Low-radiation coated glass and preparation method thereof

Abstract

The present invention relates to the field of glass technology, and specifically to a low-radiation coated glass and a preparation method thereof, comprising the following steps: a glass substrate is first immersed in a sufficient amount of a hydrochloric acid solution with a mass fraction of 2% for ultrasonic treatment, with an ultrasonic power of 350-400W, ultrasonic for 1h, ultrasonic termination, water washing, and drying; and a coating layer is set on the glass substrate of step 1 to obtain a glass with a coating layer. The coated glass of the present invention uses a glass substrate as a raw material, is treated with a hydrochloric acid solution to optimize its active efficiency and cleanliness, and is then treated with a coating layer, and is simultaneously matched with a coating liquid to further optimize its low radiation, wear resistance, and easy-to-clean performance, as well as coordinately improve the scrub resistance, high temperature, and corrosion resistance stability of the product.

Description

Technical Field

[0001] The present invention relates to the technical field of glass, and in particular to a low-radiative coated glass and a preparation method thereof. Background Art

[0002] As a building decoration material, glass has been widely used in all aspects of people's daily production and life, and the surface treatment of glass has gradually become a new direction for the development of glass. Coated glass is mainly achieved by depositing one or more layers of thin film materials (such as metal, alloy or metal compound thin films) on the surface of the glass substrate, thereby changing the optical, electrical and mechanical properties of the glass to meet energy saving requirements.

[0003] The existing coated glass has poor low-radiation properties, and the product's wear resistance and easy-cleaning performance are poor. It is difficult to achieve coordinated improvements in low-radiation, wear resistance and easy-cleaning performance. The product also has poor scrub resistance, high temperature and corrosion resistance, which further limits the product's efficiency. Summary of the invention

[0004] In view of the defects of the prior art, the purpose of the present invention is to provide a low-emissivity coated glass and a preparation method thereof to solve the problems raised in the above background technology.

[0005] The present invention solves the technical problem by adopting the following technical solution:

[0006] The present invention provides a method for preparing low-emissivity coated glass, comprising the following steps:

[0007] Step 1: pre-treat the glass substrate, and set it aside after the pre-treatment is completed;

[0008] Step 2: sputtering Ti powder and Al onto the pretreated glass substrate in sequence to obtain a coated glass layer;

[0009] Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then a low-emissivity coated glass is made;

[0010] The improved coating liquid comprises the following raw materials in parts by weight:

[0011] 40-45 parts of polyurethane emulsion, 10-15 parts of acetone solvent, 5-8 parts of modified additives, 2-4 parts of silane coupling agent KH560, 4-6 parts of coordinating agent, 5-7 parts of curing agent, 2-3 parts of carboxymethyl cellulose;

[0012] The modified additive is prepared by mixing heat-insulated montmorillonite and modified liquid with urea solution, sodium lignin sulfonate and nano-silica sol after ball milling.

[0013] The modified liquid includes the following raw materials in parts by weight: 3-5 parts of sodium silicate solution, 4-6 parts of dopamine hydrochloride solution, 2-4 parts of silicon carbide, 2-3 parts of boron nitride and 1-3 parts of yttrium oxide;

[0014] The coordinated adjustment agent is prepared by mixing nano zinc oxide, wollastonite impregnation agent, lanthanum chloride solution and chitosan solution, filtering and drying.

[0015] The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

[0016] Preferably, the specific steps of pretreatment in step 1 are: the glass substrate is first immersed in a sufficient amount of hydrochloric acid solution with a mass fraction of 2% for ultrasonic treatment, the ultrasonic power is 350-400W, the ultrasonic treatment is for 1h, the ultrasonic treatment is terminated, the glass substrate is washed with water, and dried to obtain a pretreated glass substrate;

[0017] The specific operation method of sputtering Ti powder and Al in sequence in step 2 is:

[0018] Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively;

[0019] The glass transition temperature of the polyurethane emulsion is 44-45°C, and the minimum film-forming temperature is 26-28°C; the curing agent is a polyisocyanate curing agent.

