CN115302887A - Heat-insulation weather-resistant glass explosion-proof membrane and preparation method thereof - Google Patents
Heat-insulation weather-resistant glass explosion-proof membrane and preparation method thereof Download PDFInfo
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- CN115302887A CN115302887A CN202210843419.8A CN202210843419A CN115302887A CN 115302887 A CN115302887 A CN 115302887A CN 202210843419 A CN202210843419 A CN 202210843419A CN 115302887 A CN115302887 A CN 115302887A
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
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- Inorganic Chemistry (AREA)
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- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Joining Of Glass To Other Materials (AREA)
Abstract
The invention belongs to the technical field of high polymer material manufacturing, and particularly relates to a preparation method of a heat-insulating weather-resistant glass explosion-proof membrane, wherein S1, firstly, a yellowing-resistant TPU (thermoplastic polyurethane) film is prepared; s2, then, carrying out modification treatment on the surface of the obtained yellowing-resistant TPU film; s3, attaching the yellowing-resistant TPU film, the glass layer and the PET film together; and S4, finally, coating the heat shielding layer and the scratch-resistant layer on the film in sequence to obtain the heat-insulating weather-resistant glass explosion-proof film. According to the invention, the PET film and the glass layer are stably connected together by using the yellowing-resistant TPU film, and then the heat shielding layer and the photocuring surface scratch-resistant layer are sequentially coated on the PET film to complete the preparation of the heat-insulating weather-resistant glass explosion-proof film, so that the glass has better impact resistance and heat-insulating property, and also has good light modulation property, thereby being convenient for better meeting the use requirements.
Description
Technical Field
The invention relates to the technical field of polymer material manufacturing, in particular to a heat-insulating weather-resistant glass explosion-proof membrane and a preparation method thereof.
Background
In the explosion and traffic accidents of the vehicle glass, the glass fragments are most harmful to people, and the sticking of the high-performance explosion-proof film on the surface of the glass is the most effective way for guaranteeing the life safety in the accident. The product of the existing market is the traditional glass explosion-proof membrane, the explosion-proof membrane adopts the simple combination of two layers of thicker PET membranes, has certain anti-splashing effect through increasing the thickness, but has no explosion-proof effect at all, and the two layers of thicker hard and brittle PET base membranes are combined to be very easy to delaminate, the impact resistance is poor, and the explosion-proof membrane is very easy to run through. Meanwhile, in the use process of the vehicle glass, the high performance and the high functionalization of the explosion-proof film are urgent needs of the current market, and particularly, the explosion-proof film has good explosion-proof performance, and meanwhile, the heat insulation effect is endowed, so that energy can be saved, the dimming effect is endowed, dazzling glare can be prevented, the visual effect is enhanced, and a comfortable private space is easily created. At present, domestic glass film products only have single performance, and an explosion-proof film has certain impact resistance and does not have heat insulation and dimming functions; while the general glass film products have either only heat insulation performance or only light modulation performance. The number of domestic vehicles is huge, the requirements on vehicle use safety are higher and higher, the requirements on vehicle glass films are also higher and higher, products of high-performance heat-insulation dimming glass explosion-proof films are urgently needed, and the blank of the product field in China is filled.
Disclosure of Invention
Technical problem to be solved
Aiming at the defects of the prior art, the invention provides a heat-insulating weather-resistant glass explosion-proof membrane and a preparation method thereof, and solves the problems that a vehicle glass film only has impact resistance or dimming performance, and is single in performance and inconvenient to use.
(II) technical scheme
The invention specifically adopts the following technical scheme for realizing the purpose:
a preparation method of a heat-insulating weather-resistant glass explosion-proof membrane comprises the following steps:
s1, firstly, drying TPU in a vacuum oven at 80 ℃ for 4h,then the dried TPU and the prepared polyacrylic acid modified CeO 2 The anti-UV agent and the antioxidant lubricant are uniformly mixed together by stirring, a single-screw extruder is used for blending and extruding, the mixture is conveyed to a clothes hanger type sheet head through the melt plasticizing effect of a screw of the extruder, and a TPU sheet extruded from the head is finally wound through the cooling of a casting roller and the clamping of a clamping roller to obtain a yellowing-resistant TPU film;
s2, then, carrying out modification treatment on the surface of the obtained yellowing-resistant TPU film, and improving the bonding performance between the yellowing-resistant TPU film and the glass layer and between the yellowing-resistant TPU film and the PET film;
s3, respectively cleaning the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film with ethanol, then drying the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film in an oven at 80 ℃ for 4 hours, superposing the dried sample according to the basic structure of the heat-insulating weather-resistant glass explosion-proof film, then putting the superposed sample in a vacuum oven, heating the sample in a vacuum environment at 130 ℃ for 3 hours, and placing a 1kg weight on the sample in the heating process to accelerate air exhaust and promote adhesion;
and S4, finally, naturally cooling the heated sample to obtain the heat-insulating weather-resistant glass explosion-proof membrane.
