Disclosure of Invention
The invention aims to provide SGP film laminated glass and a production process thereof, which solve the problem that the heat insulation effect of films in the SGP film laminated glass at the present stage is common.
The aim of the invention can be achieved by the following technical scheme:
a production process of SGP film laminated glass specifically comprises the following steps:
Step S1, mixing a modified prepolymer, ethylenediamine and DMF (dimethyl formamide), introducing nitrogen for protection, reacting for 2-3 hours at the rotating speed of 150-200r/min and the temperature of 30-40 ℃, adding KH560, adjusting the pH value to 11-12, reacting for 3-5 hours to obtain pretreated polyurethane, mixing pretreated polyurethane, diphenylmethane diisocyanate and DMF, introducing nitrogen for protection, reacting for 5-6 hours at the rotating speed of 150-200r/min and the temperature of 30-40 ℃, adding N- (2-hydroxyethyl) maleimide, and continuing to react for 4-6 hours to obtain modified polyurethane;
And S2, uniformly mixing modified polyurethane, modified filler, dimethyl diethoxysilane, ethanol and DMF (dimethyl formamide), stirring and adding deionized water and hydrochloric acid at the rotating speed of 120-150r/min and the temperature of 65-70 ℃ for reaction for 2-3 hours, adding tetrabutyl titanate, continuing to react for 2-3 hours, heating to 120-130 ℃ for reaction for 3-5 hours to obtain modified resin, mixing the modified resin, SGP laminating resin and dicumyl peroxide, extruding and casting to form a film at the feeding section temperature of 190 ℃ and the melting section temperature of 180 ℃ and the discharging section temperature of 150 ℃ to obtain laminated glass, and placing the laminated glass between two pieces of glass for high-temperature pressing to obtain the SGP laminated glass.
The molar ratio of the isocyanate groups to the ethylenediamine on the modified prepolymer in the step S1 is 1:1, and the hydroxyl groups, the diphenylmethane diisocyanate and the N- (2-hydroxyethyl) maleimide n:2 on the pretreated polyurethane are natural numbers larger than 1.
The dosage ratio of the modified polyurethane to the modified filler to the dimethyl diethoxysilane to the ethanol to the DMF to the deionized water to the hydrochloric acid solution to the tetrabutyl titanate is 5g:80mg:1mmo l:10mL:50mL:20mL:3mL:1.5mmo l, the mass fraction of the hydrochloric acid solution is 10%, and the weight ratio of the modified resin to the SGP laminating resin is 30-50:80-100:1-3.
Further, the modified prepolymer is prepared by the following steps:
Uniformly mixing p-chloro-o-nitroaniline, p-hydroxystyrene, sodium nitrite and potassium hydrogen sulfate, placing in a mortar, grinding for 20-30min at the temperature of 20-25 ℃ to obtain azo dye, uniformly mixing the azo dye, ethanol and sodium hydroxide solution, stirring at the rotating speed of 600-800r/min and the temperature of 80-85 ℃ and adding sodium dithionite, and reacting for 1-1.5h to obtain an intermediate 1;
Step A2, uniformly mixing metal magnesium, iodine and tetrahydrofuran, introducing nitrogen for protection, stirring and adding 2-bromothiophene at the rotation speed of 60-80r/min and the temperature of 20-25 ℃, heating to 60-70 ℃ for reaction for 3-5h to obtain an intermediate 2, uniformly mixing the intermediate 1, the intermediate 2 and the tetrahydrofuran, and reacting for 5-6h at the rotation speed of 150-200r/min and the temperature of 60-70 ℃ to obtain a modifier;
And step A3, uniformly mixing a modifier, diethanolamine and DMF, introducing nitrogen for protection, stirring and adding sodium hydroxide to a pH value of 10-11 under the conditions of a rotating speed of 120-150r/min and a temperature of 20-25 ℃ for reaction for 3-5 hours, regulating the pH value to be neutral to obtain a modified monomer, mixing the modified monomer, diphenylmethane diisocyanate and DMF, and reacting for 2-4 hours under the conditions of a rotating speed of 120-150r/min and a temperature of 40-50 ℃ to obtain the modified prepolymer.