[0020] Preferably, the specific preparation method of the modified additive is:

[0021] S01: Mix silicon micropowder and nano-titanium dioxide in a weight ratio of 3:5, and then place them in toluene with a weight of 7-9 times the total amount of silicon micropowder, and then add silane coupling agent KH550 with a weight of 30-35% of the total amount of silicon micropowder, and perform ultrasonic treatment at an ultrasonic power of 350-400W for 1h. After the ultrasonic treatment is completed, wash with water, filter and dry;

[0022] S02: heat treating the montmorillonite at 210-220°C for 5-10 minutes, then cooling to 55°C at a rate of 2-5°C / min, and heat-insulating to obtain heat-insulated montmorillonite;

[0023] S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying;

[0024] S04: 5-8 parts of S01 product, 7-11 parts of urea solution, 2-3 parts of sodium lignin sulfonate, 4-7 parts of montmorillonite modifier and 1-2 parts of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

[0025] Preferably, the ball milling speed of the ball milling modification treatment in S03 is 1000-1500 r / min, and the ball milling is for 2 hours; the stirring speed of the blending and stirring treatment in S04 is 450-500 r / min, stirring is for 1 hour, and the stirring temperature is 48-52°C.

[0026] Preferably, the mass fraction of the sodium silicate solution is 3-5%; the mass fraction of the dopamine hydrochloride solution is 2-4%.

[0027] Preferably, the specific preparation method of the coordinated adjustment agent is:

[0028] S11: 2-4 parts of hydroxyapatite, 1-3 parts of basalt fiber and 3-5 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution;

[0029] The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent.

[0030] S12: 3-5 parts of nano zinc oxide and 2-4 parts of wollastonite impregnating agent are added to 5-8 parts of lanthanum chloride solution, and then 2-3 parts of chitosan solution are added, stirred sufficiently, filtered and dried to obtain a coordinated adjusting agent.

[0031] Preferably, the immersion ultrasonic treatment has an immersion ultrasonic power of 350-400 W and the immersion is for 1 hour.

[0032] Preferably, the mass fraction of the lanthanum chloride solution is 4-7%; the mass fraction of the chitosan solution is 2-5%.

[0033] The present invention also provides a method for preparing low-radiation coated glass and low-radiation coated glass prepared therefrom.

[0034] Compared with the prior art, the present invention has the following beneficial effects:

[0035] The coated glass of the present invention adopts a glass substrate as a raw material, is treated with a hydrochloric acid solution to optimize its activity efficiency and cleanliness, and is then treated with a coating layer and a coating liquid is applied to further optimize its low radiation, wear resistance and easy-to-clean performance, and coordinately improve the scrub resistance, high temperature and corrosion resistance of the product; the modified additive in the improved coating liquid is prepared by blending silicon micropowder and nano-titanium dioxide, and is ultrasonically treated with toluene and a silane coupling agent KH550, and montmorillonite is first heat-treated at 210-220°C for 5-10min, and then cooled to 55°C at a rate of 2-5°C / min, and its interlaminar spacing is optimized through thermal improvement, and its activity efficiency is improved; at the same time, after the modified liquid is improved, the sodium silicate solution, dopamine hydrochloride solution, silicon carbide, boron nitride and yttrium oxide in the modified liquid are coordinated and blended, and through the co-coordination and synergy between the raw materials, silicon carbide and boron nitride are used as the matrix raw materials, and after co-coordination and coordination, the modified liquid improved The effect of montmorillonite is better. The improved montmorillonite is blended and stirred with S01 product, urea solution and sodium lignin sulfonate, as well as montmorillonite modifier and nano silica sol. The coordination between the raw materials is optimized through the coordination between the raw materials, so that the modified additives in the system enhance the low radiation, wear resistance and easy cleaning performance of the product, and coordinate and improve the scrub resistance, high temperature and corrosion resistance of the product. The coordinated adjusting agent adopts wollastonite and is immersed in the re-immersion liquid for ultrasonic treatment. The re-immersion liquid is blended with hydroxyapatite, basalt fiber and 5% sodium citrate solution by mass, and then treated with wollastonite. The obtained wollastonite impregnating agent is blended with nano zinc oxide, lanthanum chloride solution and chitosan solution. Wollastonite is used to blend raw materials such as basalt fiber. Through the mutual coordination and assistance between the raw materials, the coordinated adjusting agent and the modified additive are further blended and coordinated, so that the performance of the product is further improved, and the performance of the product is further optimized and improved. DETAILED DESCRIPTION

[0036] The following is a clear and complete description of the technical solutions in the embodiments of the present invention in conjunction with specific embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0037] A method for preparing low-emissivity coated glass in this embodiment includes the following steps:

[0038] Step 1: pre-treat the glass substrate, and set it aside after the pre-treatment is completed;

[0039] Step 2: sputtering Ti powder and Al onto the pretreated glass substrate in sequence to obtain a coated glass layer;

[0040] Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then a low-emissivity coated glass is made;

[0041] The improved coating liquid comprises the following raw materials in parts by weight:

[0042] 40-45 parts of polyurethane emulsion, 10-15 parts of acetone solvent, 5-8 parts of modified additives, 2-4 parts of silane coupling agent KH560, 4-6 parts of coordinating agent, 5-7 parts of curing agent, 2-3 parts of carboxymethyl cellulose;

[0043] The modified additive is prepared by mixing heat-insulated montmorillonite and modified liquid with urea solution, sodium lignin sulfonate and nano-silica sol after ball milling.

