Preparation process of a heat-insulating sandwich insulating glass

Abstract

The present invention relates to the technical field of insulating glass preparation, and specifically to a preparation process for a heat-insulating interlayer insulating glass. In the present invention, glass substrates are cut, edged, cleaned, and dried, and then semi-tempered treatment is carried out to obtain tempered glass sheets. After heat-pressing heat-insulating interlayers on the two surfaces of the tempered glass sheets, they are pushed into a dust-proof chamber and laminated and assembled with spacer frames, and then sealed and fixed to prepare the heat-insulating interlayer insulating glass. The obtained heat-insulating interlayer insulating glass has an impact resistance of 1969 J / cm<supgt;2< / supgt;, a light transmittance of 99.1%, a thermal conductivity of 0.9 W / (m<supgt;2< / supgt>·K), and an ultraviolet ray blocking rate of 78% for ultraviolet rays with a wavelength of 350 nm. In addition, a heat-insulating interlayer with silicone sol coated on a polycarbonate plate is prepared, and its vertical burning rating is V-0 level, having a flame-retardant effect. The insulating glass prepared by the present invention has strong explosion-proof performance, good airtightness, has a heat-insulating effect, and can block ultraviolet rays.

Description

Technical Field

[0001] The present invention relates to the technical field of insulating glass preparation, and specifically to a preparation process for heat-insulating laminated insulating glass. Background Art

[0002] As a building material with heat-insulating performance, heat-insulating laminated insulating glass has been widely used in the construction field in recent years. Colorless float glass, coated glass, tempered glass, etc. are usually selected as the base materials for heat-insulating laminated insulating glass. After a series of treatments, a heat-insulating layer is coated to prepare the glass. The prepared glass materials can meet the daily requirements in terms of transparency and heat-insulating performance. The spacer material therein mainly plays a role in support and heat insulation. In addition, inert gases such as argon and nitrogen are often filled in the spacer layer. These gases have low thermal conductivity and can significantly improve the heat-insulating performance of the insulating glass. In addition, flame-retardant materials can be added to the heat-insulating layer of the insulating glass to improve its flame-retardant performance and effectively prevent the spread of fire.

[0003] However, the product quality in the current insulating glass field is uneven. For example, Chinese Patent CN113565407B provides a method for processing insulating glass, including the following steps: cutting, edge grinding, and tempering the coated glass and white glass according to the required dimensions, and coating a certain thickness of inner heat-insulating soft glue around to form an insulating glass cavity. Then, the coated glass and white glass after filling and injecting the outer support soft glue are subjected to a curing treatment to form the insulating glass. The said method can be widely applied to the processing of insulating glass, but the prepared insulating glass has poor impact resistance, and the airtightness of the coated heat-insulating soft glue is poor, which is easy to cause leakage of inert gas. Another example is Chinese Patent CN111421918B, which discloses a laminated insulating and intelligent dimming glass with a nano transparent heat-insulating layer. It includes at least two glass layers, and a dimming film is provided between adjacent two glass layers through an adhesive film. A nano transparent heat-insulating layer is provided on the surface of one of the glass layers, and the glass can be intelligently controlled to present a transparent state and different colored non-transparent states by controlling the on-off of the current. The construction is more convenient, and at the same time, it also has good heat-insulating performance. However, for the insulating glass prepared by this invention, the used nano transparent heat-insulating layer is on the surface layer, which is easily affected by long-term light and affects its service life, and it does not have a flame-retardant effect. Another example is CN107446545B, a heat-insulating and flame-retardant insulating glass and its preparation method. The prepared heat-insulating and flame-retardant insulating glass includes a heat-insulating glue layer with a thickness of 10-20 μm, and a flame-retardant PET film is also adhered outside the heat-insulating glue layer, which greatly improves the heat-insulating performance of the insulating glass. Even if the glass bursts in a fire, the flame-retardant PET film can further prevent the spread of fire. However, the insulating glass prepared by this invention does not have the performance of blocking ultraviolet rays.

[0004] Therefore, a preparation process for heat-insulating laminated insulating glass is proposed. Summary of the Invention

[0005] The object of the present invention is to provide a preparation process for heat-insulating interlayer insulating glass. By cutting, edging, cleaning, and drying the glass substrate, and then performing semi-tempering treatment to obtain tempered glass sheets. After hot-pressing heat-insulating interlayers on both surfaces of the tempered glass sheets, they are pushed into a dust-proof chamber and laminated and assembled with spacer frames, and then sealed and fixed to prepare heat-insulating interlayer insulating glass. The obtained heat-insulating interlayer insulating glass has an impact resistance of 1969 J / cm 2 , a light transmittance of 99.1%, a thermal conductivity of 0.9 W / (m 2 ·K), and an ultraviolet ray blocking rate of 78% for ultraviolet rays with a wavelength of 350 nm. In addition, a heat-insulating interlayer coated with silicone sol on a polycarbonate plate is prepared, and its vertical burning rating is V-0, having a flame retardant effect. The insulating glass prepared by the present invention has strong explosion-proof performance, good airtightness, has a heat-insulating effect, and can block ultraviolet rays.

