CN113999407A - Temperature-sensitive intelligent Low-E glass and preparation method and application thereof - Google Patents
Temperature-sensitive intelligent Low-E glass and preparation method and application thereof Download PDFInfo
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- CN113999407A CN113999407A CN202111368607.1A CN202111368607A CN113999407A CN 113999407 A CN113999407 A CN 113999407A CN 202111368607 A CN202111368607 A CN 202111368607A CN 113999407 A CN113999407 A CN 113999407A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/52—Amides or imides
- C08F220/54—Amides, e.g. N,N-dimethylacrylamide or N-isopropylacrylamide
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- E—FIXED CONSTRUCTIONS
- E06—DOORS, WINDOWS, SHUTTERS, OR ROLLER BLINDS IN GENERAL; LADDERS
- E06B—FIXED OR MOVABLE CLOSURES FOR OPENINGS IN BUILDINGS, VEHICLES, FENCES OR LIKE ENCLOSURES IN GENERAL, e.g. DOORS, WINDOWS, BLINDS, GATES
- E06B3/00—Window sashes, door leaves, or like elements for closing wall or like openings; Layout of fixed or moving closures, e.g. windows in wall or like openings; Features of rigidly-mounted outer frames relating to the mounting of wing frames
- E06B3/66—Units comprising two or more parallel glass or like panes permanently secured together
- E06B3/67—Units comprising two or more parallel glass or like panes permanently secured together characterised by additional arrangements or devices for heat or sound insulation or for controlled passage of light
- E06B3/6715—Units comprising two or more parallel glass or like panes permanently secured together characterised by additional arrangements or devices for heat or sound insulation or for controlled passage of light specially adapted for increased thermal insulation or for controlled passage of light
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2333/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
- C08J2333/24—Homopolymers or copolymers of amides or imides
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
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Abstract
The invention discloses temperature-sensitive intelligent Low-E glass and a preparation method and application thereof. Compared with the prior art, the invention has the following advantages: (1) the temperature-sensitive intelligent Low-E glass has good light transmission at Low temperature, can isolate part of infrared light, and can isolate light transmission by opacification at high temperature so as to regulate and control light heat transmission; (2) the hydrogel filler is sealed in the middle of the quartz glass, so that the hydrogel filler has good recycling effect, strong repeatability and stability and no secondary pollution; (3) the preparation method is simple and high in yield.
Description
Technical Field
The invention belongs to the technical field of Low-E glass fillers, and relates to a composite hydrogel material responding to environmental temperature, in particular to temperature-sensitive intelligent Low-E glass and a preparation method and application thereof.
Background
According to the research report of the energy consumption of the Chinese buildings, the energy consumption of the buildings in China accounts for 46.5 percent of the total energy consumption of the country, and the windows, which are the lowest energy efficiency parts of the buildings, have great potential in the energy-saving market. The traditional energy-saving glass has single function and limited application, and both the hollow glass utilizing a hollow low heat transfer system for heat insulation and the reflective glass for adjusting the solar energy transmission capacity only isolate the environments on two sides of the glass, so that the intelligent energy transfer cannot be smoothly realized.
Disclosure of Invention
The technical problem to be solved is as follows: in order to overcome the defects of the prior art, the intelligent Low-E glass and the temperature-sensitive intelligent Low-E glass which can change the properties of the glass according to environmental changes and reduce energy consumption, and the preparation method and the application thereof are obtained.
The technical scheme is as follows: the temperature-sensitive intelligent Low-E glass comprises double layers of quartz glass and hydrogel filled between the double layers of quartz glass; the hydrogel takes N-isopropyl acrylamide and acrylamide as substrates, is initiated and assembled by ammonium persulfate and tetramethylethylenediamine to form thermal response hydrogel, and then the thermal response hydrogel is mixed with a tin antimony oxide solution according to the volume ratio of 1:1-20 to obtain the hydrogel; wherein, the concentration of N-isopropyl acrylamide in the thermal response hydrogel is 0.05-0.15g/mL, the concentration of acrylamide is 0.01-0.05g/mL, and the concentration of tin antimony oxide in the tin antimony oxide solution is 0.01-0.08 g/mL.
