance, but also has good wear resistance and weather aging resistance.

Description

Technical Field

[0001] The invention belongs to the technical field of organosilicon coatings, and in particular relates to a polysiloxane organosilicon elastic glass coating and a preparation process thereof. Background Art

[0002] With the development of science and technology and the changes in market demand, the requirements for glass materials are no longer limited to transparency and mechanical strength, but also include decorative, safety, durability and other aspects. As a new type of coating material, silicone elastic glass coating can meet the diverse needs of different application scenarios with its excellent weather resistance, corrosion resistance, salt spray resistance and good high and low temperature adaptability. This coating is made of silicone polymer as a film-forming material through a special process. It can not only effectively enhance the safety performance of glass and reduce the risk of breakage caused by accidental impact, but also provide a rich color selection as needed to enhance the visual effect. In addition, this coating also has excellent weather aging resistance and can maintain good physical and chemical stability even when exposed to harsh environments for a long time. For modern architectural design, the use of silicone elastic glass coating can significantly improve the appearance and safety factor of the building while reducing maintenance costs. In the automotive industry, the application of this coating can also increase the safety performance of the vehicle and give the body more possibilities for personalized design. With its unique advantages, silicone elastic glass coating plays an increasingly important role in various application fields.

[0003] Chinese patent CN108948881A discloses a nano thermal insulation coating for glass coating and a preparation method, comprising the following steps: mixing methyl methacrylate, solvent, nano semiconductor material composite, dispersant, and initiator for heating reaction, compounding with nano semiconductor material by high pressure spray drying, and then mixing with polysiloxane, amino resin, ethylene-vinyl acetate copolymer, glass powder, nano silicon dioxide, thickening and leveling agent, and water; the coating prepared by this patent has strong adhesion and good thermal insulation when used for glass coating, but the weather resistance and corrosion resistance of the coating need to be improved. Chinese patent CN104673090A discloses a novel nano self-cleaning coating and nano self-cleaning glass containing the coating formed by the coating, wherein the coating comprises the following components: polysiloxane, silicon dioxide nanoparticles, anatase titanium dioxide, nanoporogen and solvent, wherein the polysiloxane is selected from linear polysiloxane or branched polysiloxane; when the coating described in the patent is used for glass coating, it has high light transmittance, anti-fogging and self-cleaning ability, but the heat resistance and weathering resistance of the coating need to be improved. Therefore, it is urgent to develop a polysiloxane silicone elastic glass coating with excellent comprehensive performance. Summary of the invention

[0004] In view of the shortcomings of the prior art, the present invention provides a polysiloxane organosilicon elastic glass coating, which further improves the wear resistance, weathering resistance and antibacterial performance of the glass coating by adding organosilicon modified resin and composite filler for synergistic effect.

[0005] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0006] 20-40 parts by weight of polysiloxane, 5-10 parts by weight of organosilicon modified resin, 1-4 parts by weight of composite filler, 1-3 parts by weight of crosslinking aid, 0.2-0.4 parts by weight of catalyst, 0.1-0.3 parts by weight of film-forming aid, and 100-150 parts by weight of solvent.

[0007] Preferably, the polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 30,000-50,000 mPa·s (25° C.).

[0008] Preferably, the composite filler is a mixture of molybdenum disulfide and aluminum oxide.

[0009] Preferably, the weight ratio of molybdenum disulfide to aluminum oxide is 1-2:1; wherein the average particle size of molybdenum disulfide and aluminum oxide is 0.1-1 μm.

[0010] Preferably, the organosilicon modified resin is prepared by the following method:

[0011] Dicyclohexylmethane-4,4'-diisocyanate, polytetramethylene glycol, polysilsesquioxane-grafted hydroxypropyl silicone oil and hydroxyl-containing quaternary ammonium polymer are added to N-methylpyrrolidone, heated under a nitrogen atmosphere, and then dibutyltin dilaurate is added to react. After the reaction is completed, it is distilled under reduced pressure to obtain a silicone modified resin.