Further, the molar ratio of the p-chloro-o-nitroaniline to the p-hydroxystyrene to the sodium nitrite to the potassium bisulfate in the step A1 is 1:1.1:1:1, and the dosage ratio of the azo dye to the ethanol to the sodium hydroxide solution to the sodium dithionite is 25mmo l:50mL:50mL:82mmo l.
Further, the dosage ratio of magnesium metal, iodine, tetrahydrofuran and 2-bromothiophene in the step A2 is 1.1mo l:1mo l:100mL:1mo l, and the molar ratio of the intermediate 1 to the intermediate 2 is 1:1.
Further, the molar ratio of the modifier to the diethanolamine in the step A3 is 1:1, and the molar ratio of the modified monomer to the diphenylmethane diisocyanate is 1:2.1.
Further, the modified filler is prepared by the following steps:
uniformly mixing triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate and deionized water, stirring at the rotating speed of 150-200r/min and the temperature of 80-85 ℃, adding tetraethoxysilane, KH550 and ethanol, reacting for 4-6 hours, centrifuging to remove a supernatant, adding a substrate into a hydrochloric acid solution, performing ultrasonic treatment at the frequency of 20-30kHz and the temperature of 20-25 ℃ for 5-10 minutes, heating to 60-70 ℃, and preserving heat for 5-7 hours to obtain the aminated nano silicon dioxide;
And B2, uniformly mixing the amination nano silicon dioxide, the stannic chloride and the ethanol, stirring and adding deionized water and ammonia water to a pH value of 10-12 at a rotating speed of 120-150r/min and a temperature of 30-40 ℃, stirring for 10-15min, heating to 150-160 ℃ for reaction for 20-25h to obtain the modified nano silicon dioxide, dispersing the modified nano silicon dioxide in the ethanol, introducing nitrogen for protection, stirring and adding 3-isocyanatopropyl triethoxysilane at a rotating speed of 300-500r/min and a temperature of 30-40 ℃ for reaction for 2-3h, and obtaining the modified filler.
Further, the dosage ratio of triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate, deionized water, ethyl orthosilicate, KH550 and ethanol in the step B1 is 65mg:380mg:550mg:25mL:10mmo l:5mmo l:5mL, the dosage ratio of the base material and the hydrochloric acid solution is 1mg to 1mL, and the mass fraction of the hydrochloric acid solution is 5%.
Further, the dosage ratio of the amination nano silicon dioxide to the stannic chloride to the ethanol to the deionized water in the step B2 is 2g:2mmo l:10mL:10mL, and the molar ratio of the amino group on the surface of the modified nano silicon dioxide to the 3-isocyanatopropyl triethoxysilane is 1:1.
The SGP film laminated glass has the beneficial effects that the laminated glass is prepared by mixing and extruding modified resin and SGP laminated resin to form a film, the laminated film is arranged between two pieces of glass and pressed at high temperature, the modified resin takes modified prepolymer and ethylenediamine as raw materials, isocyanate groups on the modified prepolymer react with amino groups on ethylenediamine to form amino end caps, the amino end caps react with KH560 to react epoxy groups on KH560 with amino groups to prepare pretreated polyurethane, the pretreated polyurethane reacts with diphenylmethane diisocyanate to react hydroxyl groups on the pretreated polyurethane with isocyanate groups on the diphenylmethane diisocyanate, the N- (2-hydroxyethyl) maleimide end caps are used to prepare modified polyurethane, and the modified polyurethane, modified filler, dimethyl diethoxysilane and tetrabutyl titanate are hydrolyzed and condensed to prepare the modified resin.
The modified prepolymer takes p-chloro-o-nitroaniline and p-hydroxy-styrene as raw materials, azo dye is formed under the action of sodium nitrite and potassium bisulfate, the azo dye is treated by sodium dithionite to form a benzotriazole structure to prepare an intermediate 1, magnesium metal and iodine are treated by 2-bromothiophene to form thienyl magnesium bromide to prepare an intermediate 2, the intermediate 1 and the intermediate 2 are reacted to enable chlorine atom sites on the intermediate 1 to react with magnesium bromide on the intermediate 2 to prepare a modifier, the modifier and ethylene glycol amine are reacted to enable double bonds on the modifier and secondary amine on the ethylene glycol amine to be Michael-added to prepare a modified monomer, and the modified monomer and diphenylmethane diisocyanate are reacted to prepare the modified prepolymer.
