CN114634705A - Heat and sound insulation blanket for vehicle and preparation method thereof - Google Patents
Heat and sound insulation blanket for vehicle and preparation method thereof Download PDFInfo
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- CN114634705A CN114634705A CN202210382127.9A CN202210382127A CN114634705A CN 114634705 A CN114634705 A CN 114634705A CN 202210382127 A CN202210382127 A CN 202210382127A CN 114634705 A CN114634705 A CN 114634705A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L75/00—Compositions of polyureas or polyurethanes; Compositions of derivatives of such polymers
- C08L75/04—Polyurethanes
- C08L75/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0061—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof characterized by the use of several polymeric components
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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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/009—Use of pretreated compounding ingredients
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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
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
- C08J2375/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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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
- C08J2471/00—Characterised by the use of polyethers obtained by reactions forming an ether link in the main chain; Derivatives of such polymers
- C08J2471/02—Polyalkylene oxides
Abstract
The invention discloses a heat and sound insulation blanket for a vehicle and a preparation method thereof, and relates to the technical field of vehicle-mounted materials. The invention is used for preparing the heat and sound insulation blanket for the vehicle, firstly oleic acid reacts with glycidyl ether to prepare modified oleic acid, polycaprolactone polyol and toluene diisocyanate react for a period of time, polyethylene glycol and the modified oleic acid are added to continuously react to prepare modified polyurethane, trimethoxy silane, diphenyl dimethoxy silane and vinyl trimethoxy silane react for a period of time, p-hydroxystyrene is added to continuously react to prepare p-hydroxyphenyl vinyl hyperbranched polysiloxane, hollow porous silicon dioxide loaded with oxalic acid sequentially reacts with p-aminophenyl trimethoxy silane and p-hydroxyphenyl vinyl hyperbranched polysiloxane to prepare modified silicon dioxide, the polyurethane is heated and placed in a mold, the temperature is reduced after the modified silicon dioxide is added, and the heat and sound insulation blanket for the vehicle is prepared after standing. The heat and sound insulation blanket for the vehicle prepared by the invention has excellent heat insulation performance, sound insulation performance and durability.
Description
Technical Field
The invention relates to the technical field of vehicle-mounted materials, in particular to a vehicle heat and sound insulation blanket and a preparation method thereof.
Background
The carpet for the vehicle is an interior trim part which is generally applied to a cab of a motor vehicle, is one of indispensable automotive interior trims, has the main functions of blocking and eliminating noise transmitted from the bottom of the vehicle to the interior of the vehicle during driving, has the effects of shock absorption, heat preservation and the like, and has soft treading feeling and can comprehensively improve the driving and riding comfort of a driver and passengers.
The existing vehicle carpet is mostly prepared from plush materials or foaming materials with high specific surface area, and the vehicle carpet is compacted and becomes compact along with treading or dust adsorption in use, so that the sound insulation and heat insulation effects and the comfort degree are reduced.
Disclosure of Invention
The invention aims to provide a heat and sound insulation blanket for a vehicle and a preparation method thereof, which aim to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the preparation method of the heat and sound insulation blanket for the vehicle is characterized in that the heat and sound insulation blanket for the vehicle is prepared by heating modified polyurethane, placing the heated modified polyurethane in a mold, adding modified silicon dioxide, cooling and standing.
As optimization, the modified polyurethane is prepared by adding polyethylene glycol and modified oleic acid into polycaprolactone polyol and toluene diisocyanate after reacting for a period of time and continuing to react; the modified oleic acid is prepared by the reaction of oleic acid and glycidyl ether.
Preferably, the modified silicon dioxide is prepared by sequentially reacting hollow porous silicon dioxide loaded with oxalic acid with p-aminophenyl trimethoxy silane and p-hydroxyphenyl vinyl hyperbranched polysiloxane.
Preferably, the p-hydroxyphenylvinyl hyperbranched polysiloxane is prepared by adding p-hydroxystyrene to continue reacting after trimethoxy silane, diphenyl dimethoxy silane and vinyl trimethoxy silane react for a period of time.
Preferably, the preparation method of the heat and sound insulation blanket for the vehicle comprises the following preparation steps:
(1) heating polycaprolactone polyol in a water bath to 90-100 ℃, standing for 1-2 h, adding toluene diisocyanate with the mass of 0.8-1 time of that of the polycaprolactone polyol, stirring at 70-80 ℃ at 500-700 r/min for 3-5 min, standing for 1-2 h, adding polyethylene glycol with the mass of 0.2-0.3 time of that of the polycaprolactone polyol, modified oleic acid with the mass of 0.4-0.5 time of that of the polycaprolactone polyol and dibutyl tin dilaurate with the mass of 0.01-0.02 time of that of the polycaprolactone polyol, stirring at 70-80 ℃ at 500-700 r/min for 3-5 min, and standing at 80-90 ℃ for 10-12 h in a nitrogen atmosphere to obtain modified polyurethane;
(2) placing hollow porous silica in a vacuum impregnator, pumping pressure to 1-10 Pa, adding an oxalic acid solution with the mass fraction of 5-8% and the mass of 3-4 times that of the hollow porous silica, introducing nitrogen to enable the pressure to reach 10-20 kPa, standing for 10-15 min at 10-20 ℃, filtering, and drying at-1-10 ℃ and 1-10 Pa for 6-8 h to prepare loaded silica;
(3) the preparation method comprises the following steps of (1) mixing pre-modified silicon dioxide, p-hydroxyphenyl vinyl hyperbranched polysiloxane and 10-15% by mass of hydrochloric acid solution according to a mass ratio of 1: 1: 6-1: 1: 8, uniformly mixing, adding a sodium nitrite aqueous solution with the mass fraction of 10-15% and the mass fraction of 3-4 times that of the pre-modified silicon dioxide at 0-5 ℃, stirring and reacting for 20-30 min at 800-1000 r/min, filtering, washing for 3-5 times by using pure water, and drying for 6-8 h at-1-10 ℃ and 1-10 Pa to obtain the modified silicon dioxide;
(4) after the modified polyurethane is pretreated, adding modified silicon dioxide with the amount of 0.2-0.3 time of that of the modified polyurethane and polyethylene glycol with the amount of 0.2-0.3 time of that of the modified polyurethane, stirring and reacting at 170-180 ℃ and 800-1000 r/min for 5-8 min, cooling to 80-90 ℃ at the speed of 5-6 ℃/min, preserving heat for 8-10 h, naturally cooling to room temperature, standing in pure water for 10-15 min, and standing at 1-10 ℃ and 1-10 Pa for 10-12 h to obtain the heat-insulating and sound-insulating blanket for the vehicle.