[0006] To achieve the above object, the present invention provides the following technical solutions:

[0007] On the one hand, the present invention includes a preparation process for heat-insulating interlayer insulating glass, which is characterized by including the following steps:

[0008] Cut the glass substrate according to the required size and perform edging treatment to obtain edge-ground glass; soak and clean the edge-ground glass in a solvent with water, surfactant, acetone, and ethanol in sequence, and after cleaning, dry it to obtain standby glass; perform semi-tempering treatment on the dried standby glass to obtain tempered glass sheets; first preheat the tempered glass sheets at 150 - 200 °C, and then hot-press heat-insulating interlayers on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; push the two prefabricated glass sheets into a dust-proof chamber in sequence and laminate and assemble them with spacer frames to form a hollow glass cavity, and then seal and fix them to obtain the heat-insulating interlayer insulating glass;

[0009] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 10 - 30 μm are coated on both sides of the prefabricated glass sheets;

[0010] The preparation method of the heat-insulating interlayer includes the following steps: dissolve tetraethyl orthosilicate in ethanol to obtain a tetraethyl orthosilicate solution; add distilled water and dilute hydrochloric acid to the tetraethyl orthosilicate solution, stir for 3 hours at 40 - 60 °C, then add a flame retardant and an ultraviolet absorber and age for 1 hour at 20 - 80 °C to obtain silicone sol; coat the silicone sol on both surfaces of a polycarbonate plate to obtain a first layer; coat PVB film on both sides of the first layer to obtain a second layer; coat PU film on both surfaces of the second layer to obtain the heat-insulating interlayer;

[0011] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0012] Preferably, the surfactant is sodium dodecyl sulfonate.

[0013] Preferably, the semi-tempered treatment is to heat the dried spare glass at a temperature of 650 - 710 °C for 20 - 60 seconds and then instantaneously quench it with high-pressure air for 10 seconds.

[0014] Preferably, the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours.

[0015] Preferably, the laminating and assembling are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%.

[0016] Preferably, an inert gas is filled into the hollow glass cavity.

[0017] Preferably, the hot pressing is carried out using a hot press; the temperature of the front roller of the hot press is 80 °C, the temperature of the rear roller is 190 °C, and the rolling speed is 0.5 - 1.5 m / min.

[0018] Preferably, the concentration of the tetraethyl orthosilicate solution is 1.8 - 3.7 g / L; the concentration of the dilute hydrochloric acid is 0.2 - 1.1 mol / L.

[0019] Preferably, the flame retardant is prepared by mixing aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is the benzotriazole ultraviolet absorber UVP-327, and its main component is 2-(2'-hydroxy-3',5'-di-tert-butylphenyl)-5-chlorobenzotriazole.

[0020] On the other hand, the present invention also includes a heat-insulating laminated insulating glass, which is characterized in that: the heat-insulating laminated insulating glass is composed of two prefabricated glass sheets on the inner and outer sides, the spacer frame, and the hollow glass cavity located between the two glass sheets; the heat-insulating laminated insulating glass is prepared by the preparation process as described above; the impact resistance strength of the heat-insulating laminated insulating glass is 1969 J / cm2; the light transmittance of the heat-insulating laminated insulating glass is 99.1%; the thermal conductivity of the heat-insulating laminated insulating glass is 0.9 W / (m2·K); the heat-insulating laminated insulating glass includes a heat-insulating layer, and the vertical burning grade of the heat-insulating layer is V-0 level; the ultraviolet ray blocking rate of the heat-insulating laminated insulating glass for ultraviolet rays with a wavelength of 350 nm is 78%.

[0021] Compared with the prior art, the beneficial effects of the present invention are:

[0022] 1. In the present invention, the glass substrate is cut according to the required size and then edge-ground. Then it is placed in a solvent and successively soaked and cleaned with water, sodium dodecyl sulfonate as a surfactant, acetone, and ethanol. After the cleaning is completed, it is dried to obtain a spare glass. The dried spare glass is semi-tempered to obtain a tempered glass sheet. The semi-tempering treatment is to heat the dried spare glass at a temperature of 680 °C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds. Through the said semi-tempering treatment, the impact resistance of the finally prepared heat-insulating laminated insulating glass is 1969 J / cm 2 . By semi-tempering ordinary glass and controlling the temperature and heating time of the semi-tempering treatment in the present invention, the finally prepared heat-insulating laminated insulating glass maintains the maximum impact resistance, has strong explosion-proof performance, and thus can withstand the action of environmental temperature difference load and pneumatic load, is not easily deformed due to fatigue, and is more suitable for use in the outer glass surface of buildings.