[0044] The modified liquid includes the following raw materials in parts by weight: 3-5 parts of sodium silicate solution, 4-6 parts of dopamine hydrochloride solution, 2-4 parts of silicon carbide, 2-3 parts of boron nitride and 1-3 parts of yttrium oxide;

[0045] The coordinated adjustment agent is prepared by mixing nano zinc oxide, wollastonite impregnation agent, lanthanum chloride solution and chitosan solution, filtering and drying.

[0046] The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

[0047] The specific steps of the pretreatment in step 1 are: the glass substrate is first immersed in a sufficient amount of a hydrochloric acid solution with a mass fraction of 2% for ultrasonic treatment, the ultrasonic power is 350-400W, the ultrasonic treatment is performed for 1 hour, the ultrasonic treatment is terminated, the glass substrate is washed with water, and dried to obtain a pretreated glass substrate;

[0048] The specific operation method of sputtering Ti powder and Al in sequence in step 2 is:

[0049] Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively;

[0050] The glass transition temperature of the polyurethane emulsion is 44-45°C, and the minimum film-forming temperature is 26-28°C; the curing agent is a polyisocyanate curing agent.

[0051] The specific preparation method of the modified additive of this embodiment is:

[0052] S01: Mix silicon micropowder and nano-titanium dioxide in a weight ratio of 3:5, and then place them in toluene with a weight of 7-9 times the total amount of silicon micropowder, and then add silane coupling agent KH550 with a weight of 30-35% of the total amount of silicon micropowder, and perform ultrasonic treatment at an ultrasonic power of 350-400W for 1h. After the ultrasonic treatment is completed, wash with water, filter and dry;

[0053] S02: heat treating the montmorillonite at 210-220°C for 5-10 minutes, then cooling to 55°C at a rate of 2-5°C / min, and heat-insulating to obtain heat-insulated montmorillonite;

[0054] S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying;

[0055] S04: 5-8 parts of S01 product, 7-11 parts of urea solution, 2-3 parts of sodium lignin sulfonate, 4-7 parts of montmorillonite modifier and 1-2 parts of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

[0056] In S03 of this embodiment, the ball milling speed of the ball milling modification treatment is 1000-1500 r / min, and the ball milling is 2 hours; in S04, the stirring speed of the blending and stirring treatment is 450-500 r / min, stirring is 1 hour, and the stirring temperature is 48-52°C.

[0057] The mass fraction of the sodium silicate solution in this embodiment is 3-5%; the mass fraction of the dopamine hydrochloride solution is 2-4%.

[0058] The specific preparation method of the coordinated adjustment agent of this embodiment is:

[0059] S11: 2-4 parts of hydroxyapatite, 1-3 parts of basalt fiber and 3-5 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution;

[0060] The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent.

[0061] S12: 3-5 parts of nano zinc oxide and 2-4 parts of wollastonite impregnating agent are added to 5-8 parts of lanthanum chloride solution, and then 2-3 parts of chitosan solution are added, stirred sufficiently, filtered and dried to obtain a coordinated adjusting agent.

[0062] The immersion ultrasonic treatment in this embodiment has an immersion ultrasonic power of 350-400 W and is carried out for 1 hour.

[0063] The mass fraction of the lanthanum chloride solution in this embodiment is 4-7%; the mass fraction of the chitosan solution is 2-5%.

[0064] The low-emissivity coated glass is prepared by a method for preparing low-emissivity coated glass in this embodiment.

[0065] Example 1.