As optimization, the preparation method of the modified oleic acid in the step (1) comprises the following steps: oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 1-2% and ethanol are mixed according to the mass ratio of 1: 1: 2: 2-1: 1: 3: 3, uniformly mixing, stirring for 1-2 h at 40-50 ℃ and 500-700 r/min, and standing for 8-10 h at 10-30 ℃ and 1-2 kPa to prepare the water-based paint.
As an optimization, the preparation method of the hollow porous silica in the step (2) comprises the following steps: ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 6-1: 10, uniformly mixing, dropwise adding 0.1-0.2 mL/s into deionized water 30-40 times of the mass of ethyl orthosilicate under the stirring condition of 200-300 r/min at 10-30 ℃, continuously stirring for 30-40 min after the stirring is finished, filtering, washing for 3-5 times by using absolute ethyl alcohol, putting into a reaction kettle with a polytetrafluoroethylene lining, adding the absolute ethyl alcohol into the reaction kettle with 70% of the total volume, adding ammonium bicarbonate 0.5-0.8 time of the mass of the ethyl orthosilicate, uniformly mixing, sealing the reaction kettle, heating for 6-8 hours at the constant temperature of 50-60 ℃, cooling to room temperature, filtering, sequentially washing for 3-5 times by using the deionized water and the absolute ethyl alcohol, and drying for 4-6 hours at the temperature of 60-70 ℃ to prepare the water-based organic silicon dioxide gel.
As optimization, the preparation method of the pre-modified silica in the step (3) comprises the following steps: loading silicon dioxide, p-aminophenyl trimethoxy silane, absolute ethyl alcohol and pure water according to a mass ratio of 1: 1: 6: 2-1: 1: 9: 3, uniformly mixing, stirring and reacting for 40-50 min at 10-20 ℃ at 800-1000 r/min, and drying for 4-6 h at 60-70 ℃ to prepare the water-based paint.
Preferably, the preparation method of the p-hydroxyphenyl vinyl hyperbranched polysiloxane in the step (3) comprises the following steps: in a nitrogen atmosphere, trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are mixed according to the mass ratio of 1: 3: 2: 8-1: 4: 2: 10, uniformly mixing, adjusting the pH to 2.9-3.1 by using hydrochloric acid with the mass fraction of 3-5%, stirring for 40-50 min at the temperature of 30-40 ℃ at 500-800 r/min, adding p-hydroxystyrene with the mass fraction of 0.3-0.5 times that of trimethoxy silane and divinyl tetramethyl disiloxane platinum salt with the mass fraction of 0.03-0.05 of trimethoxy silane, stirring for reaction for 7-9 h at the temperature of 70-80 ℃ at 500-800 r/min, adding hexamethyl disiloxane aqueous solution with the mass fraction of 85-90% that of trimethoxy silane and continuing stirring for 2-3 h, standing for 8-10 h at the temperature of 10-30 ℃, separating and taking an oil phase, and drying for 8-10 h at the temperature of 10-30 ℃ at 1-10 Pa to prepare the oil-based waterborne polyurethane emulsion.
As optimization, the pretreatment method in the step (4) comprises the following steps: and heating the modified polyurethane to 180-190 ℃ and then placing the heated modified polyurethane in a mold.
Compared with the prior art, the invention has the following beneficial effects:
when the heat and sound insulation blanket for the vehicle is prepared, firstly, polycaprolactone polyol and toluene diisocyanate are reacted for a period of time, then polyethylene glycol and modified oleic acid are added to continue the reaction to prepare modified polyurethane, the modified polyurethane is heated and then placed in a mold, and after the modified silicon dioxide is added, the temperature is reduced and the temperature is kept still, so that the heat and sound insulation blanket for the vehicle is prepared.
Firstly, p-hydroxyphenyl vinyl hyperbranched polysiloxane is prepared by reacting trimethoxy silane, diphenyl dimethoxy silane and vinyl trimethoxy silane for a period of time and then adding p-hydroxyphenyl ethylene to continue reacting, oxalic acid is loaded in hollow porous silica by a vacuum impregnation method and reacts with p-aminophenyl trimethoxy silane and the p-hydroxyphenyl vinyl hyperbranched polysiloxane in sequence to prepare modified silica, the oxalic acid remained on the surface is dissolved in the preparation process to promote the hydrolysis of the p-aminophenyl trimethoxy silane, silane hydroxyl generated by the hydrolysis is combined on the hollow porous silica and has an azo reaction with the p-hydroxyphenyl vinyl hyperbranched polysiloxane, the dispersibility of the prepared modified silica is improved, so that the loaded oxalic acid can generate gas and generate uniform and fine bubbles in a main material, thereby improving the heat insulation and sound insulation performance of the heat and sound insulation blanket for the vehicle.