The modified filler is prepared by polycondensation of tetraethoxysilane and KH550 serving as raw materials, triethanolamine, cetyltrimethylammonium bromide and sodium trifluoroacetate serving as a surfactant and a template agent, so that micropores are formed in the prepared nano silicon dioxide to prepare aminated nano silicon dioxide, tin tetrachloride serving as a raw material is inlaid in the micropores of the aminated nano silicon dioxide to prepare modified di-nano silicon dioxide, and the modified nano silicon dioxide reacts with 3-isocyanatopropyl triethoxysilane to react with amino groups on the modified nano silicon dioxide and isocyanato groups on the 3-isocyanatopropyl triethoxysilane.
When the modified resin and the SGP laminated resin are molten, double bonds on the modified resin can be grafted with molecular chains on the SGP laminated resin, a molecular chain main body of the modified resin is of a polyurethane structure containing an organosilicon chain segment, the heat insulation effect of the SGP laminated resin can be improved, and the modified filler contains a multi-cavity structure, so that the heat insulation effect is further improved, and titanium-containing organosilicon resin chain segments in the modified resin, tin dioxide on the surface of the modified filler and benzotriazole structures in the modified resin can be increased, the absorption of ultraviolet rays by a laminated sheet can be increased, and the irradiation of ultraviolet rays can be reduced.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A production process of SGP film laminated glass specifically comprises the following steps:
Step S1, mixing a modified prepolymer, ethylenediamine and DMF (dimethyl formamide), introducing nitrogen for protection, reacting for 2 hours at the temperature of 30 ℃ at the speed of 150r/min, adding KH560, adjusting the pH value to 11, reacting for 3 hours to obtain pretreated polyurethane, mixing the pretreated polyurethane, diphenylmethane diisocyanate and DMF, introducing nitrogen for protection, reacting for 5 hours at the temperature of 30 ℃ at the speed of 150r/min, adding N- (2-hydroxyethyl) maleimide, and continuing reacting for 4 hours to obtain modified polyurethane;
And S2, uniformly mixing modified polyurethane, modified filler, dimethyl diethoxysilane, ethanol and DMF (dimethyl formamide), stirring and adding deionized water and hydrochloric acid at the rotation speed of 120r/min and the temperature of 65 ℃, reacting for 2 hours, adding tetrabutyl titanate, continuously reacting for 2 hours, heating to 120 ℃, reacting for 3 hours to obtain modified resin, mixing the modified resin, SGP laminating resin and dicumyl peroxide, extruding and casting to form a film at the feeding section temperature of 190 ℃, the melting section temperature of 180 ℃ and the discharging section temperature of 150 ℃, preparing a laminating film, placing the laminating film between two pieces of glass, and pressing at high temperature to obtain SGP laminating glass.
The molar ratio of isocyanate groups to ethylenediamine on the modified prepolymer in the step S1 is 1:1, and the molar ratio of hydroxyl groups, diphenylmethane diisocyanate and N- (2-hydroxyethyl) maleimide on the pretreated polyurethane is 1:1:2.
The dosage ratio of the modified polyurethane to the modified filler to the dimethyl diethoxysilane to the ethanol to the DMF to the deionized water to the hydrochloric acid solution to the tetrabutyl titanate in the step S2 is 5g:80mg:1mmo l:10mL:50mL:20mL:3mL:1.5mmo l, the mass fraction of the hydrochloric acid solution is 10%, and the weight ratio of the modified resin to the SGP laminating resin is 30:80:1.