[0066] A method for preparing low-emissivity coated glass in this embodiment includes the following steps:

[0067] Step 1: The glass substrate is first immersed in a sufficient amount of 2% hydrochloric acid solution for ultrasonic treatment, with an ultrasonic power of 350W and ultrasonic treatment for 1 hour. After the ultrasonic treatment is completed, the glass substrate is washed with water and dried;

[0068] Step 2: The glass substrate of step 1 is provided with a coating layer to obtain a glass with a coating layer. The specific coating layer method is as follows:

[0069] Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively;

[0070] Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then the low-emissivity coated glass of the present invention is prepared;

[0071] The improved coating liquid comprises the following raw materials in parts by weight:

[0072] 40 parts of polyurethane emulsion, 10 parts of acetone solvent, 5 parts of modifying additive, 2 parts of silane coupling agent KH560, 4 parts of coordinating agent, 5 parts of curing agent, and 2 parts of carboxymethyl cellulose;

[0073] The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

[0074] The polyurethane emulsion of this embodiment has a glass transition temperature of 44°C and a minimum film-forming temperature of 26°C; the curing agent is a polyisocyanate curing agent.

[0075] The preparation method of the modified additive of this embodiment is:

[0076] S01: Silica powder and nano-titanium dioxide were mixed in a weight ratio of 3:5, and then placed in toluene with a weight of 7 times the total weight of the silica powder, followed by adding silane coupling agent KH550 with a weight of 30% of the total weight of the silica powder, and subjected to ultrasonic treatment at a power of 350W for 1 hour. After the ultrasonic treatment was completed, the mixture was washed with water, filtered, and dried;

[0077] S02: The montmorillonite is first heat-treated at 210°C for 5 minutes, then cooled to 55°C at a rate of 2°C / min, and heat-treated to obtain heat-insulated montmorillonite;

[0078] S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying;

[0079] S04: 5 parts of S01 product, 7 parts of urea solution, 2 parts of sodium lignin sulfonate, 4 parts of montmorillonite modifier and 1 part of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

[0080] In S03 of this embodiment, the ball milling speed of the ball milling modification treatment is 1000 r / min, and the ball milling is performed for 2 hours. In S04, the stirring speed of the blending and stirring treatment is 450 r / min, and the stirring is performed for 1 hour, and the stirring temperature is 48°C.

[0081] The modified solution of this embodiment includes the following raw materials in parts by weight: 3 parts of sodium silicate solution, 4 parts of dopamine hydrochloride solution, 2 parts of silicon carbide, 2 parts of boron nitride and 1 part of yttrium oxide.

[0082] The mass fraction of the sodium silicate solution in this embodiment is 3%; the mass fraction of the dopamine hydrochloride solution is 2%.

[0083] The preparation method of the coordinated adjustment agent of this embodiment is:

[0084] S11: 2 parts of hydroxyapatite, 1 part of basalt fiber and 3 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution;

[0085] The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent.

[0086] S12: 3 parts of nano zinc oxide and 2 parts of wollastonite impregnating agent are added to 5 parts of lanthanum chloride solution, and then 2 parts of chitosan solution are added, stirred thoroughly, filtered and dried to obtain a coordinated adjusting agent.

[0087] The immersion ultrasonic treatment in this embodiment has an immersion ultrasonic power of 350 W and is carried out for 1 hour.

[0088] The mass fraction of the lanthanum chloride solution in this embodiment is 4%; the mass fraction of the chitosan solution is 2%.

[0089] The low-radiation coated glass prepared by the method for preparing low-radiation coated glass in this embodiment. Example 2.

[0090] A method for preparing low-emissivity coated glass in this embodiment includes the following steps:

[0091] Step 1: The glass substrate is first immersed in a sufficient amount of 2% hydrochloric acid solution for ultrasonic treatment, with an ultrasonic power of 400W for 1 hour. After the ultrasonic treatment is completed, the glass substrate is washed with water and dried;

[0092] Step 2: The glass substrate of step 1 is provided with a coating layer to obtain a glass with a coating layer. The specific coating layer method is as follows:

[0093] Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively;

[0094] Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then the low-emissivity coated glass of the present invention is prepared;

[0095] The improved coating liquid comprises the following raw materials in parts by weight:

[0096] 45 parts of polyurethane emulsion, 15 parts of acetone solvent, 8 parts of modifying additive, 4 parts of silane coupling agent KH560, 6 parts of coordinating agent, 7 parts of curing agent, and 3 parts of carboxymethyl cellulose;

[0097] The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

[0098] The polyurethane emulsion of this embodiment has a glass transition temperature of 45°C and a minimum film-forming temperature of 28°C; the curing agent is a polyisocyanate curing agent.