Further, the polyacrylic acid modified CeO 2 The preparation steps are as follows:
s11, mixing citric acid and Ce (NO) 3 ) 3 .6H 2 Dissolving O in mixed solution of ethanol and water respectively, and waiting until citric acid solution and Ce (NO) are obtained 3 ) 3 .6H 2 O solution, wherein: citric acid and Ce (NO) 3 ) 3 .6H 2 The molar ratio of O is 3:1, and the volume ratio of ethanol to water is 1:1;
s12, adding the above Ce (NO) 3 ) 3 .6H 2 Heating and stirring the O solution in an oil bath at 55 ℃, dropwise adding a citric acid solution, and volatilizing the solvent by opening until the solution becomes gel;
s13, drying the gel at 115 ℃ for 10h, grinding the obtained solid into fine powder, calcining at 420 ℃ for 2h, grinding and crushing to obtain nano-scale CeO 2 A powder;
s14, weighing 0.5gCeO 2 Adding the powder into 10ml of toluene, and stirring for 30min by using ultrasonic waves to obtain a suspension;
s15, adding 1.5g of polyacrylic acid into ethylene glycol, introducing nitrogen, heating and stirring at 110 ℃ until the polyacrylic acid is completely dissolved, and adding CeO 2 The suspension is reacted for 50min, the temperature is adjusted to 220 ℃, the reaction is continued for 3h and then is finished, after the reactant is cooled to the room temperature, ethanol is added for precipitation, and the polyacrylic acid modified CeO is obtained after centrifugal washing and drying 2 。
Further, the surface of the yellowing-resistant TPU film is subjected to modification treatment, and the modification treatment comprises the following steps:
s21, firstly, preparing a silane coupling agent solution: wherein the mass fraction of the silane coupling agent is 1.5wt%, the mass fraction of the deionized water is 3.5wt%, the mass fraction of the absolute ethyl alcohol is 95wt%, and then a magnetic stirrer is utilized to obtain a silane coupling agent solution;
s22, drying the TPU in an oven at 80 ℃ for 4h, wiping the surface with absolute ethyl alcohol to remove dust, completely soaking the TPU in a silane coupling agent solution, dispersing silane coupling agent molecules more uniformly through ultrasonic treatment, cleaning and drying the ultrasonically treated film, and finally obtaining a finished product.
According to the heat-insulation weather-proof glass explosion-proof membrane prepared by the preparation method, the heat-insulation weather-proof glass explosion-proof membrane comprises a glass layer, a yellowing-resistant TPU thin film, a PET thin film, a heat shielding layer and a photocuring surface scratch-proof layer, and the glass layer, the yellowing-resistant TPU thin film, the PET thin film, the heat shielding layer and the photocuring surface scratch-proof layer are distributed layer by layer from bottom to top.
(III) advantageous effects
Compared with the prior art, the invention provides a heat-insulating weather-resistant glass explosion-proof membrane and a preparation method thereof, and the heat-insulating weather-resistant glass explosion-proof membrane has the following beneficial effects:
according to the invention, the PET film and the glass layer are stably connected together by using the yellowing-resistant TPU film, and then the heat shielding layer and the photocuring surface scratch-resistant layer are sequentially coated on the PET film to complete the preparation of the heat-insulating weather-resistant glass explosion-proof film, so that the glass has better impact resistance and heat-insulating property, and also has good light modulation property, thereby being convenient for better meeting the use requirements.
Drawings
FIG. 1 is a schematic structural view of an explosion-proof membrane for heat-insulating weather-resistant glass in the invention.