The modified prepolymer is prepared by the following steps:
Uniformly mixing p-chloro-o-nitroaniline, p-hydroxystyrene, sodium nitrite and potassium hydrogen sulfate, placing in a mortar, grinding for 20min at the temperature of 20 ℃ to obtain azo dye, uniformly mixing the azo dye, ethanol and sodium hydroxide solution, stirring at the rotating speed of 600r/min at the temperature of 80 ℃ and adding sodium dithionite, and reacting for 1h to obtain an intermediate 1;
Step A2, uniformly mixing metal magnesium, iodine and tetrahydrofuran, introducing nitrogen for protection, stirring and adding 2-bromothiophene under the conditions of the rotating speed of 60r/min and the temperature of 20 ℃, heating to 60 ℃, reacting for 3 hours to obtain an intermediate 2, uniformly mixing the intermediate 1, the intermediate 2 and the tetrahydrofuran, and reacting for 5 hours under the conditions of the rotating speed of 150r/min and the temperature of 60 ℃ to obtain a modifier;
And step A3, uniformly mixing a modifier, diethanolamine and DMF, introducing nitrogen for protection, stirring and adding sodium hydroxide to the pH value of 10 under the conditions of the rotating speed of 120r/min and the temperature of 20 ℃, reacting for 3 hours, regulating the pH value to be neutral, preparing a modified monomer, mixing the modified monomer, diphenylmethane diisocyanate and DMF, and reacting for 2 hours under the conditions of the rotating speed of 120r/min and the temperature of 40 ℃ to prepare the modified prepolymer.
The mol ratio of the p-chloro-o-nitroaniline to the p-hydroxystyrene to the sodium nitrite to the potassium bisulfate in the step A1 is 1:1.1:1, and the dosage ratio of the azo dye to the ethanol to the sodium hydroxide solution to the sodium dithionite is 25mmo l:50mL:50mL:82mmo l.
The dosage ratio of the magnesium metal, iodine, tetrahydrofuran and 2-bromothiophene in the step A2 is 1.1mo l:1mo l:100mL:1mo l, and the mol ratio of the intermediate 1 to the intermediate 2 is 1:1.
The mol ratio of the modifier to the diethanol amine in the step A3 is 1:1, and the mol ratio of the modified monomer to the diphenylmethane diisocyanate is 1:2.1.
The modified filler is prepared by the following steps:
Uniformly mixing triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate and deionized water, stirring at the rotating speed of 150r/min and the temperature of 80 ℃, adding tetraethoxysilane, KH550 and ethanol, reacting for 4 hours, centrifuging to remove a supernatant, adding a substrate into a hydrochloric acid solution, performing ultrasonic treatment at the frequency of 20kHz and the temperature of 20 ℃ for 5 minutes, heating to 60 ℃, and preserving heat for 5 hours to obtain the aminated nano silicon dioxide;
And B2, uniformly mixing the aminated nano silicon dioxide, the stannic chloride and the ethanol, stirring and adding deionized water and ammonia water to the pH value of 10 at the rotation speed of 120r/min and the temperature of 30 ℃, stirring for 10min, heating to 150 ℃ for reaction for 20 hours to obtain the modified nano silicon dioxide, dispersing the modified nano silicon dioxide in the ethanol, introducing nitrogen for protection, stirring and adding 3-isocyanatopropyl triethoxysilane at the rotation speed of 300r/min and the temperature of 30 ℃ for reaction for 2 hours, and obtaining the modified filler.
And B1, wherein the dosage ratio of triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate, deionized water, tetraethoxysilane, KH550 and ethanol is 65mg:380mg:550mg:25mL:10mmo l:5mmo l:5mL, the dosage ratio of the base material to the hydrochloric acid solution is 1 mg/1 mL, and the mass fraction of the hydrochloric acid solution is 5%.
The dosage ratio of the amination nanometer silicon dioxide to the stannic chloride to the ethanol to the deionized water in the step B2 is 2g:2mmo l:10mL:10mL, and the molar ratio of the amino group on the surface of the modified nanometer silicon dioxide to the 3-isocyanatopropyl triethoxysilane is 1:1.
Example 2
A production process of SGP film laminated glass specifically comprises the following steps:
Step S1, mixing a modified prepolymer, ethylenediamine and DMF (dimethyl formamide), introducing nitrogen for protection, reacting for 3 hours at the rotation speed of 150r/min and the temperature of 35 ℃, adding KH560, adjusting the pH value to 11, reacting for 4 hours to obtain pretreated polyurethane, mixing the pretreated polyurethane, diphenylmethane diisocyanate and DMF, introducing nitrogen for protection, reacting for 6 hours at the rotation speed of 150r/min and the temperature of 35 ℃, adding N- (2-hydroxyethyl) maleimide, and continuing to react for 5 hours to obtain modified polyurethane;
And S2, uniformly mixing modified polyurethane, modified filler, dimethyl diethoxysilane, ethanol and DMF (dimethyl formamide), stirring and adding deionized water and hydrochloric acid at the rotation speed of 120r/min and the temperature of 68 ℃, reacting for 3 hours, adding tetrabutyl titanate, continuously reacting for 2 hours, heating to 125 ℃, reacting for 4 hours to obtain modified resin, mixing the modified resin, SGP laminating resin and dicumyl peroxide, extruding and casting to form a film at the feeding section temperature of 190 ℃, the melting section temperature of 180 ℃ and the discharging section temperature of 150 ℃, preparing a laminating film, placing the laminating film between two pieces of glass, and pressing at high temperature to obtain SGP laminating glass.