[0012] Preferably, the preparation method of the polysilsesquioxane grafted hydroxypropyl silicone oil is as follows: PSS-allyl-heptaisobutyl substitution and hydroxypropyl silicone oil are added to N-methylpyrrolidone, heated under a nitrogen atmosphere, and then a Custer catalyst is added for reaction. After the reaction is completed, reduced pressure distillation is performed to obtain polysilsesquioxane grafted hydroxypropyl silicone oil. In this process, the unsaturated bonds contained in the PSS-allyl-heptaisobutyl substitution are successfully grafted into a cage structure through the silicon-hydrogen bond addition reaction of the hydroxypropyl silicone oil, thereby obtaining polysilsesquioxane grafted hydroxypropyl silicone oil, and the hydroxypropyl contained in it can react with the isocyanate group during the synthesis of the organosilicon modified resin to introduce it into the polyurethane elastomer, thereby enhancing the wear resistance and weathering resistance of the glass coating.

[0013] Preferably, the preparation method of the quaternary ammonium polymer containing hydroxyl group is as follows: acryloyloxyethyl dimethyl benzyl ammonium chloride, 2-methacryloyloxyethyl phosphorylcholine and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyl triethoxysilane are added to N-methyl pyrrolidone, heated under nitrogen atmosphere, and then benzoyl peroxide is added for reaction. After the reaction is completed, reduced pressure distillation is performed to obtain the quaternary ammonium polymer containing hydroxyl group. In this process, the unsaturated bonds contained in the three monomers of acryloyloxyethyl dimethyl benzyl ammonium chloride, 2-methacryloyloxyethyl phosphorylcholine and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyl triethoxysilane are polymerized under the action of an initiator to obtain a quaternary ammonium polymer. The cationic quaternary ammonium group can be adsorbed on the surface of the bacterial structure and penetrate therein, and the bacterial cell structure is destroyed by interfering with the life activities of the bacteria, thereby achieving the purpose of sterilization. The siloxane segment in the polymer can cooperate with other components to help improve the wear resistance and aging resistance of the glass coating.

[0014] The present invention further improves the wear resistance, aging resistance and antibacterial performance of the glass coating by adding a silicone modified resin prepared by reacting dicyclohexylmethane-4,4'-diisocyanate, polytetramethylene furan ether diol, polysilsesquioxane-grafted hydroxypropyl silicone oil and a quaternary ammonium polymer containing a hydroxyl group, and synergizing with the composite fillers of molybdenum disulfide and aluminum oxide, while maintaining good adhesion, salt spray resistance, water resistance, stain resistance and toughness.

[0015] In the preparation process of silicone-modified resin, first, the reaction between dicyclohexylmethane-4,4'-diisocyanate and polytetramethylene ether diol generates a polyurethane elastic segment with good flexibility and durability, which enhances the strength, toughness and impact resistance of the glass coating. When the polyurethane elastic segment is combined with a hydroxyl-containing quaternary ammonium polymer and polysilsesquioxane-grafted hydroxypropyl silicone oil, a complex three-dimensional network structure can be formed, further improving the overall stability and durability of the coating. Secondly, the introduction of polysilsesquioxane grafted hydroxypropyl silicone oil brings good wear resistance and weathering resistance to the coating. Due to its special nano-scale cage structure and surface activity, polysilsesquioxane can form a protective layer on the surface of the material, effectively preventing the invasion of moisture and other corrosive substances. At the same time, the grafted copolymer prepared by the addition reaction of the unsaturated bonds contained in PSS-allyl-heptaisobutyl substitution and the silicon-hydrogen bonds in hydroxypropyl silicone oil not only further enhances the cross-linking density of the coating, but also improves its thermal stability, which enables the coating to maintain good performance in a heated environment and reduces the aging phenomenon caused by temperature changes. Furthermore, when a hydroxyl-containing quaternary ammonium polymer with antibacterial effect is added to the system, its cationic quaternary ammonium group part can destroy the cell structure of microorganisms, thereby achieving the purpose of antibacterial. This quaternary ammonium salt polymer can not only provide a lasting antibacterial function, but also synergize with other components to improve the adhesion and surface smoothness of the coating. In addition, the quaternary ammonium polymer forms hydrogen bonds with the polyurethane elastic segment and the polysiloxane segment, which enhances the cohesion of the entire system, thereby improving the wear resistance and scratch resistance of the coating. In summary, there is good compatibility and interaction between the siloxane segment in the organosilicon-modified resin and the polysiloxane main body in the raw material system, and synergizes with the composite filler molybdenum disulfide and the soft and hard particles of aluminum oxide, which not only gives the glass coating good antibacterial properties, but also significantly improves the wear resistance and weathering resistance of the glass coating.