In the figure: 1. a glass layer; 2. a yellowing resistant TPU film; 3. a PET film; 4. a thermal barrier layer; 5. and (3) photocuring the surface scratch-resistant layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Examples
One embodiment of the invention provides: a preparation method of a heat-insulating weather-resistant glass explosion-proof membrane comprises the following steps:
s1, firstly, drying TPU in a vacuum oven at 80 ℃ for 4 hours, and then drying the dried TPU and prepared polyacrylic acid modified CeO 2 The anti-UV agent and the antioxidant lubricant are uniformly mixed together by stirring, a single-screw extruder is used for blending and extruding, the mixture is conveyed to a clothes hanger type sheet head through the melt plasticizing effect of a screw of the extruder, and a TPU sheet extruded from the head is finally wound through the cooling of a casting roller and the clamping of a clamping roller to obtain a yellowing-resistant TPU film;
wherein: TPU and prepared polyacrylic acid modified CeO 2 The anti-UV agent and the antioxidant lubricant comprise the following components in parts by weight: 85-95, 0.5-10, 0.3-5, 0.3-2 and 0.2-2;
the single screw extrusion temperature was: 160-200 ℃, and the single-screw extrusion speed is as follows: 40-60rpm, casting head temperature: 175-185 ℃, casting roll temperature: 30-50 ℃, and the rotating speed of the casting roller is as follows: 2-3m/min;
the yellowing-resistant TPU film is used as an intermediate layer material, an adhesive effect is achieved between the inorganic glass and the PET film, the inorganic glass and the PET film are stably connected together, and the integrity of the whole body is ensured;
s2, then, carrying out modification treatment on the surface of the obtained yellowing-resistant TPU film, and improving the bonding performance between the yellowing-resistant TPU film and the glass layer and between the yellowing-resistant TPU film and the PET film;
because the yellowing-resistant TPU film and the glass layer are bonded mainly by virtue of hydrogen bonds, but the strength of the hydrogen bonds is easily influenced by the environment, and the risk of weakening the bonding strength is easily caused in the actual use process, a covalent bond with more stable chemical property can be formed between the yellowing-resistant TPU film and the glass layer by modifying the surface of the yellowing-resistant TPU film, and the bonding performance between the yellowing-resistant TPU film and the PET film is further improved;
s3, respectively cleaning the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film with ethanol, then drying the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film in an oven at 80 ℃ for 4 hours, superposing the dried sample according to the basic structure of the heat-insulating weather-resistant glass explosion-proof film, then putting the superposed sample in a vacuum oven, heating the sample in a vacuum environment at 130 ℃ for 3 hours, and placing a 1kg weight on the sample in the heating process to accelerate air exhaust and promote adhesion;
and S4, finally, naturally cooling the heated sample to obtain the heat-insulating weather-resistant glass explosion-proof membrane.
Wherein, ceO modified by polyacrylic acid 2 The preparation steps are as follows:
s11, mixing citric acid and Ce (NO) 3 ) 3 .6H 2 Dissolving O in mixed solution of ethanol and water respectively, and waiting until citric acid solution and Ce (NO) are obtained 3 ) 3 .6H 2 O solution, wherein: citric acid and Ce (NO) 3 ) 3 .6H 2 The molar ratio of O is 3:1, and the volume ratio of ethanol to water is 1:1;
s12, adding the above Ce (NO) 3 ) 3 .6H 2 Heating and stirring the O solution in an oil bath at 55 ℃, dropwise adding a citric acid solution, and volatilizing the solvent by opening until the solution becomes gel;
s13, drying the gel at 115 ℃ for 10h, grinding the obtained solid into fine powder, calcining at 420 ℃ for 2h, and grinding the powderCrushing to obtain nano-grade CeO 2 Powder;
s14, weighing 0.5gCeO 2 Adding the powder into 10ml of toluene, and stirring for 30min by using ultrasonic waves to obtain a suspension;
s15, adding 1.5g of polyacrylic acid into ethylene glycol, introducing nitrogen, heating and stirring at 110 ℃ until the polyacrylic acid is completely dissolved, and adding CeO 2 The suspension is reacted for 50min, the temperature is adjusted to 220 ℃, the reaction is continued for 3h and then is finished, after the reactant is cooled to the room temperature, ethanol is added for precipitation, and the polyacrylic acid modified CeO is obtained after centrifugal washing and drying 2 。
The method comprises the following steps of modifying the surface of the yellowing-resistant TPU film:
s21, firstly, preparing a silane coupling agent solution: wherein the mass fraction of the silane coupling agent is 1.5wt%, the mass fraction of the deionized water is 3.5wt%, the mass fraction of the absolute ethyl alcohol is 95wt%, and then a magnetic stirrer is utilized to obtain a silane coupling agent solution;
s22, drying the TPU in an oven at 80 ℃ for 4h, wiping the surface with absolute ethyl alcohol to remove dust, completely soaking the TPU in a silane coupling agent solution, dispersing silane coupling agent molecules more uniformly through ultrasonic treatment, cleaning and drying the ultrasonically treated film, and finally obtaining a finished product.