[0023] 2. In the present invention, the tempered glass sheet is first preheated at 180 °C, and then a heat-insulating interlayer is hot-pressed on both surfaces of the tempered glass sheet to obtain a prefabricated glass sheet; the hot pressing is carried out using a hot press, the temperature of the front roller of the hot press is 80 °C, the temperature of the rear roller is 190 °C, and the roller pressing speed is 0.8 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; then the two prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with a spacer frame to form a hollow glass cavity, and an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; then it is sealed and fixed to obtain the heat-insulating laminated insulating glass. The heat-insulating laminated insulating glass obtained by the said method has high transparency in the visible light wavelength range (380 - 780 nm), and its light transmittance is 99.1%. The higher the visible light transmittance, the better the permeability and aesthetics of the heat-insulating laminated insulating glass. In addition, through the above preparation processes of pressing and laminating, the obtained hollow glass has very good airtightness, can keep the inert gas from leaking, improves the heat-insulating performance of the hollow glass to a certain extent, alleviates the temperature difference between the two sides of the glass, and avoids the phenomena of fogging and frosting.

[0024] 3. In the present invention, tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 2.2 g / L. Distilled water and dilute hydrochloric acid with a concentration of 0.5 mol / L are added to the tetraethyl orthosilicate solution. The organosilica sol prepared by the above preparation method is used to coat both surfaces of a polycarbonate plate to obtain a heat-insulating interlayer, which is hot-pressed on both surfaces of the tempered glass sheet. Finally, the thermal conductivity of the prepared heat-insulating laminated insulating glass is 0.9 W / (m 2·K). In the present invention, tetraethyl orthosilicate is used as the silicon source, which hydrolyzes into silanol under acidic conditions and then further crosslinks into silica sol. The silica sol has a three-dimensional network structure, and adding a flame retardant and an ultraviolet absorber can enter the interior of the silica sol structure, making the flame retardant performance and ultraviolet absorption performance of the final organosilica sol more stable. In addition, the network structure of the organosilica sol can effectively limit the infrared thermal radiation of the environmental temperature, thereby reducing local heat conduction, and introducing an inert gas also has a certain heat insulation effect. The heat-insulating laminated insulating glass prepared by the present invention as building glass can achieve the effects of maintaining room temperature, reducing the air conditioner startup frequency, and saving energy.

[0025] 4. In the present invention, the tetraethyl orthosilicate solution and water provide an acidic condition through dilute hydrochloric acid, and after stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 60 °C for 1 hour to obtain an organosilica sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is the benzotriazole ultraviolet light absorber UVP-327. The organosilica sol obtained by the above method is finally coated on a polycarbonate plate, and the heat-insulating laminate is hot-pressed on the two surfaces of the tempered glass sheet. The vertical burning grade of the obtained heat-insulating laminate is V-0 level, which can effectively prevent the spread of fire in case of a fire. The insulating glass prepared by the present invention is composed of two prefabricated glass sheets, and heat-insulating laminates are hot-pressed on its two surfaces. The heat-insulating laminate contains an organosilica sol. By controlling the reaction temperature and aging temperature of the organosilica sol, the finally obtained organosilica sol can have a more regular spatial structure, which is beneficial to the dispersion of the flame retardant inside the organosilica sol. Therefore, the finally prepared heat-insulating laminate has a flame retardant effect. Hot-pressing it on the exterior wall glass of a building can effectively block the temperature and the spread of fire, and improve the escape rate in case of a fire.

[0026] 5. The present invention coats silicone sol on both surfaces of a polycarbonate plate to obtain the first layer, coats PVB film on both sides of the first layer to obtain the second layer, and coats PU film on both surfaces of the second layer to obtain a heat-insulating interlayer; and heat-insulating interlayers with a thickness of 20 μm are coated on both sides of the prefabricated glass sheet, the thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm. Through the above-mentioned preparation process, the heat-insulating interlayer insulating glass finally prepared can have an ultraviolet ray blocking rate of 78% for ultraviolet rays with a wavelength of 350 nm. When preparing the silicone sol in the present invention, benzotriazole ultraviolet light absorber UVP-327 is added, which has good chemical stability and can absorb ultraviolet rays with a wavelength of 270-380 nm, so that the finally prepared heat-insulating interlayer insulating glass can achieve a certain barrier to ultraviolet rays. And the silicone sol is in the inner layer of the heat-insulating interlayer and will not be affected by long-term light irradiation. Ultraviolet irradiation will accelerate the aging of human skin. Therefore, good ultraviolet ray protection performance can protect the interior from ultraviolet irradiation; and a PVB film is coated in the heat-insulating interlayer. The PVB film can absorb impact energy. Even if the glass is damaged, its glass fragments will still stick to the intermediate film, which can reduce the probability of fragment splashing and improve the safety performance of the prepared glass. Description of the Drawings

[0027] Figure 1 It is a schematic structural diagram of the heat-insulating interlayer prepared by the present invention, where 0 represents the innermost layer, 1 represents the first layer, A and B respectively represent two surfaces. For example, 1A represents the A surface of the first layer, and so on. Detailed Embodiments

[0028] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0029] Please refer to Figure 1 , the present invention provides a preparation process for a heat-insulating interlayer insulating glass, and the technical solution is as follows:

[0030] Example 1

[0031] A preparation process for a heat-insulating interlayer insulating glass includes the following steps:

[0032] The glass substrate is cut into the required size and then edge-ground to obtain edge-ground glass; the edge-ground glass is placed in a solvent and soaked and cleaned successively with water, the surfactant sodium dodecyl sulfonate, acetone, and ethanol, and after cleaning is completed, it is dried to obtain standby glass; the dried standby glass is semi-tempered to obtain tempered glass sheets; the semi-tempering treatment is to heat the dried standby glass at a temperature of 650 °C for 20 seconds and then instantaneously quench it with high-pressure air for 10 seconds; the tempered glass sheets are first preheated at 150 °C, and then heat-insulating interlayers are hot-pressed on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; the hot pressing is carried out using a hot press; the front roller temperature of the hot press is 80 °C, the rear roller temperature is 190 °C, and the roller pressing speed is 0.5 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; two of the prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with spacer frames to form a hollow glass cavity; an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; and then it is sealed and fixed to obtain the heat-insulating interlayer hollow glass;

[0033] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 10 μm are coated on both sides of the prefabricated glass sheets;

[0034] The preparation method of the heat-insulating interlayer includes the following steps: tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 1.8 g / L; distilled water and dilute hydrochloric acid with a concentration of 0.2 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 20 °C for 1 hour to obtain an organosilicate sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is the benzotriazole-based ultraviolet light absorber UVP-327; the organosilicate sol is coated on both surfaces of a polycarbonate plate to obtain a first layer; a PVB film is coated on both sides of the first layer to obtain a second layer; a PU film is coated on both surfaces of the second layer to obtain the heat-insulating interlayer;

[0035] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0036] In Example 1, the glass substrate is an initial glass sheet, and the production company is Huizhou Yanghang Glass Products Co., Ltd.; for others where specific conditions are not specified, they are carried out according to conventional conditions or the conditions recommended by the manufacturer; for reagents or instruments whose manufacturers are not specified, they are all conventional products that can be obtained by purchasing on the market.

[0037] During the preparation of the heat-insulating interlayer hollow glass in Examples 2-8, the temperature and heating time of the semi-tempering treatment are shown in Table 1, and the remaining steps, operations, and Example 1 are the same.

[0038] Table 1 Temperatures and Heating Times for Heat-Strengthening Treatment in Examples 2 - 8

[0039]

[0040]

[0041] Example 9

[0042] The impact resistance of the heat-insulating laminated insulating glass prepared in Examples 1 - 8 above was detected. The heat-insulating laminated insulating glass was tested for impact resistance using a direct-drive electronic universal testing machine. The test results are shown in Table 2.

[0043] In Example 5, the glass substrate was cut to the required size and then edge-ground. Then it was placed in a solvent and successively soaked and cleaned with water, the surfactant sodium dodecyl sulfate, acetone, and ethanol. After cleaning, it was dried to obtain a spare glass. The dried spare glass was heat-strengthened to obtain a heat-strengthened glass sheet. The heat-strengthening treatment was to heat the dried spare glass at a temperature of 680°C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds. Through the heat-strengthening treatment, the impact resistance of the finally prepared heat-insulating laminated insulating glass was 1969 J / cm 2 . By heat-strengthening ordinary glass and controlling the temperature and heating time of the heat-strengthening treatment, the finally prepared heat-insulating laminated insulating glass maintains the maximum impact resistance, has strong explosion-proof performance, can therefore withstand the action of environmental temperature difference loads and aerodynamic loads, is not easily deformed due to fatigue, and is more suitable for use in the exterior glass surface of buildings.

[0044] Table 2 Impact Resistance of Heat-Insulating Laminated Insulating Glass Prepared in Examples 1 - 8

[0045] <![CDATA[Impact strength (J / cm 2 )]]> Example 1 1765 Example 2 1730 Example 3 1854 Example 4 1655 Example 5 1969 Example 6 1831 Example 7 1828 Example 8 1791

[0046] Example 10

[0047] A preparation process for heat-insulating laminated insulating glass, comprising the following steps:

[0048] The glass substrate is cut into the required size and then edge-ground to obtain edge-ground glass; the edge-ground glass is placed in a solvent and soaked and cleaned successively with water, the surfactant sodium dodecyl sulfonate, acetone, and ethanol, and after the cleaning is completed, it is dried to obtain standby glass; the dried standby glass is semi-tempered to obtain tempered glass sheets; the semi-tempering treatment is to heat the dried standby glass at a temperature of 680 °C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds; the tempered glass sheets are first preheated at 160 °C, and then heat-insulating interlayers are hot-pressed on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; the hot pressing is carried out using a hot press; the temperature of the front roller of the hot press is 80 °C, the temperature of the rear roller is 190 °C, and the roller pressing speed is 0.8 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; two of the prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with spacer frames to form a hollow glass cavity; an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; and then it is sealed and fixed to obtain the heat-insulating interlayer hollow glass;