[0016] Preferably, the organosilicon modified resin is prepared by the following method:

[0017] Add 15-20 parts by weight of PSS-allyl-heptaisobutyl substituted and 18-22 parts by weight of hydroxypropyl silicone oil to 70-85 parts by weight of N-methylpyrrolidone, heat to 90-95°C at 100-150rpm in a nitrogen atmosphere, then add 0.1-0.15 parts by weight of Custer catalyst to react for 4-6h. After the reaction is completed, recover N-methylpyrrolidone by vacuum distillation to obtain polysilsesquioxane-grafted hydroxypropyl silicone oil;

[0018] 25-30 parts by weight of acryloyloxyethyl dimethylbenzyl ammonium chloride, 25-30 parts by weight of 2-methacryloyloxyethyl phosphorylcholine and 8-12 parts by weight of N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane are added to 140-160 parts by weight of N-methylpyrrolidone, heated to 85-90° C. at 100-150 rpm in a nitrogen atmosphere, then 0.1-0.3 parts by weight of benzoyl peroxide are added to react for 8-10 hours, and after the reaction is completed, the N-methylpyrrolidone is recovered by reduced pressure distillation to obtain a hydroxyl-containing quaternary ammonium polymer;

[0019] 15-25 parts by weight of dicyclohexylmethane-4,4'-diisocyanate, 10-20 parts by weight of polytetramethylene glycol, 5-10 parts by weight of polysilsesquioxane-grafted hydroxypropyl silicone oil and 2-5 parts by weight of hydroxyl-containing quaternary ammonium polymer are added to 50-80 parts by weight of N-methylpyrrolidone, heated to 80-85° C. at 100-150 rpm in a nitrogen atmosphere, then 0.1-0.2 parts by weight of dibutyltin dilaurate are added and reacted for 2-5 hours. After the reaction is completed, N-methylpyrrolidone is recovered by reduced pressure distillation to obtain a silicone modified resin.

[0020] Preferably, the crosslinking aid is at least one of methyltrimethoxysilane, dimethyldimethoxysilane and vinyltrimethoxysilane.

[0021] Preferably, the catalyst is at least one of tetrabutyl titanate, bismuth 2-ethylhexanoate, and dibutyltin dilaurate.

[0022] Preferably, the film-forming aid is alcohol ester dodecaned.

[0023] Preferably, the solvent is at least one of ethylene glycol monobutyl ether, N-methyl pyrrolidone, and propylene glycol methyl ether acetate.

[0024] The present invention also provides a process for preparing a polysiloxane organosilicon elastic glass coating, comprising the following steps:

[0025] According to the raw material formula, polysiloxane, organosilicon modified resin, composite filler, crosslinking aid, catalyst, film-forming aid and solvent are mixed evenly to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 45-60°C for 5-8h, and cooled to room temperature to obtain the polysiloxane organosilicon elastic glass coating. Preferably, the thickness of the coating is 10-30 μm.

[0026] In a specific implementation manner, the glass substrate is cleaned with acetone and water in sequence before coating, and is dried for later use.

[0027] Beneficial effects of the present invention:

[0028] The present invention provides a polysiloxane organosilicon elastic glass coating, which is prepared by reacting dicyclohexylmethane-4,4'-diisocyanate, polytetramethylene ether diol, polysilsesquioxane grafted hydroxypropyl silicone oil with a quaternary ammonium polymer containing a hydroxyl group by adding an organosilicon modified resin, and synergistically acts with a composite filler to further improve the wear resistance, aging resistance and antibacterial performance of the glass coating, while maintaining good toughness, hardness, water resistance, salt spray resistance and stain resistance. The present invention also provides a preparation process of the polysiloxane organosilicon elastic glass coating, which is simple and easy to operate. DETAILED DESCRIPTION

[0029] The above-mentioned invention contents of the present invention are further described in detail below in conjunction with specific implementation methods. The embodiments are only for illustrating the technical concept and features of the present invention, and their purpose is to enable people familiar with the technology to understand the contents of the present invention and implement them accordingly, and they cannot be used to limit the protection scope of the present invention. Any equivalent changes or modifications made according to the spirit and essence of the present invention should be included in the protection scope of the present invention.