The preparation method of the heat-shielding PET film comprises the following steps:
the raw material is sodium tungstate (Na) 2 WO 4. 2H 2 O) and cesium carbonate (Cs) 2 CO 3 ) The reducing agent is citric acid, and (Cs) is synthesized X WO 3 ) Nano powder, then utilizing ultrasonic wave technology to synthesize (Cs) X WO 3 ) The nano powder is subjected to ultra-fine treatment and simultaneously added with other auxiliary agents such as dispersant to obtain (Cs) X WO 3 ) Nano powder slurry, coating (Cs) X WO 3 ) The nano powder is uniformly coated on the surface of the PET material, and on the premise of meeting the requirement of light transmittance, the shielding of the PET film on the near infrared material is improved, so that the heat insulation effect is achieved;
deionized water is added into 100g of sodium tungstate dihydrate to prepare 0.5Treating with strong acid type cation exchange resin column to obtain tungstic acid sol, adding appropriate amount of reduction inducer (such as malic acid, citric acid, oxalic acid, etc.), adding appropriate amount of Cs 2 CO 3 Preparing a corresponding mixed solution, introducing the mixed solution into a high-pressure reaction kettle, heating to 180 ℃, keeping the hydrothermal time at 48 hours, carrying out ultrasonic oscillation on a hydrothermal product, purifying and drying to obtain Cs X WO 3 Taking the obtained product Cs X WO 3 Adding a certain amount of dispersing assistant into the hydroalcoholic solution, placing the mixture into a ball mill, adding zirconium balls into the mixture, grinding the mixture, performing suction filtration, and adding Cs obtained from polyvinyl alcohol (PVA) X WO 3 And (3) carrying out ultrasonic oscillation on the nano dispersion liquid to obtain functional dispersion liquid with better dispersibility and temperature property, then uniformly coating the functional dispersion liquid on the surface of the PET film, and putting the PET film into an oven at 80 ℃ for drying to obtain the heat-shielding PET film.
As shown in fig. 1, an embodiment of the present invention proposes: the heat-insulating weather-proof glass explosion-proof membrane prepared by the preparation method comprises a glass layer 1, a yellowing-resistant TPU thin film 2, a PET thin film 3, a heat shielding layer 4 and a photocuring surface scratch-resistant layer 5, wherein the glass layer 1, the yellowing-resistant TPU thin film 2, the PET thin film 3, the heat shielding layer 4 and the photocuring surface scratch-resistant layer 5 are distributed layer by layer from bottom to top.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (4)
1. The preparation method of the heat-insulating weather-resistant glass explosion-proof membrane is characterized by comprising the following steps of:
s1, firstly, drying TPU in a vacuum oven at 80 ℃ for 4h, and then dryingIs/are as followsTPU and prepared polyacrylic acid modified CeO 2 The anti-UV agent and the antioxidant lubricant are uniformly mixed together by stirring, a single-screw extruder is used for blending and extruding, the mixture is conveyed to a clothes hanger type sheet head through the melt plasticizing effect of a screw of the extruder, and a TPU sheet extruded from the head is finally wound through the cooling of a casting roller and the clamping of a clamping roller to obtain a yellowing-resistant TPU film;
s2, then, carrying out modification treatment on the surface of the obtained yellowing-resistant TPU film, and improving the bonding performance between the yellowing-resistant TPU film and the glass layer and between the yellowing-resistant TPU film and the PET film;
s3, respectively cleaning the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film with ethanol, then drying the glass layer, the photocuring surface anti-scratch layer, the PET film and the yellowing-resistant TPU film in an oven at 80 ℃ for 4 hours, superposing the dried sample according to the basic structure of the heat-insulating weather-resistant glass explosion-proof film, then putting the superposed sample in a vacuum oven, heating the sample in a vacuum environment at 130 ℃ for 3 hours, and placing a 1kg weight on the sample in the heating process to accelerate air exhaust and promote adhesion;
and S4, finally, naturally cooling the heated sample to obtain the heat-insulating weather-resistant glass explosion-proof membrane.