[0049] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 10 μm are coated on both sides of the prefabricated glass sheets;

[0050] The preparation method of the heat-insulating interlayer includes the following steps: tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 1.8 g / L; distilled water and dilute hydrochloric acid with a concentration of 0.2 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 20 °C for 1 hour to obtain an organosilicate sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is the benzotriazole ultraviolet light absorber UVP-327; the organosilicate sol is coated on both surfaces of a polycarbonate plate to obtain a first layer; a PVB film is coated on both sides of the first layer to obtain a second layer; a PU film is coated on both surfaces of the second layer to obtain the heat-insulating interlayer;

[0051] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0052] In Examples 11 - 18, the preheating temperature and the roller pressing speed are shown in Table 3, and the remaining steps, operations, and Examples 10 are the same.

[0053] Table 3 Preheating temperature and roller pressing speed in Examples 11 - 18

[0054] Preheating Temperature (°C) Rolling Speed (m / min) Example 11 150 1.5 Example 12 150 1.0 Example 13 160 0.8 Example 14 160 0.5 Example 15 180 0.8 Example 16 180 1.0 Example 17 200 0.8 Example 18 200 0.5

[0055] Example 19

[0056] The light transmittance of the heat-insulating interlayer insulating glass prepared in Examples 10-18 above was detected by a light transmittance meter, model HCBT-H, and the results are shown in Table 4.

[0057] In Example 15, the tempered glass sheet was first preheated at 180°C, and then a heat-insulating interlayer was hot-pressed on both surfaces of the tempered glass sheet to obtain a prefabricated glass sheet; the hot pressing was carried out using a hot press, the temperature of the front roller of the hot press was 80°C, the temperature of the rear roller was 190°C, and the rolling speed was 0.8 m / min; the hot pressing was autoclaved for 3 hours at a temperature of 100°C and a pressure of 1.2 Mpa; then the two prefabricated glass sheets were successively pushed into a dust-proof chamber and laminated and assembled with a spacer frame to form a hollow glass cavity, and an inert gas was filled into the hollow glass cavity; the lamination and assembly were carried out in an environment with a temperature of 24±3°C and a relative humidity of 23%±5%; then it was sealed and fixed to obtain the heat-insulating interlayer insulating glass. The heat-insulating interlayer insulating glass obtained by the above method has high transparency in the visible light wavelength range (380-780 nm), its light transmittance is 99.1%, and the higher the visible light transmittance, the better the permeability and aesthetics of the heat-insulating interlayer insulating glass. In addition, through the above preparation processes of pressing and laminating, the airtightness of the obtained insulating glass is very good, which can keep the inert gas from leaking, improve the heat-insulating performance of the insulating glass to a certain extent, slow down the temperature difference between the two sides of the glass, and avoid the phenomena of fogging and frosting.

[0058] Table 4 Light transmittance of the insulating glass prepared in Examples 10-18

[0059] Light Transmittance (%) Example 10 97.5 Example 11 97.1 Example 12 98.6 Example 13 98.5 Example 14 99.0 Example 15 99.1 Example 16 98.4 Example 17 97.9 Example 18 96.8

[0060] Example 20

[0061] A preparation process for a heat-insulating interlayer insulating glass includes the following steps:

[0062] The glass substrate is cut into the required size and then edge-ground to obtain edge-ground glass; the edge-ground glass is placed in a solvent and soaked and cleaned successively with water, sodium dodecyl sulfonate as a surfactant, acetone, and ethanol, and after the cleaning is completed, it is dried to obtain standby glass; the dried standby glass is semi-tempered to obtain tempered glass sheets; the semi-tempering treatment is to heat the dried standby glass at a temperature of 680 °C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds; the tempered glass sheets are first preheated at 180 °C, and then heat-insulating interlayers are hot-pressed on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; the hot pressing is carried out using a hot press; the front roller temperature of the hot press is 80 °C, the rear roller temperature is 190 °C, and the roller pressing speed is 0.8 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; two of the prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with spacer frames to form a hollow glass cavity; an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; and then it is sealed and fixed to obtain the heat-insulating interlayer hollow glass;

[0063] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 10 μm are coated on both sides of the prefabricated glass sheets;

[0064] The preparation method of the heat-insulating interlayer includes the following steps: tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 2.0 g / L; distilled water and dilute hydrochloric acid with a concentration of 0.2 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 20 °C for 1 hour to obtain an organosilicate sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is a benzotriazole-based ultraviolet absorber UVP-327; the organosilicate sol is coated on both surfaces of a polycarbonate plate to obtain a first layer; a PVB film is coated on both sides of the first layer to obtain a second layer; a PU film is coated on both surfaces of the second layer to obtain the heat-insulating interlayer;

[0065] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0066] In Examples 21-28, the concentrations of the tetraethyl orthosilicate solution and the dilute hydrochloric acid are shown in Table 5, and the remaining steps, operations, and Examples 20 are the same.