[0099] The preparation method of the modified additive of this embodiment is:

[0100] S01: Silica powder and nano-titanium dioxide were mixed in a weight ratio of 3:5, and then placed in toluene with a weight of 9 times the total amount of silica powder, followed by adding silane coupling agent KH550 with a weight of 35% of the total amount of silica powder, and ultrasonic treatment was performed at an ultrasonic power of 400W for 1 hour. After the ultrasonic treatment was completed, the mixture was washed with water, filtered, and dried;

[0101] S02: The montmorillonite is first heat-treated at 220°C for 10 min, then cooled to 55°C at a rate of 5°C / min, and heat-treated to obtain heat-insulated montmorillonite;

[0102] S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying;

[0103] S04: 8 parts of S01 product, 11 parts of urea solution, 3 parts of sodium lignin sulfonate, 7 parts of montmorillonite modifier and 2 parts of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

[0104] In S03 of this embodiment, the ball milling speed of the ball milling modification treatment is 1500 r / min, and the ball milling is performed for 2 hours; in S04, the stirring speed of the blending and stirring treatment is 500 r / min, stirring is performed for 1 hour, and the stirring temperature is 52°C.

[0105] The modified solution of this embodiment includes the following raw materials in parts by weight: 5 parts of sodium silicate solution, 6 parts of dopamine hydrochloride solution, 4 parts of silicon carbide, 3 parts of boron nitride and 3 parts of yttrium oxide.

[0106] The mass fraction of the sodium silicate solution in this embodiment is 5%; the mass fraction of the dopamine hydrochloride solution is 4%.

[0107] The preparation method of the coordinated adjustment agent of this embodiment is:

[0108] S11: 4 parts of hydroxyapatite, 3 parts of basalt fiber and 5 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution;

[0109] The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent.

[0110] S12: 5 parts of nano zinc oxide and 4 parts of wollastonite impregnating agent are added to 8 parts of lanthanum chloride solution, and then 3 parts of chitosan solution are added, stirred thoroughly, filtered and dried to obtain a coordinated adjusting agent.

[0111] The immersion ultrasonic treatment in this embodiment has an immersion ultrasonic power of 400 W and is carried out for 1 hour.

[0112] The mass fraction of the lanthanum chloride solution in this embodiment is 7%; the mass fraction of the chitosan solution is 5%.

[0113] The low-radiation coated glass prepared by the method for preparing low-radiation coated glass in this embodiment. Example 3.

[0114] A method for preparing low-emissivity coated glass in this embodiment includes the following steps:

[0115] Step 1: The glass substrate is first immersed in a sufficient amount of 2% hydrochloric acid solution for ultrasonic treatment, with an ultrasonic power of 375W and ultrasonic treatment for 1h. After the ultrasonic treatment is completed, the glass substrate is washed with water and dried;

[0116] Step 2: The glass substrate of step 1 is provided with a coating layer to obtain a glass with a coating layer. The specific coating layer method is as follows:

[0117] Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively;

[0118] Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then the low-emissivity coated glass of the present invention is prepared;

[0119] The improved coating liquid comprises the following raw materials in parts by weight:

[0120] 42.5 parts of polyurethane emulsion, 12.5 parts of acetone solvent, 6.5 parts of modified additives, 3 parts of silane coupling agent KH560, 5 parts of coordinating agent, 6 parts of curing agent, and 2.5 parts of carboxymethyl cellulose;

[0121] The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

[0122] The polyurethane emulsion of this embodiment has a glass transition temperature of 44.5°C and a minimum film-forming temperature of 27°C; the curing agent is a polyisocyanate curing agent.

[0123] The preparation method of the modified additive of this embodiment is:

[0124] S01: Silica powder and nano-titanium dioxide were mixed in a weight ratio of 3:5, and then placed in toluene with an amount of 8 times the total amount of silica powder, followed by adding silane coupling agent KH550 with an amount of 32.5% of the total amount of silica powder, and subjected to ultrasonic treatment at an ultrasonic power of 375 W for 1 h. After the ultrasonic treatment was completed, the mixture was washed with water, filtered, and dried;

[0125] S02: The montmorillonite is first heat treated at 215°C for 7.5 minutes, then cooled to 55°C at a rate of 3.5°C / min, and heat-treated to obtain heat-insulated montmorillonite;

[0126] S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying;

[0127] S04: 6.5 parts of S01 product, 9 parts of urea solution, 2.5 parts of sodium lignin sulfonate, 5.5 parts of montmorillonite modifier and 1.5 parts of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

[0128] In S03 of this embodiment, the ball milling speed of the ball milling modification treatment is 1250 r / min, and the ball milling is carried out for 2 hours. In S04, the stirring speed of the blending and stirring treatment is 470 r / min, stirring is carried out for 1 hour, and the stirring temperature is 50°C.