2. The method for preparing the explosion-proof membrane of the heat-insulating weather-proof glass as claimed in claim 1, which is characterized in that: the polyacrylic acid modified CeO 2 The preparation steps are as follows:
s11, mixing citric acid and Ce (NO) 3 ) 3 .6H 2 Dissolving O in mixed solution of ethanol and water, and waiting until citric acid solution and Ce (NO) 3 ) 3 .6H 2 O solution, wherein: citric acid and Ce (NO) 3 ) 3 .6H 2 The molar ratio of O is 3:1, and the volume ratio of ethanol to water is 1:1;
s12, adding the above Ce (NO) 3 ) 3 .6H 2 Heating and stirring the O solution in an oil bath at 55 ℃, dropwise adding a citric acid solution, and volatilizing the solvent by opening until the solution becomes gel;
s13, drying the gel at 115 ℃ for 10h, and grinding the obtained solidPulverizing into fine powder, calcining at 420 deg.C for 2 hr, grinding and pulverizing to obtain nano-grade CeO 2 A powder;
s14, weighing 0.5gCeO 2 Adding the powder into 10ml of toluene, and stirring for 30min by using ultrasonic waves to obtain a suspension;
s15, adding 1.5g of polyacrylic acid into ethylene glycol, introducing nitrogen, heating and stirring at 110 ℃ until the polyacrylic acid is completely dissolved, and adding CeO 2 The suspension liquid reacts for 50min, the temperature is adjusted to 220 ℃, the reaction is continued for 3h and then is finished, after the reactant is cooled to the room temperature, ethanol is added for precipitation, and polyacrylic acid modified CeO is obtained after centrifugal washing and drying 2 。
3. The method for preparing the heat-insulating weather-proof glass explosion-proof membrane according to claim 1, characterized in that: the modifying treatment steps of the surface of the yellowing-resistant TPU film are as follows:
s21, firstly, preparing a silane coupling agent solution: wherein the mass fraction of the silane coupling agent is 1.5wt%, the mass fraction of the deionized water is 3.5wt%, the mass fraction of the absolute ethyl alcohol is 95wt%, and then a magnetic stirrer is utilized to obtain a silane coupling agent solution;
s22, drying the TPU in an oven at 80 ℃ for 4h, wiping the surface with absolute ethyl alcohol to remove dust, completely soaking the TPU in a silane coupling agent solution, dispersing silane coupling agent molecules more uniformly through ultrasonic treatment, cleaning and drying the ultrasonically treated film, and finally obtaining a finished product.
4. The heat-insulating weather-resistant glass rupture membrane prepared by the preparation method according to any one of claims 1 to 3, wherein: the heat-insulating weather-proof glass explosion-proof membrane comprises a glass layer (1), a yellowing-resistant TPU film (2), a PET film (3), a heat shielding layer (4) and a photocuring surface scratch-resistant layer (5), and the glass layer (1), the yellowing-resistant TPU film (2), the PET film (3), the heat shielding layer (4) and the photocuring surface scratch-resistant layer (5) are distributed layer by layer from bottom to top.
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| EP3243652A1 (en) * | 2016-05-11 | 2017-11-15 | Covestro Deutschland AG | Thermoplastic carrier/glass composite |
| EP3912808A1 (en) * | 2020-04-21 | 2021-11-24 | Implanta Beteiligungs-GmbH | Multilayered protective glass composite, display device with a dimensionally flexible display element and a protective glass composite of this type fixed to the display element, and use of a thin glass sheet as protective glass |
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