[0067] Table 5 Concentrations of tetraethyl orthosilicate solution and dilute hydrochloric acid in Examples 21-28

[0068]

[0069] Example 29

[0070] Detect the heat insulation performance of the heat-insulating interlayer insulating glass prepared in Examples 20-28 above. The heat insulation performance is characterized by the thermal conductivity. The detection method of the thermal conductivity is the heat flow meter method, and the instrument used is a heat flow sensor, model HFP-01. The detection results are shown in Table 6.

[0071] In Example 24 of the present invention, tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 2.2 g / L. Distilled water and dilute hydrochloric acid with a concentration of 0.5 mol / L are added to the tetraethyl orthosilicate solution. The organosilica sol prepared by the above preparation method is used to coat both surfaces of a polycarbonate plate to obtain a heat-insulating interlayer, which is hot-pressed onto both surfaces of a tempered glass sheet. Finally, the thermal conductivity of the prepared heat-insulating interlayer insulating glass is 0.9 W / (m 2 ·K). In the present invention, tetraethyl orthosilicate is used as the silicon source, which hydrolyzes into silanol under acidic conditions and then further crosslinks into a silica sol. The silica sol has a three-dimensional network structure. Adding a flame retardant and an ultraviolet absorber can enter the interior of the silica sol structure, making the flame retardant performance and ultraviolet absorption performance of the final organosilica sol more stable. In addition, the network structure of the organosilica sol can effectively limit the infrared thermal radiation of the ambient temperature, thereby reducing local heat conduction, and introducing an inert gas also has a certain heat insulation effect. The heat-insulating interlayer insulating glass prepared by the present invention can be used as building glass to achieve the effects of maintaining room temperature, reducing the air conditioner startup frequency, and saving energy.

[0072] Table 6 Thermal Conductivity of Insulating Glass Prepared in Examples 20-28

[0073] <![CDATA[Thermal conductivity (W / (m 2 ·K))]]> Example 20 1.0 Example 21 1.0 Example 22 1.1 Example 23 1.0 Example 24 0.9 Example 25 1.0 Example 26 1.1 Example 27 1.2 Example 28 1.1

[0074] Example 30

[0075] A preparation process for a heat-insulating interlayer insulating glass, comprising the following steps:

[0076] The glass substrate is cut according to the required size and then edge-ground to obtain edge-ground glass; the edge-ground glass is placed in a solvent and soaked and cleaned successively with water, sodium dodecyl sulfonate as a surfactant, acetone, and ethanol, and after cleaning, it is dried to obtain standby glass; the dried standby glass is semi-tempered to obtain tempered glass sheets; the semi-tempering treatment is to heat the dried standby glass at a temperature of 680 °C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds; the tempered glass sheets are first preheated at 180 °C, and then heat-insulating interlayers are hot-pressed on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; the hot pressing is carried out using a hot press; the temperature of the front roller of the hot press is 80 °C, the temperature of the rear roller is 190 °C, and the roller pressing speed is 0.8 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; two of the prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with spacer frames to form a hollow glass cavity; an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; and then it is sealed and fixed to obtain the heat-insulating interlayer hollow glass;

[0077] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 10 μm are coated on both sides of the prefabricated glass sheets;

[0078] The preparation method of the heat-insulating interlayer includes the following steps: tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 2.2 g / L; distilled water and dilute hydrochloric acid with a concentration of 0.5 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 50 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 20 °C for 1 hour to obtain an organosilicate sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is benzotriazole ultraviolet light absorber UVP-327; the organosilicate sol is coated on both surfaces of a polycarbonate plate to obtain a first layer; a PVB film is coated on both sides of the first layer to obtain a second layer; a PU film is coated on both surfaces of the second layer to obtain a heat-insulating interlayer;

[0079] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0080] In Examples 31-36, the stirring temperature and aging temperature for preparing the organosilicate sol are shown in Table 7, and the other reagents, operations are the same as in Example 30.

[0081] Table 7 Stirring temperature and aging temperature for preparing the organosilicate sol in Examples 31-36

[0082] Stirring Temperature (°C) Aging Temperature (°C) Example 31 40 80 Example 32 40 60 Example 33 50 60 Example 34 50 40 Example 35 60 40 Example 36 60 20

[0083] Example 37

[0084] The flame retardancy of the heat insulation interlayer prepared in Examples 30-36 above was detected. The flame retardancy was described by the vertical burning rating, and the test results are shown in Table 8.