[0129] The modified solution of this embodiment includes the following raw materials in parts by weight: 4 parts of sodium silicate solution, 5 parts of dopamine hydrochloride solution, 3 parts of silicon carbide, 2.5 parts of boron nitride and 2 parts of yttrium oxide.

[0130] The mass fraction of the sodium silicate solution in this embodiment is 4%; the mass fraction of the dopamine hydrochloride solution is 3%.

[0131] The preparation method of the coordinated adjustment agent of this embodiment is:

[0132] S11: 3 parts of hydroxyapatite, 2 parts of basalt fiber and 4 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution;

[0133] The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent.

[0134] S12: 4 parts of nano zinc oxide and 3 parts of wollastonite impregnating agent are added to 6.5 parts of lanthanum chloride solution, and then 2.5 parts of chitosan solution are added, stirred thoroughly, filtered and dried to obtain a coordinated adjusting agent.

[0135] The immersion ultrasonic treatment in this embodiment has an immersion ultrasonic power of 375 W and is carried out for 1 hour.

[0136] The mass fraction of the lanthanum chloride solution in this embodiment is 5.5%; the mass fraction of the chitosan solution is 3.5%.

[0137] The low-radiation coated glass prepared by the method for preparing low-radiation coated glass in this embodiment. Comparative Example 1.

[0138] The difference from Example 3 is that no modifying additive is added to the coating liquid.

[0139] Comparative Example 2.

[0140] The difference from Example 3 is that no S01 product is added to the modification additive.

[0141] Comparative Example 3.

[0142] The difference from Example 3 is that the S01 product is directly replaced by nano titanium dioxide raw material.

[0143] Comparative Example 4.

[0144] The difference from Example 3 is that no montmorillonite modifier is added to the modification additive.

[0145] Comparative Example 5.

[0146] Different from Example 3, no modification liquid treatment was used in the preparation of the montmorillonite modifier.

[0147] Comparative Example 6.

[0148] The difference from Example 3 is that no heat-insulating montmorillonite is added in the preparation of the montmorillonite modifier.

[0149] Comparative Example 7.

[0150] The difference from Example 3 is that no coordinating agent is added.

[0151] Comparative Example 8.

[0152] The difference from Example 3 is that nano zinc oxide and chitosan solution are not added in the preparation of the coordinated adjustment agent.

[0153] Comparative Example 9.

[0154] The difference from Example 3 is that no wollastonite impregnating agent is added in the preparation of the coordinated adjusting agent.

[0155] Comparative Example 10.

[0156] The difference from Example 3 is that no re-immersion liquid treatment is used in the preparation of the wollastonite impregnating agent.

[0157] Comparative Example 11.

[0158] The difference from Example 3 is that hydroxyapatite is not added to the re-immersion solution.

[0159] Comparative Example 12.

[0160] The difference from Example 3 is that basalt fiber is not added to the re-immersion solution.

[0161] The products of Examples 1-3 and Comparative Examples 1-12 were subjected to radiation resistance, wear resistance (using a wear tester, rubbing the coating surface back and forth 50 times after applying 250g pressure, wear resistance test) and easy-to-clean performance tests; at the same time, the products were subjected to scrubbing, high temperature and corrosion resistance stability tests (the products were placed at 65°C for 24 hours, then placed under 5% hydrochloric acid mist conditions for 24 hours, and then scrubbed 10 times with a load of 5N, the above being one cycle, and the cycle was 20 times). The performance measurement results are as follows:

[0162]

[0163] From Examples 1-3 and Comparative Examples 1-12, it can be concluded that the emissivity, antifouling and wear rate performance effects of Example 3 of the present invention are all significant, the performance of the product can achieve coordinated improvement, and the scrubbing, high temperature and corrosion resistance stability of the product are significant;

[0164] It can be seen from Comparative Example 1, Comparative Example 7 and Example 3 that the coating liquid does not add any of the modifying additives and the synergistic adjusting agent, and the product performance deteriorates significantly. Only when the two are synergistically formulated, the performance effect of the product is most significant.