The molar ratio of isocyanate groups to ethylenediamine on the modified prepolymer in the step S1 is 1:1, and the hydroxyl groups, diphenylmethane diisocyanate and N- (2-hydroxyethyl) maleimide on the pretreated polyurethane are 2:2:2.
The dosage ratio of the modified polyurethane to the modified filler to the dimethyl diethoxysilane to the ethanol to the DMF to the deionized water to the hydrochloric acid solution to the tetrabutyl titanate in the step S2 is 5g:80mg:1mmo l:10mL:50mL:20mL:3mL:1.5mmo l, the mass fraction of the hydrochloric acid solution is 10%, and the weight ratio of the modified resin to the SGP laminating resin is 40:90:2.
The modified prepolymer is prepared by the following steps:
Uniformly mixing p-chloro-o-nitroaniline, p-hydroxystyrene, sodium nitrite and potassium hydrogen sulfate, placing in a mortar, grinding for 25min at the temperature of 20 ℃ to obtain azo dye, uniformly mixing the azo dye, ethanol and sodium hydroxide solution, stirring at the rotating speed of 600r/min at the temperature of 80 ℃ and adding sodium dithionite, and reacting for 1.5h to obtain an intermediate 1;
Step A2, uniformly mixing metal magnesium, iodine and tetrahydrofuran, introducing nitrogen for protection, stirring and adding 2-bromothiophene under the conditions of the rotating speed of 60r/min and the temperature of 25 ℃, heating to 65 ℃ for reaction for 4 hours to obtain an intermediate 2, uniformly mixing the intermediate 1, the intermediate 2 and the tetrahydrofuran, and reacting for 6 hours under the conditions of the rotating speed of 150r/min and the temperature of 65 ℃ to obtain a modifier;
And step A3, uniformly mixing a modifier, diethanolamine and DMF, introducing nitrogen for protection, stirring and adding sodium hydroxide to the pH value of 10 under the conditions of the rotating speed of 150r/min and the temperature of 20 ℃, reacting for 4 hours, regulating the pH value to be neutral, preparing a modified monomer, mixing the modified monomer, diphenylmethane diisocyanate and DMF, and reacting for 3 hours under the conditions of the rotating speed of 120r/min and the temperature of 45 ℃ to prepare the modified prepolymer.
The mol ratio of the p-chloro-o-nitroaniline to the p-hydroxystyrene to the sodium nitrite to the potassium bisulfate in the step A1 is 1:1.1:1, and the dosage ratio of the azo dye to the ethanol to the sodium hydroxide solution to the sodium dithionite is 25mmo l:50mL:50mL:82mmo l.
The dosage ratio of the magnesium metal, iodine, tetrahydrofuran and 2-bromothiophene in the step A2 is 1.1mo l:1mo l:100mL:1mo l, and the mol ratio of the intermediate 1 to the intermediate 2 is 1:1.
The mol ratio of the modifier to the diethanol amine in the step A3 is 1:1, and the mol ratio of the modified monomer to the diphenylmethane diisocyanate is 1:2.1.