[0085] In Example 32, tetraethyl orthosilicate solution and water provided an acidic condition through dilute hydrochloric acid. After stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber were added, and the mixture was aged at 60 °C for 1 hour to obtain a silicone sol; the flame retardant was a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber was the benzotriazole ultraviolet absorber UVP-327. The silicone sol obtained by the above method was finally coated on a polycarbonate plate, and the prepared heat insulation interlayer was hot-pressed on the two surfaces of a tempered glass sheet. The vertical burning rating of the obtained heat insulation interlayer was V-0 level, which could effectively prevent the spread of fire in case of a fire. The insulating glass prepared by the present invention consists of two prefabricated glass sheets, and heat insulation interlayers are hot-pressed on its two surfaces. The heat insulation interlayer contains silicone sol. By controlling the reaction temperature and aging temperature of the silicone sol, the finally obtained silicone sol can have a more regular spatial structure, which is beneficial to the dispersion of the flame retardant inside the silicone sol. Therefore, the finally prepared heat insulation interlayer has a flame retardant effect. When it is hot-pressed onto the exterior wall glass of a building, it can effectively block the temperature and the spread of fire, and improve the escape rate in case of a fire.

[0086] Table 8 Vertical burning ratings of the heat insulation interlayers prepared in Examples 30-36

[0087]

[0088]

[0089] Example 38

[0090] A preparation process of a heat insulation interlayer insulating glass includes the following steps:

[0091] The glass substrate is cut into the required size and then edge-ground to obtain edge-ground glass; the edge-ground glass is placed in a solvent and soaked and cleaned successively with water, sodium dodecyl sulfonate as a surfactant, acetone, and ethanol, and after cleaning, it is dried to obtain standby glass; the dried standby glass is semi-tempered to obtain tempered glass sheets; the semi-tempering process is to heat the dried standby glass at a temperature of 680 °C for 30 seconds and then instantaneously quench it with high-pressure air for 10 seconds; the tempered glass sheets are first preheated at 180 °C, and then heat-insulating interlayers are hot-pressed on both surfaces of the tempered glass sheets to obtain prefabricated glass sheets; the hot pressing is carried out using a hot press; the front roller temperature of the hot press is 80 °C, the rear roller temperature is 190 °C, and the roller pressing speed is 0.8 m / min; the hot pressing is carried out under the conditions of a temperature of 100 °C and a pressure of 1.2 Mpa for 3 hours; two of the prefabricated glass sheets are successively pushed into a dust-proof chamber and laminated and assembled together with spacer frames to form a hollow glass cavity; an inert gas is filled into the hollow glass cavity; the lamination and assembly are carried out in an environment with a temperature of 24 ± 3 °C and a relative humidity of 23% ± 5%; then it is sealed and fixed to obtain the heat-insulating interlayer hollow glass;

[0092] The thickness of the glass substrate is 6 mm; heat-insulating interlayers with a thickness of 15 μm are coated on both sides of the prefabricated glass sheets;

[0093] The preparation method of the heat-insulating interlayer includes the following steps: tetraethyl orthosilicate is dissolved in ethanol to obtain a tetraethyl orthosilicate solution with a concentration of 2.2 g / L; distilled water and dilute hydrochloric acid with a concentration of 0.5 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 40 °C for 3 hours, a flame retardant and an ultraviolet absorber are added and aged at 60 °C for 1 hour to obtain an organosilica sol; the flame retardant is a mixture of aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5; the ultraviolet absorber is a benzotriazole-based ultraviolet light absorber UVP-327; the organosilica sol is coated on both surfaces of a polycarbonate plate to obtain a first layer; a PVB film is coated on both sides of the first layer to obtain a second layer; a PU film is coated on both surfaces of the second layer to obtain the heat-insulating interlayer;

[0094] The thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

[0095] In Example 39, heat-insulating interlayers with a thickness of 20 μm are coated on both sides of the prefabricated glass sheets, and the other reagents, operations are the same as in Example 38.

[0096] In Example 40, heat-insulating interlayers with a thickness of 25 μm are coated on both sides of the prefabricated glass sheets, and the other reagents, operations are the same as in Example 38.

[0097] In Example 41, heat-insulating interlayers with a thickness of 30 μm are coated on both sides of the prefabricated glass sheets, and the other reagents, operations are the same as in Example 38.

[0098] In Example 42, a heat-insulating interlayer with a thickness of 20 μm was coated on one side of the prefabricated glass sheet, and the other reagents, operations were the same as in Example 38.

[0099] In Example 43, the PVB film was not coated, and the other reagents, operations were the same as in Example 38.

[0100] In Example 44, the PU film was not coated, and the other reagents, operations were the same as in Example 38.

[0101] Comparative Example 1

[0102] The heat-insulating interlayer was not hot-pressed, and the other reagents, operations were the same as in Example 39.

[0103] Comparative Example 2

[0104] Silicone sol was not added, and the other reagents, operations were the same as in Example 39.

[0105] Example 45

[0106] The ultraviolet ray cut-off rate of the heat-insulating interlayer insulating glass prepared in the above Examples 38-44 was detected, and the detection results are shown in Table 9. The ultraviolet ray cut-off rate is used to evaluate the ultraviolet ray-proof ability of the glass, and it is detected by an ultraviolet ray barrier rate tester, and the manufacturer is Dongguan Haotian Test Equipment Co., Ltd.