[0030] Example 1

[0031] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0032] 30 parts by weight of polysiloxane, 7.5 parts by weight of organosilicon modified resin, 2.5 parts by weight of composite filler, 2 parts by weight of crosslinking aid methyltrimethoxysilane, 0.3 parts by weight of catalyst tetrabutyl titanate, 0.2 parts by weight of film-forming aid alcohol ester dodecahydrate, and 120 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1.5:1.

[0033] The organosilicon modified resin is prepared by the following method:

[0034] 17 parts by weight of PSS-allyl-heptaisobutyl substituted (CAS: 351003-00-4) and 20 parts by weight of hydroxypropyl silicone oil (average molecular weight of 1000, hydroxyl content of 2.5%) were added to 80 parts by weight of N-methylpyrrolidone, heated to 92° C. at 120 rpm in a nitrogen atmosphere, and then 0.12 parts by weight of Custer catalyst were added to react for 4.5 hours. After the reaction was completed, N-methylpyrrolidone was recovered by vacuum distillation to obtain polysilsesquioxane-grafted hydroxypropyl silicone oil;

[0035] 26 parts by weight of acryloyloxyethyl dimethylbenzyl ammonium chloride (CAS: 46830-22-2), 28 parts by weight of 2-methacryloyloxyethyl phosphorylcholine (CAS: 67881-98-5) and 10 parts by weight of N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane (CAS: 123198-57-2) are added to 150 parts by weight of N-methylpyrrolidone, heated to 86° C. at 120 rpm in a nitrogen atmosphere, then 0.2 parts by weight of benzoyl peroxide is added to react for 8.5 hours, and after the reaction is completed, the N-methylpyrrolidone is recovered by reduced pressure distillation to obtain a quaternary ammonium polymer containing a hydroxyl group;

[0036] 20 parts by weight of dicyclohexylmethane-4,4'-diisocyanate (CAS: 5124-30-1), 15 parts by weight of polytetramethylene glycol (average molecular weight of 1000), 7 parts by weight of polysilsesquioxane-grafted hydroxypropyl silicone oil and 3 parts by weight of hydroxyl-containing quaternary ammonium polymer were added to 60 parts by weight of N-methylpyrrolidone, heated to 82°C at 120rpm in a nitrogen atmosphere, and then 0.13 parts by weight of dibutyltin dilaurate was added to react for 3 hours. After the reaction was completed, N-methylpyrrolidone was recovered by reduced pressure distillation to obtain a silicone modified resin.

[0037] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0038] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 50° C. for 6 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0039] Example 2

[0040] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0041] 20 parts by weight of polysiloxane, 5 parts by weight of organosilicon modified resin, 1 part by weight of composite filler, 1 part by weight of crosslinking aid methyltrimethoxysilane, 0.2 parts by weight of catalyst tetrabutyl titanate, 0.1 parts by weight of film-forming aid alcohol ester twelve, 100 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is a hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1:1. The organosilicon modified resin is the same as that in Example 1.

[0042] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0043] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 45° C. for 8 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0044] Example 3

[0045] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0046] 40 parts by weight of polysiloxane, 10 parts by weight of organosilicon modified resin, 4 parts by weight of composite filler, 3 parts by weight of crosslinking aid methyltrimethoxysilane, 0.4 parts by weight of catalyst tetrabutyl titanate, 0.3 parts by weight of film-forming aid alcohol ester twelve, 150 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is a hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 2:1. The organosilicon modified resin is the same as that in Example 1.