Secondly, oleic acid reacts with glycidyl ether to prepare modified oleic acid, polyethylene glycol and modified oleic acid are added in the preparation process of polyurethane, the polyethylene glycol and hydroxyl on the modified oleic acid participate in the reaction to modify the polyurethane, so that the modified polyurethane has the property that part of hydrophilic part is oleophilic, when the modified polyurethane is heated to be liquid, the hydrophilic part is compatible with the polyethylene glycol added subsequently, secondary micropores are formed outside bubbles, the heat insulation and sound insulation performance of the vehicle heat insulation and sound insulation blanket is further improved, the oleophylic part has good compatibility with the p-hydroxyphenyl vinyl hyperbranched polysiloxane group on the subsequent modified silicon dioxide, the influence of the subsequently added polyethylene glycol on the integrity and rebound effect of the bubble wall is reduced, the p-hydroxyphenyl vinyl hyperbranched polysiloxane free radical generated by the breakage of azo bond can be retained and dissolved in the peripheral modified polyurethane, and the polymerization of carbon-carbon double bonds on the free radicals of the modified polyurethane and the p-hydroxyphenyl vinyl hyperbranched polysiloxane is initiated to form a composite crosslinking network, so that the structure is stable, a good rebound effect is achieved, the adhesion and collapse of air bubbles in use are avoided, and the durability of the heat-insulating and sound-insulating blanket is improved.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
In order to more clearly illustrate the method provided by the present invention, the following examples are given, and the method for testing each index of the heat and sound insulation blanket for vehicle manufactured in the following examples is as follows:
heat insulation performance: the heat and sound insulating blanket for vehicle obtained in each example was made to have the same size, shape and thickness as the comparative example material, covered with the same heat source of 80 c on one side surface, placed in the same room temperature environment, and the temperature on the other side surface was measured after a certain period of time, and the temperature difference was recorded as the temperature on the other side surface-the ambient temperature.
Sound insulation performance: the heat and sound insulation blanket for vehicle obtained in each example was formed to have the same size and shape and thickness as the comparative example material, and the same intensity of sound was emitted from one side by a sound emitting device, and the intensity of sound transmitted from the other side was measured by a decibel meter, and the sound insulation rate was recorded as 1-intensity of sound transmitted/intensity of sound emitted.
Durability performance: the heat and sound insulating blankets for vehicles obtained in the respective examples and comparative examples were formed to have the same thickness and the same dimensions, pressed for a certain period of time with the same pressure, and then the sound insulating properties were measured again, and the retention of the recording properties was the sound insulating rate after pressing/the initial sound insulating rate
Example 1
A preparation method of a heat and sound insulation blanket for a vehicle mainly comprises the following preparation steps:
(1) mixing oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 1% and ethanol according to the mass ratio of 1: 1: 2: 2, uniformly mixing, stirring for 1h at 40 ℃ and 700r/min, standing for 10h at 10 ℃ and 1kPa to prepare modified oleic acid, heating polycaprolactone polyol water bath to 90 ℃, standing for 2h, adding toluene diisocyanate with the mass of 0.8 time of that of the polycaprolactone polyol, stirring for 5min at 70 ℃ and 500r/min, standing for 2h, adding polyethylene glycol with the mass of 0.2 time of that of the polycaprolactone polyol, modified oleic acid with the mass of 0.4 time of that of the polycaprolactone polyol and dibutyl tin dilaurate with the mass of 0.01-0.02 time of that of the polycaprolactone polyol, stirring for 3min at 80 ℃ and 700r/min, and standing for 10h at 90 ℃ in a nitrogen atmosphere to prepare modified polyurethane;
(2) ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 10, dripping 0.2mL/s of the mixture into deionized water 40 times of the mass of ethyl orthosilicate under the stirring condition of 300r/min at 30 ℃, continuing to stir for 30min after the stirring is finished, filtering and washing for 5 times by using absolute ethyl alcohol, putting the mixture into a reaction kettle with a polytetrafluoroethylene lining, adding 70 percent of the total volume by using the absolute ethyl alcohol, adding ammonium bicarbonate 0.8 times of the mass of the ethyl orthosilicate, uniformly mixing, sealing the reaction kettle, heating at the constant temperature of 60 ℃ for 6h, cooling to room temperature, filtering, sequentially washing for 5 times by using the deionized water and the absolute ethyl alcohol, drying for 4h at 70 ℃ to prepare hollow porous silica, putting the hollow porous silica into a vacuum impregnator, pumping the pressure to 10Pa, adding an oxalic acid solution with the mass fraction of 5 percent 4 times of the mass of the hollow porous silica, introducing nitrogen to ensure that the pressure reaches 10kPa, standing for 15min at 10 ℃, filtering and drying at-1 ℃ for 8h at 1a to obtain loaded silicon dioxide;