The modified filler is prepared by the following steps:
Uniformly mixing triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate and deionized water, stirring at the rotating speed of 150r/min and the temperature of 85 ℃, adding tetraethoxysilane, KH550 and ethanol, reacting for 5 hours, centrifuging to remove a supernatant, adding a substrate into a hydrochloric acid solution, performing ultrasonic treatment at the frequency of 25kHz and the temperature of 20 ℃ for 8 minutes, heating to 65 ℃, and preserving heat for 6 hours to obtain the aminated nano silicon dioxide;
and B2, uniformly mixing the aminated nano silicon dioxide, the stannic chloride and the ethanol, stirring and adding deionized water and ammonia water to the pH value of 10 at the rotating speed of 150r/min and the temperature of 35 ℃, stirring for 10min, heating to 155 ℃ for reaction for 23h to obtain the modified nano silicon dioxide, dispersing the modified nano silicon dioxide in the ethanol, introducing nitrogen for protection, stirring and adding 3-isocyanatopropyl triethoxysilane at the rotating speed of 500r/min and the temperature of 35 ℃ for reaction for 2h to obtain the modified filler.
And B1, wherein the dosage ratio of triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate, deionized water, tetraethoxysilane, KH550 and ethanol is 65mg:380mg:550mg:25mL:10mmo l:5mmo l:5mL, the dosage ratio of the base material to the hydrochloric acid solution is 1 mg/1 mL, and the mass fraction of the hydrochloric acid solution is 5%.
The dosage ratio of the amination nanometer silicon dioxide to the stannic chloride to the ethanol to the deionized water in the step B2 is 2g:2mmo l:10mL:10mL, and the molar ratio of the amino group on the surface of the modified nanometer silicon dioxide to the 3-isocyanatopropyl triethoxysilane is 1:1.
Example 3
A production process of SGP film laminated glass specifically comprises the following steps:
Step S1, mixing a modified prepolymer, ethylenediamine and DMF (dimethyl formamide), introducing nitrogen for protection, reacting for 3 hours at the temperature of 40 ℃ at the speed of 200r/min, adding KH560, adjusting the pH value to 12, reacting for 5 hours to obtain pretreated polyurethane, mixing the pretreated polyurethane, diphenylmethane diisocyanate and DMF, introducing nitrogen for protection, reacting for 6 hours at the temperature of 40 ℃ at the speed of 200r/min, adding N- (2-hydroxyethyl) maleimide, and continuing to react for 6 hours to obtain modified polyurethane;
And S2, uniformly mixing modified polyurethane, modified filler, dimethyl diethoxysilane, ethanol and DMF (dimethyl formamide), stirring and adding deionized water and hydrochloric acid at the rotation speed of 150r/min and the temperature of 70 ℃, reacting for 3 hours, adding tetrabutyl titanate, continuously reacting for 3 hours, heating to 130 ℃, reacting for 5 hours to obtain modified resin, mixing the modified resin, SGP laminating resin and dicumyl peroxide, extruding and casting to form a film at the feeding section temperature of 190 ℃, the melting section temperature of 180 ℃ and the discharging section temperature of 150 ℃, preparing a laminating film, placing the laminating film between two pieces of glass, and pressing at high temperature to obtain SGP laminating glass.
The molar ratio of isocyanate groups to ethylenediamine on the modified prepolymer in the step S1 is 1:1, and the hydroxyl groups, diphenylmethane diisocyanate and N- (2-hydroxyethyl) maleimide on the pretreated polyurethane are 3:3:2.
The dosage ratio of the modified polyurethane to the modified filler to the dimethyl diethoxysilane to the ethanol to the DMF to the deionized water to the hydrochloric acid solution to the tetrabutyl titanate is 5g:80mg:1mmo l:10mL:50mL:20mL:3mL:1.5mmo l, the mass fraction of the hydrochloric acid solution is 10%, and the weight ratio of the modified resin to the SGP laminating resin is 50:100:3.
The modified prepolymer is prepared by the following steps:
uniformly mixing p-chloro-o-nitroaniline, p-hydroxystyrene, sodium nitrite and potassium hydrogen sulfate, placing in a mortar, grinding for 30min at the temperature of 25 ℃ to obtain azo dye, uniformly mixing the azo dye, ethanol and sodium hydroxide solution, stirring at the rotating speed of 800r/min at the temperature of 85 ℃ and adding sodium dithionite, and reacting for 1.5h to obtain an intermediate 1;
Step A2, uniformly mixing metal magnesium, iodine and tetrahydrofuran, introducing nitrogen for protection, stirring and adding 2-bromothiophene under the conditions of the rotating speed of 80r/min and the temperature of 25 ℃, heating to 70 ℃ for reaction for 5 hours to obtain an intermediate 2, uniformly mixing the intermediate 1, the intermediate 2 and the tetrahydrofuran, and reacting for 6 hours under the conditions of the rotating speed of 200r/min and the temperature of 70 ℃ to obtain a modifier;
And step A3, uniformly mixing a modifier, diethanolamine and DMF, introducing nitrogen for protection, stirring and adding sodium hydroxide to the pH value of 11 at the rotating speed of 150r/min and the temperature of 25 ℃, reacting for 5 hours, regulating the pH value to be neutral, preparing a modified monomer, mixing the modified monomer, diphenylmethane diisocyanate and DMF, and reacting for 4 hours at the rotating speed of 150r/min and the temperature of 50 ℃ to obtain the modified prepolymer.