[0047] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0048] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 60° C. for 5 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0049] Example 4

[0050] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0051] 30 parts by weight of polysiloxane, 7.5 parts by weight of organosilicon modified resin, 2.5 parts by weight of composite filler, 2 parts by weight of crosslinking aid methyltrimethoxysilane, 0.3 parts by weight of catalyst tetrabutyl titanate, 0.2 parts by weight of film-forming aid alcohol ester dodecahydrate, and 120 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1.5:1.

[0052] The organosilicon modified resin is prepared by the following method:

[0053] 20 parts by weight of dicyclohexylmethane-4,4'-diisocyanate (CAS: 5124-30-1), 15 parts by weight of polytetramethylene glycol (average molecular weight of 1000), 7 parts by weight of hydroxypropyl silicone oil (average molecular weight of 1000, hydroxyl content of 2.5%) and 3 parts by weight of N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane (CAS: 123198-57-2) were added to 60 parts by weight of N-methylpyrrolidone, heated to 82° C. at 120 rpm in a nitrogen atmosphere, and then 0.13 parts by weight of dibutyltin dilaurate was added to react for 3 hours. After the reaction was completed, N-methylpyrrolidone was recovered by reduced pressure distillation to obtain a silicone modified resin.

[0054] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0055] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 50° C. for 6 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0056] Example 5

[0057] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0058] 30 parts by weight of polysiloxane, 7.5 parts by weight of organosilicon modified resin, 2.5 parts by weight of composite filler, 2 parts by weight of crosslinking aid methyltrimethoxysilane, 0.3 parts by weight of catalyst tetrabutyl titanate, 0.2 parts by weight of film-forming aid alcohol ester dodecahydrate, and 120 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1.5:1.

[0059] The organosilicon modified resin is prepared by the following method:

[0060] 26 parts by weight of acryloyloxyethyl dimethylbenzyl ammonium chloride (CAS: 46830-22-2), 28 parts by weight of 2-methacryloyloxyethyl phosphorylcholine (CAS: 67881-98-5) and 10 parts by weight of N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane (CAS: 123198-57-2) are added to 150 parts by weight of N-methylpyrrolidone, heated to 86° C. at 120 rpm in a nitrogen atmosphere, then 0.2 parts by weight of benzoyl peroxide is added to react for 8.5 hours, and after the reaction is completed, the N-methylpyrrolidone is recovered by reduced pressure distillation to obtain a quaternary ammonium polymer containing a hydroxyl group;

[0061] 20 parts by weight of dicyclohexylmethane-4,4'-diisocyanate (CAS: 5124-30-1), 15 parts by weight of polytetramethylene glycol (average molecular weight of 1000), 7 parts by weight of hydroxypropyl silicone oil (average molecular weight of 1000, hydroxyl content of 2.5%) and 3 parts by weight of hydroxyl-containing quaternary ammonium polymer were added to 60 parts by weight of N-methylpyrrolidone, heated to 82° C. at 120 rpm in a nitrogen atmosphere, and then 0.13 parts by weight of dibutyltin dilaurate was added to react for 3 hours. After the reaction was completed, N-methylpyrrolidone was recovered by reduced pressure distillation to obtain a silicone modified resin.

[0062] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0063] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 50° C. for 6 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0064] Example 6

[0065] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0066] 30 parts by weight of polysiloxane, 7.5 parts by weight of organosilicon modified resin, 2.5 parts by weight of composite filler, 2 parts by weight of crosslinking aid methyltrimethoxysilane, 0.3 parts by weight of catalyst tetrabutyl titanate, 0.2 parts by weight of film-forming aid alcohol ester dodecahydrate, and 120 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1.5:1.