(3) in a nitrogen atmosphere, trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are mixed according to the mass ratio of 1: 3: 2: 8, uniformly mixing, adjusting the pH to 2.9 by using hydrochloric acid with the mass fraction of 3%, stirring for 50min at 30 ℃ at 500r/min, adding p-hydroxystyrene with the mass fraction of 0.3 time that of trimethoxy silane and divinyl tetramethyl disiloxane platinum salt with the mass fraction of 0.03 time that of trimethoxy silane, stirring for reaction for 9h at 70 ℃ at 500r/min, adding hexamethyldisiloxane aqueous solution with the mass fraction of 85% that of trimethoxy silane and continuing to stir for 2h, standing for 10h at 10 ℃, separating and taking an oil phase, drying for 10h at 10 ℃ under 1Pa to prepare p-hydroxyphenyl vinyl hyperbranched polysiloxane, and mixing the loaded silicon dioxide, p-aminophenyl trimethoxy silane, absolute ethyl alcohol and pure water according to the mass ratio of 1: 1: 6: 2, uniformly mixing, stirring at 10 ℃ and 800r/min for reaction for 50min, drying at 60 ℃ for 6h to prepare pre-modified silicon dioxide, mixing the pre-modified silicon dioxide, the p-hydroxyphenyl vinyl hyperbranched polysiloxane and a hydrochloric acid solution with the mass fraction of 10% according to the mass ratio of 1: 1: 6, uniformly mixing, adding a sodium nitrite aqueous solution with the mass fraction of 15% and the mass of 3 times that of the pre-modified silicon dioxide at 0 ℃, stirring and reacting for 30min at 800r/min, filtering, washing for 5 times by using pure water, and drying for 8h at-1 ℃ under 1Pa to obtain the modified silicon dioxide;
(4) heating the modified polyurethane to 180 ℃, placing the heated modified polyurethane in a mold, adding modified silicon dioxide with the mass 0.2 time of that of the modified polyurethane and polyethylene glycol with the mass 0.2 time of that of the modified polyurethane, stirring and reacting for 8min at 170 ℃ and 800r/min, cooling to 80 ℃ at 5 ℃/min, preserving heat for 10h, naturally cooling to room temperature, placing the cooled modified polyurethane in pure water for 10min, and standing for 12h at 1 ℃ and 1Pa to obtain the heat and sound insulation blanket for the vehicle.
Example 2
A preparation method of a heat and sound insulation blanket for a vehicle mainly comprises the following preparation steps:
(1) oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 1.5% and ethanol are mixed according to the mass ratio of 1: 1: 2.5: 2.5, uniformly mixing, stirring for 1.5h at 45 ℃, 600r/min, standing for 9h at 20 ℃, 1.5kPa to obtain modified oleic acid, heating polycaprolactone polyol water bath to 95 ℃, standing for 1.5h, adding toluene diisocyanate with the mass of 0.9 time of that of the polycaprolactone polyol, stirring for 4min at 75 ℃, 600r/min, standing for 1.5h, adding polyethylene glycol with the mass of 0.2-0.3 time of that of the polycaprolactone polyol, modified oleic acid with the mass of 0.4-0.5 time of that of the polycaprolactone polyol and dibutyl tin dilaurate with the mass of 0.01-0.02 time of that of the polycaprolactone polyol, stirring for 4min at 75 ℃, 600r/min, standing for 11h at 85 ℃ in a nitrogen atmosphere to obtain modified polyurethane;
(2) ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 8, dripping 0.15mL/s into deionized water with the mass 35 times of that of ethyl orthosilicate under the stirring condition of 20 ℃ and 250r/min, continuing to stir for 35min after the stirring is finished, filtering and washing for 4 times by using absolute ethyl alcohol, putting into a reaction kettle with a polytetrafluoroethylene lining, adding 70 percent of absolute ethyl alcohol into the total volume, adding ammonium bicarbonate with the mass 0.6 time of that of ethyl orthosilicate, uniformly mixing, sealing the reaction kettle, heating at the constant temperature of 55 ℃ for 7h, cooling to room temperature, filtering, sequentially washing for 4 times by using deionized water and absolute ethyl alcohol, drying at the temperature of 65 ℃ for 5h to obtain hollow porous silica, putting the hollow porous silica into a vacuum impregnator, pumping the pressure to 5Pa, adding an oxalic acid solution with the mass fraction 6 percent 3.5 times of the mass of the hollow porous silica, introducing nitrogen to ensure that the pressure reaches 15kPa, standing at the temperature of 15 ℃ for 12min, filtering and drying at-5 ℃ and 5Pa for 7h to prepare loaded silicon dioxide;
(3) trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are added in a nitrogen atmosphere according to the mass ratio of 1: 3.5: 2: 9, uniformly mixing, adjusting the pH to 3 by using hydrochloric acid with the mass fraction of 4%, stirring for 45min at 35 ℃ and 650r/min, adding p-hydroxystyrene with the mass of 0.4 time that of trimethoxy silane and platinum salt of divinyl tetramethyl disiloxane with the mass of 0.04 of trimethoxy silane, stirring for reacting for 8h at 75 ℃ and 650r/min, adding aqueous solution of hexamethyldisiloxane with the mass fraction of 87% that of trimethoxy silane with the mass fraction of 4 time that of trimethoxy silane, continuously stirring for 2.5h, standing for 9h at 20 ℃, separating and taking an oil phase, drying for 9h at 20 ℃ and 5Pa to prepare p-hydroxyphenyl vinyl hyperbranched polysiloxane, mixing the loaded silicon dioxide, p-aminophenyl trimethoxy silane, absolute ethyl alcohol and pure water according to the mass ratio of 1: 1: 7: 2.5, uniformly mixing, stirring at 15 ℃ and 900r/min for reaction for 45min, drying at 65 ℃ for 5h to prepare pre-modified silicon dioxide, mixing the pre-modified silicon dioxide, the p-hydroxyphenyl vinyl hyperbranched polysiloxane and a hydrochloric acid solution with the mass fraction of 12% according to the mass ratio of 1: 1: 7, uniformly mixing, adding a sodium nitrite aqueous solution with the mass fraction of 12 percent and the mass of 3.5 times that of the pre-modified silicon dioxide at the temperature of 2 ℃, stirring and reacting for 25min at the speed of 900r/min, filtering, washing for 4 times by using pure water, and drying for 7h at the temperature of-5 ℃ under the pressure of 5Pa to obtain the modified silicon dioxide;
(4) heating the modified polyurethane to 185 ℃, then placing the heated modified polyurethane in a mould, adding modified silicon dioxide with the mass of 0.25 time of that of the modified polyurethane and polyethylene glycol with the mass of 0.25 time of that of the modified polyurethane, stirring and reacting the mixture at 175 ℃ and 900r/min for 6.5min, cooling the mixture to 85 ℃ at 5.5 ℃/min, preserving the heat for 9h, naturally cooling the mixture to room temperature, then placing the mixture in pure water for standing for 12min, and standing the mixture at 5 ℃ and 5Pa for 11h to obtain the heat and sound insulation blanket for the vehicle.