The mol ratio of the p-chloro-o-nitroaniline to the p-hydroxystyrene to the sodium nitrite to the potassium bisulfate in the step A1 is 1:1.1:1, and the dosage ratio of the azo dye to the ethanol to the sodium hydroxide solution to the sodium dithionite is 25mmo l:50mL:50mL:82mmo l.
The dosage ratio of the magnesium metal, iodine, tetrahydrofuran and 2-bromothiophene in the step A2 is 1.1mo l:1mo l:100mL:1mo l, and the mol ratio of the intermediate 1 to the intermediate 2 is 1:1.
The mol ratio of the modifier to the diethanol amine in the step A3 is 1:1, and the mol ratio of the modified monomer to the diphenylmethane diisocyanate is 1:2.1.
The modified filler is prepared by the following steps:
Uniformly mixing triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate and deionized water, stirring at the rotating speed of 200r/min and the temperature of 85 ℃, adding tetraethoxysilane, KH550 and ethanol, reacting for 6 hours, centrifuging to remove a supernatant, adding a substrate into a hydrochloric acid solution, performing ultrasonic treatment at the frequency of 30kHz and the temperature of 25 ℃ for 10 minutes, heating to 70 ℃, and preserving heat for 7 hours to obtain the aminated nano silicon dioxide;
And B2, uniformly mixing the aminated nano silicon dioxide, the stannic chloride and the ethanol, stirring and adding deionized water and ammonia water to reach the pH of 12 at the rotation speed of 150r/min and the temperature of 40 ℃, stirring for 15min, heating to 160 ℃, reacting for 25h to obtain the modified nano silicon dioxide, dispersing the modified nano silicon dioxide in the ethanol, introducing nitrogen for protection, stirring and adding 3-isocyanatopropyl triethoxysilane at the rotation speed of 500r/min and the temperature of 40 ℃, and reacting for 3h to obtain the modified filler.
And B1, wherein the dosage ratio of triethanolamine, cetyltrimethylammonium bromide, sodium trifluoroacetate, deionized water, tetraethoxysilane, KH550 and ethanol is 65mg:380mg:550mg:25mL:10mmo l:5mmo l:5mL, the dosage ratio of the base material to the hydrochloric acid solution is 1 mg/1 mL, and the mass fraction of the hydrochloric acid solution is 5%.
The dosage ratio of the amination nanometer silicon dioxide to the stannic chloride to the ethanol to the deionized water in the step B2 is 2g:2mmo l:10mL:10mL, and the molar ratio of the amino group on the surface of the modified nanometer silicon dioxide to the 3-isocyanatopropyl triethoxysilane is 1:1.
Comparative example 1
This comparative example uses nanosilica instead of modified filler as compared to example 1, the rest of the procedure being the same.
Comparative example 2
This comparative example uses aminated nanosilica instead of modified nanosilica as compared to example 1, the rest of the procedure being the same.
Comparative example 3
This comparative example uses diphenylmethane diisocyanate instead of the modified prepolymer as compared to example 1, with the remainder of the procedure being the same.
Comparative example 4
This comparative example uses SGP pinch instead of pinch as compared to example 1, the rest of the procedure being the same.
The laminated glass and the common glass obtained in examples 1 to 3 and comparative examples 1 to 4 were prepared into a sample having a volume of 1m 3, and the sample was manually subjected to a simulation of a solar light source, irradiated for 8 hours, and compared with the temperature difference in the space of the common glass, and the detection results were shown in the following table.
The table shows that the application has good heat insulation effect.
The foregoing is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.