[0067] The organosilicon modified resin is prepared by the following method:

[0068] 17 parts by weight of PSS-allyl-heptaisobutyl substituted (CAS: 351003-00-4) and 20 parts by weight of hydroxypropyl silicone oil (average molecular weight of 1000, hydroxyl content of 2.5%) were added to 80 parts by weight of N-methylpyrrolidone, heated to 92° C. at 120 rpm in a nitrogen atmosphere, and then 0.12 parts by weight of Custer catalyst were added to react for 4.5 hours. After the reaction was completed, N-methylpyrrolidone was recovered by vacuum distillation to obtain polysilsesquioxane-grafted hydroxypropyl silicone oil;

[0069] 20 parts by weight of dicyclohexylmethane-4,4'-diisocyanate (CAS: 5124-30-1), 15 parts by weight of polytetramethylene glycol (average molecular weight of 1000), 7 parts by weight of polysilsesquioxane-grafted hydroxypropyl silicone oil and 3 parts by weight of N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane (CAS: 123198-57-2) were added to 60 parts by weight of N-methylpyrrolidone, heated to 82° C. at 120 rpm in a nitrogen atmosphere, and then 0.13 parts by weight of dibutyltin dilaurate was added to react for 3 hours. After the reaction was completed, N-methylpyrrolidone was recovered by reduced pressure distillation to obtain a silicone modified resin.

[0070] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0071] According to the raw material formula, polysiloxane, silicone modified resin, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 50° C. for 6 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0072] Example 7

[0073] A polysiloxane organosilicon elastic glass coating is made from the following raw materials in parts by weight:

[0074] 37.5 parts by weight of polysiloxane, 2.5 parts by weight of composite filler, 2 parts by weight of crosslinking aid methyltrimethoxysilane, 0.3 parts by weight of catalyst tetrabutyl titanate, 0.2 parts by weight of film-forming aid alcohol ester dodecahydrate, and 120 parts by weight of solvent ethylene glycol monobutyl ether. The polysiloxane is hydroxyl-terminated polydimethylsiloxane with a viscosity of 35000 mPa·s (25°C). The composite filler is a mixture of molybdenum disulfide (average particle size of 0.5 μm) and aluminum oxide (average particle size of 0.5 μm) in a weight ratio of 1.5:1.

[0075] A preparation process of a polysiloxane organosilicon elastic glass coating comprises the following steps:

[0076] According to the raw material formula, polysiloxane, composite filler, cross-linking aid, catalyst, film-forming aid and solvent are evenly mixed to obtain a film-forming liquid; the film-forming liquid is coated on a glass substrate, cured at 50° C. for 6 hours, and cooled to room temperature to obtain the polysiloxane silicone elastic glass coating, and the coating has a thickness of 20 μm.

[0077] Test Example 1

[0078] The basic properties of the polysiloxane organosilicon elastic glass coating obtained in the above examples were measured. Among them, the adhesion was measured with reference to GB / T 9286-2021, the flexibility was measured with reference to GB / T 1731-2020, the hardness was measured with reference to GB / T 6739-2022, the salt spray resistance (neutral) was measured with reference to GB / T 1771-2007, the water resistance was measured with reference to GB 5209-1985, and the stain resistance was measured with reference to GB 5209-1985. The test results are shown in Table 1.

[0079] Table 1 Basic properties of polysiloxane silicone elastic glass coating

[0080]

[0081] Test Example 2

[0082] The wear resistance (1000g / 500r) of the polysiloxane organosilicon elastic glass coating obtained in the above embodiment was measured with reference to GB / T 1768-2006; the aging resistance of the polysiloxane organosilicon elastic glass coating obtained in the above embodiment was measured (the method is: the rolling angle is tested after 1200h of simulated light aging, and a rolling angle less than 10° indicates good performance); the antibacterial performance (Escherichia coli AS1.90) of the polysiloxane organosilicon elastic glass coating obtained in the above embodiment was measured with reference to HG / T 3950-2007. The test results are shown in Table 2.

[0083] Table 2 Wear resistance / aging resistance / antibacterial properties of polysiloxane silicone elastic glass coating

[0084]

[0085] From the comparison of the above test results, it can be seen that the polysiloxane silicone elastic glass coating prepared in Examples 1-3 not only has good salt spray resistance, water resistance, stain resistance, adhesion, toughness and hardness, but also has excellent wear resistance, aging resistance and antibacterial properties; the reason is that the present invention adopts a silicone modified resin made by reacting dicyclohexylmethane-4,4'-diisocyanate, polytetrahydrofuran ether diol, polysilsesquioxane grafted hydroxypropyl silicone oil with a quaternary ammonium polymer containing a hydroxyl group, and synergizes with the composite filler, thereby effectively improving the wear resistance, aging resistance and antibacterial properties of the glass coating, and maintaining good comprehensive performance. Compared with Examples 1-3, Examples 4-7 do not use the above-mentioned specific silicone modified resin. It can be seen from Table 2 that the wear resistance, aging resistance and antibacterial properties of the glass coating deteriorate, which shows that Examples 4-7 do not use the necessary technical solution of the present invention, resulting in a significant deterioration in the corresponding performance test, thereby proving the importance of the necessary technical solution defined by the present invention to its technical effect.