[0165] From Comparative Examples 1-6 and Example 3, it can be seen that the performance of the products has a tendency to deteriorate to varying degrees when the S01 product is not added to the modified additive, the S01 product is directly replaced by a nano titanium dioxide raw material, the montmorillonite modifier is not added to the modified additive, the montmorillonite modifier is not treated with a modified liquid, and the montmorillonite modifier is not added with heat-insulating montmorillonite. The modified additive obtained by the specific method of the present invention has the most significant performance effect of the product, and the effect of replacing by other methods is not as obvious as that of the present invention;

[0166] It can be seen from Comparative Examples 8-12 and Example 3 that the performance of the products tends to deteriorate to varying degrees when no nano zinc oxide and chitosan solution are added in the preparation of the synergistic adjusting agent, no wollastonite impregnating agent is added in the preparation of the synergistic adjusting agent, no re-immersion liquid treatment is used in the preparation of the wollastonite impregnating agent, no hydroxyapatite is added in the re-immersion liquid, and no basalt fiber is added in the re-immersion liquid. Only when the synergistic adjusting agent obtained by the specific method of the present invention is combined with the modifying additive of the present invention, the performance effect of the product is the most significant, and other methods are not as obvious as the effect of the present invention.

[0167] Based on the above tests, the present invention further explores the product performance through the composition of the modified liquid;

[0168] The modified liquid comprises the following raw materials in parts by weight: 3-5 parts of sodium silicate solution, 4-6 parts of dopamine hydrochloride solution, 2-4 parts of silicon carbide, 2-3 parts of boron nitride and 1-3 parts of yttrium oxide; the mass fraction of the sodium silicate solution is 3-5%; the mass fraction of the dopamine hydrochloride solution is 2-4%.

[0169] Experimental example 1.

[0170] The same as Example 3, the only difference is that silicon carbide is not added to the modified liquid.

[0171] Experimental example 2.

[0172] The same as Example 3, except that no boron nitride is added to the modified solution.

[0173] Experimental Example 3.

[0174] The same as Example 3, the only difference is that no sodium silicate solution is added to the modified liquid.

[0175] Experimental Example 4.

[0176] The same as Example 3, the only difference is that no dopamine hydrochloride solution is added to the modified liquid.

[0177] Experimental Example 5.

[0178] The same as Example 3, the only difference is that yttrium oxide is not added to the modified solution.

[0179] The performance tests of Experimental Examples 1-5 are as follows:

[0180]

[0181] It can be seen from Experimental Examples 1-5 that when silicon carbide and boron nitride are not added to the modifying liquid, the performance of the product has a relatively obvious trend of deterioration. At the same time, when sodium silicate solution is not added to the modifying liquid, dopamine hydrochloride solution is not added to the modifying liquid, and yttrium oxide is not added to the modifying liquid, the performance of the product has a trend of deterioration. The modifying liquid obtained by the specific method of the present invention has the most obvious product performance effect, and the use of other methods instead is not as significant as the effect of the present invention.

[0182] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the present invention can be implemented in other specific forms without departing from the spirit or essential features of the present invention. Therefore, the embodiments should be considered exemplary and non-restrictive in all respects, and the scope of the present invention is defined by the appended claims rather than the above description, and it is intended that all changes falling within the meaning and scope of the equivalent elements of the claims be included in the present invention.

[0183] In addition, it should be understood that although the present specification is described according to implementation modes, not every implementation mode contains only one independent technical solution. This description of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment may also be appropriately combined to form other implementation modes that can be understood by those skilled in the art.

Claims

1. A method for preparing low-emissivity coated glass, characterized in that: The following steps are involved: Step 1: pre-treat the glass substrate, and set it aside after the pre-treatment is completed; Step 2: sputtering Ti powder and Al onto the pretreated glass substrate in sequence to obtain a coated glass layer; Step 3: Then the surface of the product of step 2 is coated with the improved coating liquid, with a coating thickness of 0.2 mm. After the coating is completed, it is naturally dried to obtain a coating body, and then a low-emissivity coated glass is made; The improved coating liquid comprises the following raw materials in parts by weight: 40-45 parts of polyurethane emulsion, 10-15 parts of acetone solvent, 5-8 parts of modified additives, 2-4 parts of silane coupling agent KH560, 4-6 parts of coordinating agent, 5-7 parts of curing agent, 2-3 parts of carboxymethyl cellulose; The modified additive is prepared by mixing heat-insulated montmorillonite and modified liquid with urea solution, sodium lignin sulfonate and nano-silica sol after ball milling. The modified liquid includes the following raw materials in parts by weight: 3-5 parts of sodium silicate solution, 4-6 parts of dopamine hydrochloride solution, 2-4 parts of silicon carbide, 2-3 parts of boron nitride and 1-3 parts of yttrium oxide; The coordinated adjustment agent is prepared by mixing nano zinc oxide, wollastonite impregnation agent, lanthanum chloride solution and chitosan solution, filtering and drying. The improved coating liquid is prepared by weighing raw materials according to weight portions, and then mixing the raw materials to obtain the improved coating liquid.