Example 3
A preparation method of a heat and sound insulation blanket for a vehicle mainly comprises the following preparation steps:
(1) mixing oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 2% and ethanol according to the mass ratio of 1: 1: 3: 3, uniformly mixing, stirring for 1h at 50 ℃ and 700r/min, standing for 8h at 30 ℃ and 2kPa to prepare modified oleic acid, heating polycaprolactone polyol water bath to 100 ℃, standing for 1h, adding toluene diisocyanate with the mass of 1 time of that of the polycaprolactone polyol, stirring for 3min at 80 ℃ and 700r/min, standing for 2h, adding polyethylene glycol with the mass of 0.3 time of that of the polycaprolactone polyol, modified oleic acid with the mass of 0.5 time of that of the polycaprolactone polyol and dibutyl tin dilaurate with the mass of 0.02 time of that of the polycaprolactone polyol, stirring for 3min at 80 ℃ and 700r/min, and standing for 12h at 90 ℃ in a nitrogen atmosphere to prepare modified polyurethane;
(2) ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 10, dripping 0.2mL/s of the mixture into deionized water 40 times of the mass of ethyl orthosilicate under the stirring condition of 300r/min at 30 ℃, continuing to stir for 40min after the stirring is finished, filtering and washing for 5 times by using absolute ethyl alcohol, putting the mixture into a reaction kettle with a polytetrafluoroethylene lining, adding 70 percent of the total volume by using the absolute ethyl alcohol, adding ammonium bicarbonate 0.8 times of the mass of the ethyl orthosilicate, uniformly mixing, sealing the reaction kettle, heating at the constant temperature of 60 ℃ for 6h, cooling to room temperature, filtering, sequentially washing for 5 times by using the deionized water and the absolute ethyl alcohol, drying for 4h at 70 ℃, preparing hollow porous silica, putting the hollow porous silica into a vacuum impregnator, pumping the pressure to 10Pa, adding oxalic acid solution with the mass fraction of 8 percent 4 times of the mass of the hollow porous silica, introducing nitrogen to ensure that the pressure reaches 20kPa, standing for 10min at 20 ℃, filtering and drying at-10 ℃ and 10Pa for 6h to prepare loaded silicon dioxide;
(3) in a nitrogen atmosphere, trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are mixed according to the mass ratio of 1: 4: 2: 10, uniformly mixing, adjusting the pH to 2.9 by using hydrochloric acid with the mass fraction of 5%, stirring at 40 ℃ and 800r/min for 40min, adding p-hydroxystyrene with the mass of 0.5 time of that of trimethoxy silane and platinum salt of divinyl tetramethyl disiloxane with the mass of 0.05 time of that of trimethoxy silane, stirring at 80 ℃ and 800r/min for reaction for 7h, adding hexamethyldisiloxane aqueous solution with the mass fraction of 90% of that of trimethoxy silane, continuously stirring for 2h, standing at 30 ℃ for 8h, separating and taking an oil phase, drying at 30 ℃ and 10Pa for 8h to prepare p-hydroxyphenyl vinyl hyperbranched polysiloxane, and mixing the loaded silicon dioxide, p-aminophenyl trimethoxy silane, absolute ethyl alcohol and pure water according to the mass ratio of 1: 1: 9: 3, uniformly mixing, stirring and reacting at 20 ℃ and 1000r/min for 40min, drying at 70 ℃ for 4h to prepare pre-modified silicon dioxide, and mixing the pre-modified silicon dioxide, the p-hydroxyphenyl vinyl hyperbranched polysiloxane and a hydrochloric acid solution with the mass fraction of 15% according to a mass ratio of 1: 1: 8, uniformly mixing, adding a sodium nitrite aqueous solution with the mass fraction of 10 percent and the mass of 4 times that of the pre-modified silicon dioxide at the temperature of 5 ℃, stirring and reacting for 20min at the speed of 1000r/min, filtering, washing for 5 times by using pure water, and drying for 6h at the temperature of 10Pa below zero to obtain the modified silicon dioxide;
(4) heating the modified polyurethane to 190 ℃, placing the heated modified polyurethane in a mold, adding modified silicon dioxide which is 0.3 time of the mass of the modified polyurethane and polyethylene glycol which is 0.3 time of the mass of the modified polyurethane, stirring and reacting for 5min at 180 ℃ and 1000r/min, cooling to 90 ℃ at 6 ℃/min, preserving heat for 10h, naturally cooling to room temperature, placing the cooled modified polyurethane in pure water for 10min, and standing at 10 ℃ and 10Pa for 10h to obtain the heat and sound insulation blanket for the vehicle.