[0086] The preferred specific embodiments of the present invention are described in detail above. It should be understood that a person skilled in the art can make many modifications and changes based on the concept of the present invention without creative work. Therefore, any technical solution that can be obtained by a person skilled in the art through logical analysis, reasoning or limited experiments based on the concept of the present invention on the basis of the prior art should be within the scope of protection determined by the claims.

Claims

1. A polysiloxane organosilicon elastic glass coating, characterized in that: Made from the following raw materials in parts by weight: 20-40 parts by weight of polysiloxane, 5-10 parts by weight of organosilicon modified resin, 1-4 parts by weight of composite filler, 1-3 parts by weight of crosslinking aid, 0.2-0.4 parts by weight of catalyst, 0.1-0.3 parts by weight of film-forming aid, and 100-150 parts by weight of solvent.

2. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The organosilicon modified resin is prepared by the following method: Dicyclohexylmethane-4,4'-diisocyanate, polytetramethylene glycol, polysilsesquioxane-grafted hydroxypropyl silicone oil and hydroxyl-containing quaternary ammonium polymer are added to N-methylpyrrolidone, heated under a nitrogen atmosphere, and then dibutyltin dilaurate is added to react. After the reaction is completed, it is distilled under reduced pressure to obtain a silicone modified resin.

3. The polysiloxane organosilicon elastic glass coating according to claim 2, characterized in that: The preparation method of the polysilsesquioxane grafted hydroxypropyl silicone oil is as follows: PSS-allyl-heptaisobutyl substituted hydroxypropyl silicone oil is added to N-methylpyrrolidone, heated under a nitrogen atmosphere, and then a Custer catalyst is added to react, and after the reaction is completed, reduced pressure distillation is performed to obtain the polysilsesquioxane grafted hydroxypropyl silicone oil; The preparation method of the hydroxyl-containing quaternary ammonium polymer comprises the following steps: adding acryloyloxyethyl dimethylbenzyl ammonium chloride, 2-methacryloyloxyethyl phosphorylcholine and N-(3-acryloyloxy-2-hydroxypropyl)-3-aminopropyltriethoxysilane to N-methylpyrrolidone, heating under a nitrogen atmosphere, then adding benzoyl peroxide for reaction, and after the reaction is completed, performing reduced pressure distillation to obtain the hydroxyl-containing quaternary ammonium polymer.

4. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The polysiloxane is hydroxyl-terminated polydimethylsiloxane.

5. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The composite filler is a mixture of molybdenum disulfide and aluminum oxide.

6. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The cross-linking aid is at least one of methyltrimethoxysilane, dimethyldimethoxysilane and vinyltrimethoxysilane.

7. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The catalyst is at least one of tetrabutyl titanate, bismuth 2-ethylhexanoate, and dibutyltin dilaurate.

8. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The film-forming aid is alcohol ester dodecahydrate.

9. The polysiloxane organosilicon elastic glass coating according to claim 1, characterized in that: The solvent is at least one of ethylene glycol monobutyl ether, N-methyl pyrrolidone, and propylene glycol methyl ether acetate.

10. The process for preparing the polysiloxane organosilicon elastic glass coating according to any one of claims 1 to 9, characterized in that: The following steps are involved: According to the raw material formula, polysiloxane, organosilicon modified resin, composite filler, crosslinking aid, catalyst, film-forming aid and solvent are uniformly mixed to obtain film-forming liquid; the film-forming liquid is coated on a glass substrate, solidified and cooled to obtain the polysiloxane organosilicon elastic glass coating.

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