2. The method for preparing low-emissivity coated glass according to claim 1, characterized in that: The specific steps of the pretreatment in step 1 are: the glass substrate is first immersed in a sufficient amount of a hydrochloric acid solution with a mass fraction of 2% for ultrasonic treatment, the ultrasonic power is 350-400W, the ultrasonic treatment is performed for 1 hour, the ultrasonic treatment is terminated, the glass substrate is washed with water, and dried to obtain a pretreated glass substrate; The specific operation method of sputtering Ti powder and Al in sequence in step 2 is: Ti powder and Al were used as raw materials, argon with a purity of 99.99% was used as the ionization gas, nitrogen with a purity of 99.99% was used as the reaction gas, and the vacuum degree was 3×10 Pa, sputtering time 10min, sputtering to obtain Ti film layer and Al film layer, Ti film layer, Al film layer and glass substrate are arranged from top to bottom, and the film thickness of Ti film layer and Al film layer are 150nm and 200nm respectively; The glass transition temperature of the polyurethane emulsion is 44-45°C, and the minimum film-forming temperature is 26-28°C; the curing agent is a polyisocyanate curing agent.

3. The method for preparing low-emissivity coated glass according to claim 1, characterized in that: The specific preparation method of the modified additive is: S01: Mix silicon micropowder and nano-titanium dioxide in a weight ratio of 3:5, and then place them in toluene with a weight of 7-9 times the total amount of silicon micropowder, and then add silane coupling agent KH550 with a weight of 30-35% of the total amount of silicon micropowder, and perform ultrasonic treatment at an ultrasonic power of 350-400W for 1h. After the ultrasonic treatment is completed, wash with water, filter and dry; S02: heat treating the montmorillonite at 210-220°C for 5-10 minutes, then cooling to 55°C at a rate of 2-5°C / min, and heat-insulating to obtain heat-insulated montmorillonite; S03: The heat-insulated montmorillonite and the modified liquid are subjected to ball milling modification treatment in a weight ratio of 5:

3. After the ball milling is completed, the montmorillonite modifier is obtained by suction filtration and drying; S04: 5-8 parts of S01 product, 7-11 parts of urea solution, 2-3 parts of sodium lignin sulfonate, 4-7 parts of montmorillonite modifier and 1-2 parts of nano-silica sol are mixed and stirred, and after the stirring is completed, the mixture is filtered and dried to obtain a modified additive.

4. The method for preparing low-emissivity coated glass according to claim 3, characterized in that: The ball milling speed of the ball milling modification treatment in S03 is 1000-1500r / min, and the ball milling is 2h; the stirring speed of the blending and stirring treatment in S04 is 450-500r / min, stirring is 1h, and the stirring temperature is 48-52℃.

5. The method for preparing low-emissivity coated glass according to claim 1, characterized in that: The mass fraction of the sodium silicate solution is 3-5%; the mass fraction of the dopamine hydrochloride solution is 2-4%.

6. The method for preparing low-emissivity coated glass according to claim 1, characterized in that: The specific preparation method of the coordinated adjustment agent is: S11: 2-4 parts of hydroxyapatite, 1-3 parts of basalt fiber and 3-5 parts of 5% by mass sodium citrate solution are uniformly mixed to obtain a re-immersion solution; The wollastonite is immersed in the re-immersion solution at a weight ratio of 2:5 and then ultrasonically treated. After the immersion is completed, the wollastonite is filtered and dried to obtain a wollastonite impregnating agent. S12: 3-5 parts of nano zinc oxide and 2-4 parts of wollastonite impregnating agent are added to 5-8 parts of lanthanum chloride solution, and then 2-3 parts of chitosan solution are added, stirred sufficiently, filtered and dried to obtain a coordinated adjusting agent.

7. The method for preparing low-emissivity coated glass according to claim 6, characterized in that: The immersion ultrasonic treatment was performed at an immersion ultrasonic power of 350-400 W and the immersion was performed for 1 hour.

8. The method for preparing low-emissivity coated glass according to claim 6, characterized in that: The mass fraction of the lanthanum chloride solution is 4-7%; the mass fraction of the chitosan solution is 2-5%.

9. Low-E coated glass prepared by the method for preparing low-E coated glass according to any one of claims 1 to 8.

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