Comparative example 1
The preparation method of the thermal and acoustical insulation blanket for vehicles of comparative example 1 is different from that of example 2 only in the difference of step (1), and step (1) is modified as follows: oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 1.5% and ethanol are mixed according to the mass ratio of 1: 1: 2.5: 2.5, uniformly mixing, stirring for 1.5h at 45 ℃ and 600r/min, standing for 9h at 20 ℃ and 1.5kPa to obtain modified oleic acid, heating polycaprolactone polyol water bath to 95 ℃, standing for 1.5h, adding toluene diisocyanate with the mass of 0.9 time of that of polycaprolactone polyol, stirring for 4min at 75 ℃ and 600r/min, standing for 1.5h, adding polyethylene glycol with the mass of 0.2-0.3 time of that of polycaprolactone polyol and dibutyltin dilaurate with the mass of 0.01-0.02 time of that of polycaprolactone polyol, stirring for 4min at 75 ℃ and 600r/min, and standing for 11h at 85 ℃ in a nitrogen atmosphere to obtain the modified polyurethane. The remaining steps were performed in the same manner as in example 2.
Comparative example 2
The method for manufacturing the thermal and acoustical insulation blanket for vehicles of comparative example 2 is different from example 2 only in the difference of step (2), and step (2) is modified as follows: ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 10, uniformly mixing, dropwise adding 0.2mL/s into deionized water 40 times of the mass of tetraethoxysilane under the stirring condition of 300r/min at 30 ℃, continuing to stir for 40min after the stirring is finished, filtering, washing for 5 times by using absolute ethyl alcohol, putting into a reaction kettle with a polytetrafluoroethylene lining, adding the absolute ethyl alcohol into the reaction kettle with 70 percent of the total volume, sealing the reaction kettle, heating for 6h at the constant temperature of 60 ℃, cooling to room temperature, filtering, sequentially washing for 5 times by using the deionized water and the absolute ethyl alcohol, drying for 4h at 70 ℃ to obtain silicon dioxide, putting the silicon dioxide into a vacuum impregnator, pumping the pressure to 10Pa, adding oxalic acid solution with the mass fraction of 8 percent, the pressure of which is 4 times of the mass of the silicon dioxide, introducing nitrogen to enable the pressure to reach 20kPa, standing for 10min at 20 ℃, filtering, and drying for 6h at-10 ℃ and 10Pa to obtain the loaded silicon dioxide. The remaining steps were performed in the same manner as in example 2.
Comparative example 3
The method for manufacturing the heat and sound insulating blanket for vehicles of comparative example 3 is different from that of example 2 only in the difference of step (3), and step (3) is modified as follows: in a nitrogen atmosphere, trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are mixed according to the mass ratio of 1: 3: 2: 8, uniformly mixing, adjusting the pH to 2.9 by using hydrochloric acid with the mass fraction of 3%, stirring for 9h at 30 ℃ and 500r/min, adding hexamethyldisiloxane aqueous solution with the mass fraction of 85% and the mass fraction of 3 times that of the trimethoxysilane, continuously stirring for 2h, standing for 10h at 10 ℃, separating to obtain an oil phase, drying for 10h at 10 ℃ and 1Pa to prepare the vinyl hyperbranched polysiloxane, and mixing the loaded silicon dioxide, the p-aminophenyl trimethoxysilane, the absolute ethyl alcohol and the pure water according to the mass ratio of 1: 1: 6: 2, uniformly mixing, stirring and reacting at 10 ℃ and 800r/min for 50min, drying at 60 ℃ for 6h to prepare pre-modified silicon dioxide, mixing the pre-modified silicon dioxide, the vinyl hyperbranched polysiloxane and a hydrochloric acid solution with the mass fraction of 10% according to the mass ratio of 1: 1: 6, uniformly mixing, adding a sodium nitrite aqueous solution with the mass fraction of 15 percent and the mass of 3 times of that of the pre-modified silicon dioxide at 0 ℃, stirring and reacting for 30min at 800r/min, filtering, washing for 5 times by using pure water, and drying for 8h at the temperature of minus 1 ℃ under 1Pa to obtain the modified silicon dioxide. The remaining steps were performed in the same manner as in example 2.
Comparative example 4
The method for manufacturing the heat and sound insulating blanket for vehicles of comparative example 4 is different from example 2 in that step (3) is not performed and step (4) is modified as follows: heating the modified polyurethane to 190 ℃, placing the heated modified polyurethane in a mold, adding the loaded silicon dioxide with the mass of 0.3 time of that of the modified polyurethane and the polyethylene glycol with the mass of 0.3 time of that of the modified polyurethane, stirring and reacting for 5min at 180 ℃ and 1000r/min, cooling to 90 ℃ at the speed of 6 ℃/min, preserving heat for 10h, naturally cooling to room temperature, placing the mixture in pure water for 10min, and standing for 10h at the temperature of 10 ℃ and 10Pa to obtain the heat and sound insulation blanket for the vehicle. The remaining steps were performed in the same manner as in example 2.
Effects of the invention
The following table 1 shows the results of performance analysis of the heat insulating property, the sound insulating property, and the durability of the heat and sound insulating blankets for vehicles using examples 1 to 3 and comparative examples 1 to 4 of the present invention.