The preparation method of the temperature-sensitive intelligent Low-E glass comprises the following steps:
s1, adding N-isopropyl acrylamide and acrylamide into water to dissolve, adding ammonium persulfate, fully mixing, then adding tetramethyl ethylenediamine, and placing the solution at normal temperature until the solution is transparent after gelation to obtain thermal response hydrogel;
s2, mixing tin particles, antimony trioxide powder and concentrated sulfuric acid, carrying out high-temperature oil bath reaction until the particles are dissolved, then pouring hydrogen peroxide and water under an ice bath condition, adding the mixture into a reaction kettle, carrying out reaction in a high-temperature oven, and carrying out centrifugal washing and drying to obtain tin antimony oxide powder;
s3, adding tin antimony oxide powder into water, adding triethylamine, mixing uniformly to obtain a tin antimony oxide solution, mixing with the thermal response hydrogel, standing after mixing uniformly, filling the product between double layers of quartz glass, and sealing to obtain the temperature-sensitive intelligent Low-E glass.
Preferably, the mass ratio of ammonium persulfate in S1 to the volume ratio of the base polymer solution is 0.1-0.5g:10mL, and the volume ratio of tetramethylethylenediamine to the base polymer solution is 1: 20-50.
Preferably, the mass ratio of the tin particles to the antimony trioxide in S2 is 1:0.2-0.5, the mass ratio of the tin particles to the sulfuric acid is 1g:5-10mL, the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 1:1-3, and the volume ratio of the concentrated sulfuric acid to the water is 1: 1-3.
Preferably, the oil bath temperature in S2 is 90-98 ℃, the ice-bath reaction time is 20-30min, and the hydrothermal reaction temperature in the reaction kettle is 150-200 ℃.
Preferably, the volume ratio of the mass of the tin antimony oxide to the water in the tin antimony oxide solution in S3 is 0.5-2g:20mL, and the volume ratio of the mass of the tin antimony oxide to the triethylamine is 0.5-2g: 200. mu.L.
Preferably, the volume ratio of the tin antimony oxide solution to the thermal response hydrogel in S3 is 1: 2-10.
Preferably, the volume ratio of the tin antimony oxide solution to the thermal response hydrogel in S3 is 1: 3-9.
The temperature-sensitive intelligent Low-E glass is applied to the preparation of windows capable of intelligently identifying the environmental temperature and changing the self heat insulation property.
Preferably, the intelligent recognition of the ambient temperature and the change of the self-heat insulation property are high transmittance and low heat insulation rate under low temperature condition and low transmittance and high heat insulation rate under high temperature condition.
The principle of the temperature-sensitive intelligent Low-E glass provided by the invention is as follows: the thermal response hydrogel synthesized by N-isopropyl acrylamide has good hydrophilicity at low temperature to form a transparent state due to the phenomenon of low critical solution temperature, is beneficial to transmitting heat energy by infrared light transmission, has hydrophobicity at high temperature and is contracted into an opaque state to block the infrared light transmission and reduce the heat energy transmission. And the high crystal grain conductivity of the tin antimony oxide ensures that the crystal grain has excellent characteristics of metal-like conductivity and high infrared light reflectivity while keeping high visible light transmissivity, further reduces the transmission efficiency of infrared light and ultraviolet light of hydrogel in a transparent state, enhances the isolation efficiency of the temperature-sensitive intelligent Low-E glass, and can achieve the effect of being warm in winter and cool in summer in application of building glass.
Has the advantages that: (1) the temperature-sensitive intelligent Low-E glass has good light transmission at Low temperature, can isolate part of infrared light, and can isolate light transmission by opacification at high temperature so as to regulate and control light heat transmission; (2) the hydrogel filler is sealed in the middle of the quartz glass, so that the hydrogel filler has good recycling effect, strong repeatability and stability and no secondary pollution; (3) the preparation method is simple and high in yield.