[0107] In Example 39, silicone sol was coated on both surfaces of the polycarbonate plate to obtain the first layer, PVB film was coated on both sides of the first layer to obtain the second layer, and PU film was coated on both surfaces of the second layer to obtain the heat-insulating interlayer, and heat-insulating interlayers with a thickness of 20 μm were coated on both sides of the prefabricated glass sheet, the thickness of the PVB film was 0.80 mm, and the thickness of the PU film was 1 mm. As Figure 1The following is a schematic diagram of the heat-insulating interlayer prepared by the present invention. Through the above-described preparation process, the finally prepared heat-insulating interlayer insulating glass can have a UV cut-off rate of 78% for ultraviolet rays with a wavelength of 350 nm. When preparing the silicone sol in the present invention, benzotriazole ultraviolet light absorber UVP-327 is added, which has good chemical stability and can absorb ultraviolet rays with wavelengths of 270-380 nm, enabling the finally prepared heat-insulating interlayer insulating glass to achieve a certain degree of UV blocking. And the silicone sol is located in the inner layer of the heat-insulating interlayer and will not be affected by long-term light irradiation. Ultraviolet irradiation can accelerate the aging of human skin. Therefore, good UV protection performance can protect the interior from ultraviolet irradiation; and a PVB film is coated in the heat-insulating interlayer. The PVB film can absorb impact energy. Even if the glass is damaged, its glass fragments will still stick to the intermediate film, which can reduce the probability of fragment splashing and improve the safety performance of the prepared glass. In Example 43, the heat-insulating interlayer prepared without coating the PVB film has glass fragments that are prone to splashing, posing a safety hazard. In Comparative Example 1, the heat-insulating interlayer is not hot-pressed, and its heat-insulating effect is poor, with a thermal conductivity of 1.4 W / (m 2 ·K). In Comparative Example 2, no silicone sol is added, and its thermal conductivity is 1.3 W / (m 2 ·K), indicating that the silicone sol plays an important role in the heat-insulating effect of the heat-insulating interlayer.

[0108] Table 9 UV cut-off rate of the insulating glass prepared in Examples 38-44

[0109]

[0110]

[0111] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions, and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A process for preparing heat-insulating laminated hollow glass, characterized in that: The following steps are involved: Cut the glass substrate according to the required size and perform edge grinding to obtain edged glass; soak the edged glass in a solvent with water, sodium dodecyl sulfate, acetone and ethanol in turn, wash it, and dry it after washing to obtain spare glass; heat the dried spare glass at 650-710°C for 20-60 seconds and then quench it instantly with high-pressure air for 10 seconds to obtain a tempered glass sheet; preheat the tempered glass sheet at 150-200°C, and then hot-press the two surfaces of the tempered glass sheet to obtain a prefabricated glass sheet, the hot pressing temperature is 100°C, the hot pressing pressure is 1.2MPa, and the hot pressing time is 3h; push two prefabricated glass sheets into a dustproof room in turn, stack and assemble them together with a spacing frame to form a hollow glass cavity, and fill the hollow glass cavity with inert gas; then seal and fix them to obtain the insulating interlayer hollow glass; The thickness of the glass substrate is 6 mm; both sides of the prefabricated glass sheet are coated with the thermal insulation interlayer with a thickness of 10 to 30 μm; The preparation method of the thermal insulation interlayer comprises the following steps: dissolving tetraethyl orthosilicate with a mass concentration of 1.8-3.7 g / L in ethanol to obtain a tetraethyl orthosilicate solution; Distilled water and dilute hydrochloric acid with a molar concentration of 0.2-1.1 mol / L are added to the tetraethyl orthosilicate solution, and after stirring at 40-60° C. for 3 hours, a flame retardant and a benzotriazole ultraviolet light absorber UVP-327 are added, and the mixture is aged at 20-80° C. for 1 hour to obtain an organic silica sol; the organic silica sol is applied to both surfaces of a polycarbonate board to obtain a first layer; PVB film is applied on both sides of the first layer to obtain a second layer; PU film is applied on both surfaces of the second layer to obtain a heat insulating interlayer; the flame retardant is obtained by mixing aluminum hydroxide and ammonium polyphosphate in a mass ratio of 1:1.5, the thickness of the PVB film is 0.80 mm, and the thickness of the PU film is 1 mm.

2. The process for preparing a heat-insulating laminated hollow glass according to claim 1, characterized in that: The lamination and bonding are carried out in an environment with a temperature of 24±3° C. and a relative humidity of 23%±5%.

3. The process for preparing a heat-insulating laminated hollow glass according to claim 1, characterized in that: The hot pressing adopts a hot press; the temperature of the front roller of the hot press is 80°C, the temperature of the rear roller is 190°C, and the roller speed is 0.5-1.5m / min.

4. A heat-insulating laminated hollow glass prepared by the process of claim 1, characterized in that: The heat-insulating laminated hollow glass is composed of two inner and outer prefabricated glass sheets, a spacing frame, and a hollow glass cavity located between the two prefabricated glass sheets; the prefabricated glass sheet is composed of two PU film layers, two PVB film layers, two organic silicon sol layers, and a polycarbonate board.

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