TABLE 1
| Temperature difference | Sound insulation rate | Retention rate | Temperature difference | Sound insulation rate | Retention rate | ||
| Example 1 | 7.3℃ | 97.2％ | 99.4％ | Comparative example 1 | 7.6℃ | 96.8％ | 95.1％ |
| Example 2 | 6.9℃ | 97.5％ | 99.5％ | Comparative example 2 | 11.8℃ | 91.1％ | 99.3％ |
| Example 3 | 6.8℃ | 97.4％ | 99.5％ | Comparative example 3 | 10.5℃ | 93.4％ | 94.6％ |
| Comparative example 4 | 13.7℃ | 85.6％ | 85.6％ |
As can be seen from the comparison of the experimental data of examples 1 to 3 and comparative examples 1 to 4 in Table 1, the heat and sound insulation blankets for vehicles prepared by the present invention have good heat insulation performance, sound insulation performance and durability.
The comparison of the experimental data of examples 1, 2 and 3 and comparative example 1 shows that the retention rate of examples 1, 2 and 3 is reduced compared with comparative example 1, which illustrates that the modified polyurethane is partially oleophylic by adding modified oleic acid during the preparation process, the oleophylic part has good compatibility with the p-hydroxyphenyl vinyl hyperbranched polysiloxane groups on the subsequent modified silica, the integrity and rebound effect of the bubble wall by the subsequently added polyethylene glycol are reduced, the p-hydroxyphenyl vinyl hyperbranched polysiloxane free radicals generated by the rupture of azo bonds can be retained and dissolved in the peripheral modified polyurethane, and the polymerization of carbon-carbon double bonds on the modified polyurethane and the p-hydroxyphenyl vinyl hyperbranched polysiloxane free radicals is initiated to form a composite crosslinking network, so that the toughness and surface activity of the formed bubble wall are increased, the structure is stable and the rebound effect is good, the adhesion and collapse of air bubbles during use are avoided, so that the durability of the heat and sound insulation blanket is improved; from the comparison of the experimental data of examples 1, 2 and 3 and comparative example 2, it can be seen that the temperature variation of examples 1, 2 and 3 is low and the sound insulation rate is high compared with comparative example 2, which indicates that the addition of ammonium bicarbonate makes silica have a hollow porous structure, which is easy to protect and load oxalic acid, and is not easy to run off in the interior, so that the foaming effect of oxalic acid generated gas on the subject material at high temperature in the subsequent process is improved, and the heat and sound insulation performance of the heat and sound insulation blanket is improved; compared with the experimental data of the comparative examples 1, 2 and 3, the experimental data of the comparative example 3 shows that the temperature variation of the examples 1, 2 and 3 is low compared with the comparative example 3, which illustrates that the p-hydroxystyrene is added to participate in the reaction to prepare the p-hydroxystyrene-based hyperbranched polysiloxane, the p-hydroxystyrene-based hyperbranched polysiloxane can react with the pre-modified silica to form azo connection, the dispersibility of the silica in the main body is improved, and the generated bubbles are more uniform, so that the heat insulation and sound insulation performance of the heat and sound insulation blanket is improved, and then the azo connection is broken at high temperature, so that the p-hydroxystyrene-based hyperbranched polysiloxane is separated from the modified silica to form free radicals and initiate the polymerization of carbon-carbon double bonds, and the polyurethane around is combined to form a composite cross-linked network of the polysiloxane and the polyurethane, the toughness and the rebound effect of the bubble wall are improved, and the durability of the heat and sound insulation blanket is improved.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (10)
1. The preparation method of the heat and sound insulation blanket for the vehicle is characterized in that the heat and sound insulation blanket for the vehicle is prepared by heating modified polyurethane, placing the heated modified polyurethane in a mold, adding modified silicon dioxide, cooling and standing.
2. The preparation method of the heat and sound insulation blanket for the vehicle according to claim 1, wherein the modified polyurethane is prepared by adding polyethylene glycol and modified oleic acid into polycaprolactone polyol and toluene diisocyanate after reacting for a period of time and continuing to react; the modified oleic acid is prepared by the reaction of oleic acid and glycidyl ether.
3. The method for preparing a thermal and acoustical insulation blanket for vehicle as claimed in claim 1, wherein the modified silica is prepared by loading oxalic acid on hollow porous silica, and reacting with aminophenyltrimethoxysilane and p-hydroxyphenylvinyl hyperbranched polysiloxane in sequence.
4. The method for preparing a heat and sound insulating blanket for vehicle according to claim 3, wherein the p-hydroxystyrene-based hyperbranched polysiloxane is prepared by adding p-hydroxystyrene to the trimethoxy silane, the diphenyldimethoxy silane and the vinyltrimethoxy silane after reacting for a period of time and continuing the reaction.