Drawings
FIG. 1 is a pictorial view of the temperature sensitive smart Low-E glass of example 1;
FIG. 2 is a transmission electron microscope photograph of the hydrogel filler of example 1;
FIG. 3 is an X-ray diffraction pattern of antimony tin oxide of example 1;
FIG. 4 shows the IR radiation blocking effect of the temperature sensitive smart Low-E glass of example 1;
FIG. 5 is a graph showing the change in transparency of the temperature-sensitive smart Low-E glass of example 1 after cycling at Low and high temperatures;
FIG. 6 is a graph showing the effect of temperature sensitive smart Low-E glasses of examples 1 to 7 on blocking infrared radiation.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
(1) Preparation of thermally responsive hydrogels
Firstly weighing 3g N-isopropyl acrylamide and 1g acrylamide, dissolving in 30mL ultrapure water, ultrasonically mixing for 30 minutes, then weighing 1g ammonium persulfate, dissolving in the solution, ultrasonically treating for 30 minutes, injecting 1mL tetramethyl ethylene diamine, reacting for 30 minutes, and standing at 27 ℃ to obtain the transparent thermal response hydrogel.
(2) Synthesis of tin antimony oxide powder
Weighing 1g of tin granules and 0.5g of antimony trioxide powder, placing the tin granules and the antimony trioxide powder in a three-neck flask, adding 8mL of concentrated sulfuric acid, heating and stirring at 95 ℃ for 36H, then completely mixing in an ice-water bath, and adding 32mL of H2O2The reaction was carried out for 20min, and 24mL of H was added2And (3) reacting for 20min, after the reaction is finished, putting the solution into a reaction kettle, reacting for 10h at 160 ℃, centrifugally separating the mixed liquid after the reaction is finished, drying the obtained solid, and grinding the solid into powder to obtain the tin antimony oxide powder.
(3) Filling to obtain the temperature-sensitive intelligent Low-E glass
Putting 1g of tin antimony oxide powder into 17mL of ultrapure water, then adding 200 mu L of triethylamine into the ultrapure water, and dispersing the tin antimony oxide into the ultrapure water after violent shaking to obtain a tin antimony oxide solution. And mixing 17mL of tin antimony oxide solution with 3mL of thermal response hydrogel, and performing ultrasonic treatment for 20min to obtain the hydrogel filler. And filling 5mL of filler into the space between two pieces of quartz glass of 5 multiplied by 5cm, and sealing the seal to obtain the temperature-sensitive intelligent Low-E glass.
FIG. 1 is a diagram of a temperature-sensitive intelligent Low-E glass in example 1, which is transparent at room temperature and does not affect the lighting of the visual field.
Fig. 2 is a transmission electron microscope image of the hydrogel filler in example 1, which shows that tin antimony oxide is uniformly distributed in the hydrogel, no aggregation effect occurs, reflection of infrared light caused by aggregation of nano materials is avoided, and the absorption effect is reduced.
FIG. 3 is an X-ray diffraction pattern of antimony tin oxide of example 1, with diffraction peaks and SnO at 2 θ values of 26.59 °, 33.77 °, 37.98 °, 51.70 ° and 65.27 ° for ATO2The diffraction planes of (110), (101), (200), (211) and (112) are identical, and these characteristic peaks indicate that the Sn element has been successfully incorporated into antimony trioxide to form antimony tin oxide.
Fig. 4 shows the infrared radiation blocking effect of the temperature-sensitive intelligent Low-E glass in example 1, the prepared filling liquid is filled between the glasses, a xenon lamp is used to simulate solar light irradiation, an infrared measuring instrument is placed at a target position, the change of the infrared radiation blocking rate of the glass caused by the temperature change under the illumination condition is calculated by recording the infrared radiation of the target position at different time periods, and it can be seen that the filling liquid increases the infrared radiation blocking rate of the double-layer glass from 12.38% to 85.22%, the glass becomes opaque after the temperature is increased from 25 ℃ to 40 ℃, the infrared radiation blocking rate is gradually increased from 70.54% to 76.34%, and finally reaches 85.22% at 45 ℃; when the temperature is reduced, the filling liquid gradually restores the original transparent state, and when the temperature is reduced to 35 ℃, the infrared radiation blocking rate of the glass is also gradually reduced, from 85.22% to 72.17%, and finally the state of the glass is restored to 25 ℃ and is 70.35%. The specific variation is shown in the following table:
FIG. 5 shows the change of transparency of the temperature-sensitive intelligent Low-E glass in example 1 after Low-temperature and high-temperature cycles, wherein the glass is transparent at normal temperature, and becomes opaque after continuous illumination and temperature rise, and the transparency is recovered after temperature recovery.
Example 2
The difference between this example and example 1 is step (1): weighing 2g N-isopropyl acrylamide and 1g acrylamide, dissolving in 30mL ultrapure water, ultrasonically mixing for 30 minutes, weighing 1g ammonium persulfate, dissolving in the solution, ultrasonically treating for 30 minutes, injecting 1mL tetramethyl ethylenediamine, reacting for 30 minutes, and standing at 27 ℃ to obtain the transparent thermal response hydrogel.
Example 3
The difference between this example and example 1 is step (1): weighing 4g N-isopropyl acrylamide and 1g acrylamide, dissolving in 30mL ultrapure water, ultrasonically mixing for 30 minutes, weighing 1g ammonium persulfate, dissolving in the solution, ultrasonically treating for 30 minutes, injecting 1mL tetramethyl ethylenediamine, reacting for 30 minutes, and standing at 27 ℃ to obtain the transparent thermal response hydrogel.
Example 4
The difference between this example and example 1 is step (2): weighing 1g of tin granules and 0.25g of antimony trioxide powder, placing the tin granules and the antimony trioxide powder in a three-neck flask, adding 8mL of concentrated sulfuric acid, heating and stirring at 95 ℃ for 36H, then completely mixing in an ice-water bath, and adding 32mL of H2O2The reaction was carried out for 20min, and 24mL of H was added2And (3) reacting for 20min, after the reaction is finished, putting the solution into a reaction kettle, reacting for 10h at 160 ℃, centrifugally separating the mixed liquid after the reaction is finished, drying the obtained solid, and grinding the solid into powder to obtain the tin antimony oxide powder.
Example 5
The difference between this example and example 1 is step (2): weighing 1g of tin granules and 0.75g of antimony trioxide powder, placing the tin granules and the antimony trioxide powder into a three-neck flask, adding 8mL of concentrated sulfuric acid, heating and stirring at 95 ℃ for 36H, then completely mixing in an ice-water bath, and adding 32mL of H2O2The reaction was carried out for 20min, and 24mL of H was added2O reaction for 20min, after finishingAnd putting the solution into a reaction kettle to react for 10 hours at 160 ℃, centrifugally separating the mixed liquid after the reaction is finished, drying the obtained solid, and grinding the solid into powder to obtain the tin antimony oxide powder.
Example 6
The difference between this example and example 1 is step (3): putting 1g of tin antimony oxide powder into 18mL of ultrapure water, then adding 200 mu L of triethylamine into the ultrapure water, and dispersing the tin antimony oxide into the ultrapure water after violent shaking to obtain a tin antimony oxide solution. And (3) mixing 18mL of tin antimony oxide solution with 2mL of thermal response hydrogel, and performing ultrasonic treatment for 20min to obtain the hydrogel filler. And filling 5mL of filler into the space between two pieces of quartz glass of 5 multiplied by 5cm, and sealing the seal to obtain the temperature-sensitive intelligent Low-E glass.
Example 7
The difference between this example and example 1 is step (3): putting 1g of tin antimony oxide powder into 16mL of ultrapure water, then adding 200 mu L of triethylamine into the ultrapure water, and dispersing the tin antimony oxide into the ultrapure water after violent shaking to obtain a tin antimony oxide solution. And mixing 16mL of tin antimony oxide solution with 4mL of thermal response hydrogel, and performing ultrasonic treatment for 20min to obtain the hydrogel filler. And filling 5mL of filler into the space between two pieces of quartz glass of 5 multiplied by 5cm, and sealing the seal to obtain the temperature-sensitive intelligent Low-E glass.
FIG. 6 is a graph comparing the infrared radiation blocking effect of the temperature-sensitive smart Low-E glasses of examples 1-7, and it can be seen from the graph (a) that the infrared blocking effect of examples 1, 2 and 3 is similar at Low temperature, and the effect of example 2 is relatively poor at high temperature, because the blocking efficiency at high temperature mainly depends on the concentration of N-isopropylacrylamide in the hydrogel, which determines the high-temperature hydrophobicity and the degree of crosslinking of the hydrogel, and the higher the concentration is, the more obvious the hydrophobic effect at high temperature is, and the stronger the impermeability is. It can be seen from the graph (b) that the infrared blocking effect of example 4 is the worst at low temperature, probably because when the content of antimony trioxide powder is too low, the crystal form of the generated tin antimony oxide is not good, and the absorption and reflection performance of the material to infrared light is affected. In the graph (c), the performance of the temperature-sensitive intelligent Low-E glass is researched by changing the mixture ratio of the tin antimony oxide solution and the thermal response hydrogel, and it can be seen that the example 7 has good effect because the concentration of the N-isopropylacrylamide in the filler is also determined, and the thermal hydrophobicity of the hydrogel is more difficult to show in the filler as the concentration of the thermal response hydrogel after being diluted is smaller.