5. The method for manufacturing a heat and sound insulating blanket for vehicles according to claim 1, wherein the method for manufacturing a heat and sound insulating blanket for vehicles comprises the following steps:
(1) heating polycaprolactone polyol in a water bath to 90-100 ℃, standing for 1-2 h, adding toluene diisocyanate with the mass of 0.8-1 time of that of polycaprolactone polyol, stirring at 70-80 ℃ and 500-700 r/min for 3-5 min, standing for 1-2 h, adding polyethylene glycol with the mass of 0.2-0.3 time of that of polycaprolactone polyol, modified oleic acid with the mass of 0.4-0.5 time of that of polycaprolactone polyol and dibutyltin dilaurate with the mass of 0.01-0.02 time of that of polycaprolactone polyol, stirring at 70-80 ℃ and 500-700 r/min for 3-5 min, and standing at 80-90 ℃ for 10-12 h in a nitrogen atmosphere to obtain modified polyurethane;
(2) placing hollow porous silica in a vacuum impregnator, pumping pressure to 1-10 Pa, adding an oxalic acid solution with the mass fraction of 5-8% and the mass of 3-4 times that of the hollow porous silica, introducing nitrogen to enable the pressure to reach 10-20 kPa, standing for 10-15 min at 10-20 ℃, filtering, and drying at-1-10 ℃ and 1-10 Pa for 6-8 h to prepare loaded silica;
(3) the preparation method comprises the following steps of (1) mixing pre-modified silicon dioxide, p-hydroxyphenyl vinyl hyperbranched polysiloxane and 10-15% by mass of hydrochloric acid solution according to a mass ratio of 1: 1: 6-1: 1: 8, uniformly mixing, adding 10-15% by mass of sodium nitrite aqueous solution which is 3-4 times of the mass of the pre-modified silicon dioxide at 0-5 ℃, stirring and reacting for 20-30 min at 800-1000 r/min, filtering, washing for 3-5 times by using pure water, and drying for 6-8 h at-1-10 ℃ at 1-10 Pa to obtain modified silicon dioxide;
(4) after the modified polyurethane is pretreated, adding modified silicon dioxide with the amount of 0.2-0.3 time of that of the modified polyurethane and polyethylene glycol with the amount of 0.2-0.3 time of that of the modified polyurethane, stirring and reacting at 170-180 ℃ and 800-1000 r/min for 5-8 min, cooling to 80-90 ℃ at the speed of 5-6 ℃/min, preserving heat for 8-10 h, naturally cooling to room temperature, standing in pure water for 10-15 min, and standing at 1-10 ℃ and 1-10 Pa for 10-12 h to obtain the heat-insulating and sound-insulating blanket for the vehicle.
6. The method for preparing a heat and sound insulation blanket for a vehicle according to claim 5, wherein the method for preparing the modified oleic acid in the step (1) comprises the following steps: oleic acid, glycidyl ether, hydrochloric acid with the mass fraction of 1-2% and ethanol are mixed according to the mass ratio of 1: 1: 2: 2-1: 1: 3: 3, uniformly mixing, stirring for 1-2 h at 40-50 ℃ and 500-700 r/min, and standing for 8-10 h at 10-30 ℃ and 1-2 kPa to prepare the water-based paint.
7. The method for preparing a thermal and acoustical insulation blanket for vehicle as claimed in claim 5, wherein the method for preparing the hollow porous silica of step (2) comprises: ethyl orthosilicate and absolute ethyl alcohol are mixed according to a mass ratio of 1: 6-1: 10, uniformly mixing, dropwise adding 0.1-0.2 mL/s into deionized water 30-40 times of the mass of tetraethoxysilane under the stirring condition of 10-30 ℃ and 200-300 r/min, continuously stirring for 30-40 min after the stirring is finished, filtering, washing for 3-5 times by using absolute ethyl alcohol, putting into a reaction kettle with a polytetrafluoroethylene lining, adding the absolute ethyl alcohol into the reaction kettle with 70% of the total volume, adding ammonium bicarbonate 0.5-0.8 time of the mass of tetraethoxysilane, uniformly mixing, sealing the reaction kettle, heating for 6-8 hours at the constant temperature of 50-60 ℃, cooling to room temperature, filtering, sequentially washing for 3-5 times by using the deionized water and the absolute ethyl alcohol, and drying for 4-6 hours at the temperature of 60-70 ℃ to prepare the water-based organic silicon dioxide nano-silicon dioxide.
8. The method for preparing a thermal and acoustical insulation blanket for vehicle as claimed in claim 5, wherein the pre-modified silica of step (3) is prepared by: loading silicon dioxide, p-aminophenyl trimethoxy silane, absolute ethyl alcohol and pure water according to a mass ratio of 1: 1: 6: 2-1: 1: 9: 3, uniformly mixing, stirring and reacting for 40-50 min at 10-20 ℃ at 800-1000 r/min, and drying for 4-6 h at 60-70 ℃ to prepare the water-based paint.
9. The method for preparing a heat and sound insulation blanket for a vehicle according to claim 5, wherein the method for preparing the p-hydroxyphenyl vinyl hyperbranched polysiloxane of the step (3) comprises the following steps: in a nitrogen atmosphere, trimethoxy silane, diphenyl dimethoxy silane, vinyl trimethoxy silane and ethanol are mixed according to the mass ratio of 1: 3: 2: 8-1: 4: 2: 10, uniformly mixing, adjusting the pH to 2.9-3.1 by using hydrochloric acid with the mass fraction of 3-5%, stirring for 40-50 min at the temperature of 30-40 ℃ at 500-800 r/min, adding p-hydroxystyrene with the mass fraction of 0.3-0.5 times that of trimethoxy silane and divinyl tetramethyl disiloxane platinum salt with the mass fraction of 0.03-0.05 of trimethoxy silane, stirring for reaction for 7-9 h at the temperature of 70-80 ℃ at 500-800 r/min, adding hexamethyl disiloxane aqueous solution with the mass fraction of 85-90% that of trimethoxy silane and continuing stirring for 2-3 h, standing for 8-10 h at the temperature of 10-30 ℃, separating and taking an oil phase, and drying for 8-10 h at the temperature of 10-30 ℃ at 1-10 Pa to prepare the oil-based waterborne polyurethane emulsion.
10. The method for preparing a thermal and acoustical insulation blanket for vehicle as claimed in claim 5, wherein the pretreatment in step (4) comprises: and heating the modified polyurethane to 180-190 ℃ and then placing the heated modified polyurethane in a mold.
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