Claims (10)
1. The temperature-sensitive intelligent Low-E glass is characterized by comprising double-layer quartz glass and hydrogel filled between the double-layer quartz glass; the hydrogel takes N-isopropyl acrylamide and acrylamide as substrates, is initiated and assembled by ammonium persulfate and tetramethylethylenediamine to form thermal response hydrogel, and then the thermal response hydrogel is mixed with a tin antimony oxide solution according to the volume ratio of 1:1-20 to obtain the hydrogel; wherein, the concentration of N-isopropyl acrylamide in the thermal response hydrogel is 0.05-0.15g/mL, the concentration of acrylamide is 0.01-0.05g/mL, and the concentration of tin antimony oxide in the tin antimony oxide solution is 0.01-0.08 g/mL.
2. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 1, characterized in that the method comprises the following steps:
s1, adding N-isopropyl acrylamide and acrylamide into water to dissolve, adding ammonium persulfate, fully mixing, then adding tetramethyl ethylenediamine, and placing the solution at normal temperature until the solution is transparent after gelation to obtain thermal response hydrogel;
s2, mixing tin particles, antimony trioxide powder and concentrated sulfuric acid, carrying out high-temperature oil bath reaction until the particles are dissolved, then pouring hydrogen peroxide and water under an ice bath condition, adding the mixture into a reaction kettle, carrying out reaction in a high-temperature oven, and carrying out centrifugal washing and drying to obtain tin antimony oxide powder;
s3, adding tin antimony oxide powder into water, adding triethylamine, mixing uniformly to obtain a tin antimony oxide solution, mixing with the thermal response hydrogel, standing after mixing uniformly, filling the product between double layers of quartz glass, and sealing to obtain the temperature-sensitive intelligent Low-E glass.
3. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 2, wherein the volume ratio of the mass of ammonium persulfate to the volume of the base polymer solution in S1 is 0.1-0.5g:10mL, and the volume ratio of tetramethylethylenediamine to the volume of the base polymer solution is 1: 20-50.
4. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 2, wherein the mass ratio of the tin particles to the antimony trioxide in S2 is 1:0.2-0.5, the mass ratio of the tin particles to the sulfuric acid is 1g:5-10mL, the volume ratio of the concentrated sulfuric acid to the hydrogen peroxide is 1:1-3, and the volume ratio of the concentrated sulfuric acid to the water is 1: 1-3.
5. The method for preparing temperature-sensitive intelligent Low-E glass according to claim 2, wherein the oil bath temperature in S2 is 90-98 ℃, the ice bath reaction time is 20-30min, and the hydrothermal reaction temperature in the reaction kettle is 150-200 ℃.
6. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 2, wherein the volume ratio of the mass of tin antimony oxide to water in the tin antimony oxide solution in S3 is 0.5-2g:20mL, and the volume ratio of the mass of tin antimony oxide to triethylamine is 0.5-2g:200 μ L.
7. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 2, wherein the volume ratio of the tin antimony oxide solution to the thermal response hydrogel in S3 is 1: 2-10.
8. The preparation method of the temperature-sensitive intelligent Low-E glass according to claim 2, wherein the volume ratio of the tin antimony oxide solution to the thermal response hydrogel in S3 is 1: 3-9.
9. The use of the temperature-sensitive smart Low-E glass of claim 1 in the manufacture of a window for intelligently identifying ambient temperature and altering self-insulating properties.
10. The use according to claim 9, wherein the smart identification of ambient temperature and the change of self-insulating properties is the possession of high transmittance and low insulating rate under low temperature condition and low transmittance and high insulating rate under high temperature condition.
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| CN115653457A (en) * | 2022-11-01 | 2023-01-31 | 福州大学 | Preparation method of gel-based intelligent window |
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