CN113861745A

CN113861745A - Preparation of low-fading nano heat-insulating slurry and coating and application of heat-insulating automobile film

Info

Publication number: CN113861745A
Application number: CN202111215674.XA
Authority: CN
Inventors: 余兴亮; 董亚东
Original assignee: Haian Haochi Technology Co ltd
Current assignee: Haian Haochi Technology Co ltd
Priority date: 2021-10-19
Filing date: 2021-10-19
Publication date: 2021-12-31

Abstract

The invention discloses preparation of low-fading nano heat-insulation slurry and coating and application of a heat-insulation automobile film, wherein nano silicon dioxide and modified silicon dioxide are mixed and dispersed to generate bonding effect to form uniform dispersion suspension; and mixing the dispersed suspension and the high-performance ATO solution by a liquid dispersion machine, and adjusting the zeta potential value of the mixed solution to prepare the low-fading nano heat-insulating slurry. The low-fading nano heat insulation slurry is mixed with a solvent, and the composite glue is added to prepare the low-fading nano heat insulation coating. The invention uses the chemical bonding effect among molecules, adjusts the zeta potential value of the mixed liquid by a flocculating agent through a mechanical dispersion procedure, thereby preparing the nano heat insulation slurry with stable performance. The low-fading nano heat-insulating slurry with stable performance of the heat-insulating vehicle film does not generate blue light and white fog, is not oxidized, faded and blocked GPS, has lasting color and luster, can be kept for a long time without fading, and has long service life.

Description

Preparation of low-fading nano heat-insulating slurry and coating and application of heat-insulating automobile film

Technical Field

The invention relates to the field of vehicle membranes, in particular to a preparation process and application of low-fading nano heat-insulating slurry and coating

Use of a thermally insulating automotive film.

Background

Energy conservation and environmental protection are the main subjects of the world. Modern automobiles and the like commonly use glass windows, particularly in summer. The heat insulation problem cannot be effectively reduced, so that great energy consumption and environmental problems are brought.

The nano transparent heat insulation coating has excellent heat insulation performance and higher visible light transmittance, can achieve better effects of saving energy and reducing consumption, has very high application value and wide market prospect, and thus is more and more widely concerned by people.

Because the cold air is always not cool after being arranged in the vehicle, after the film is pasted for a period of time or in hot summer of the next year, the phenomenon that the cold air is not blown at noon and is cooled at dusk occurs in the vehicle, and people can think that the cold air is a problem generally under the condition. Otherwise, the heat insulation effect of the heat insulation film is degraded or the heat insulation of the film attached to a new car is low, which is a main cause of coolness.

The general films sold in the market have large quality difference of heat insulation performance, the poor films are easy to fade and have low heat insulation, after the general films are used for a period of time, almost only one layer of film without heat insulation is adhered, the temperature rise in the car cannot be rapidly reduced, the refrigeration effect in the car is poor, and in order to solve the defects that the existing car films are easy to fade and have low heat insulation, the heat insulation car adhering film with stable performance and low fading of infrared ray blocking rate is urgently needed to be developed.

Disclosure of Invention

Aiming at the defects in the prior art, the invention provides a preparation process of low-fading nano heat-insulating slurry and application of a heat-insulating automobile film, so that the current situation of the heat-insulating film which is easy to fade and low in heat insulation is relieved, and the problem of the quality of ambient air can be effectively relieved.

In order to achieve the purpose, the invention provides the following technical scheme: the preparation process of the low-recession nano heat insulation slurry comprises the following steps of: mixing and dispersing the nano silicon dioxide and the modified silicon dioxide to generate bonding effect to form uniform dispersed suspension;

mixing a dispersion suspension and a high-performance ATO solution by a liquid disperser, wherein the ATO solution is a high-performance heat insulation liquid, adjusting the zeta potential value of the mixed solution, adjusting the zeta potential value of the dispersion suspension by a flocculating agent, and preparing the low-fading nano heat insulation slurry, wherein the weight percentage of the flocculating agent is not more than 2% of the weight of the dispersion suspension;

preferably, the power of the liquid dispersion machine is 8-15KW, and the rotating speed of the main shaft is 40-45 r/min.

Preferably, the modified silicon dioxide is prepared by blending and dispersing octa-aminopropyl cage-type polysilsesquioxane accounting for 0.05-1 wt% of the mass of the nano silicon dioxide, and amino contained in the octa-aminopropyl cage-type polysilsesquioxane and hydrogen-containing groups such as hydroxyl or carboxyl and the like contained in the silicon dioxide generate bonding action by removing water molecules.

The preparation process of the low-fading nano heat-insulating coating comprises the following steps of: mixing the prepared low-fading nano heat-insulating slurry with a solvent, wherein the solvent is toluene, stirring for 0.5-1.5 hours at the rotation speed of 550rpm of a mixing stirrer, adding the composite adhesive, mixing for 10-15 minutes, then adding the curing agent, and continuously stirring uniformly to prepare the low-fading nano heat-insulating coating.

Preferably, the weight ratio of the low-fading nano thermal insulation slurry to the solvent is 2: 1.

Preferably, the composite adhesive accounts for 10-15% of the weight of the low-fading nano heat insulation slurry.

Further, the compound glue is prepared by the following steps: mixing glue and a solvent, then adding a siloxane coupling agent to prepare the silicone resin modified acrylic emulsion, wherein the used solvent is toluene, the weight ratio of the glue to the solvent is 1:1, and stirring for 1 hour at the rotating speed of 500rpm to achieve the aim of uniform mixing.

Preferably, the siloxane coupling agent accounts for 1-5% of the weight of the composite adhesive.

A low-fading nano heat-insulating coating is applied to the field of preparation of nano heat-insulating automobile films.

Compared with the prior art, the invention has the following beneficial effects: the heat insulation slurry, the preparation process of the low-fading nano heat insulation coating, the prepared low-fading nano heat insulation slurry, the low-fading nano heat insulation coating and the application of the coating on a heat insulation vehicle membrane have the following beneficial effects:

(1) the invention uses the chemical bonding effect among molecules, adjusts the zeta potential value of the mixed liquid by a flocculating agent through a mechanical dispersion procedure, thereby preparing the nano heat insulation slurry with stable performance.

(2) The low-fading nano heat-insulating slurry with stable performance of the heat-insulating vehicle film does not generate blue light and white fog, is not oxidized, faded and blocked GPS, has lasting color and luster, and more importantly, can be kept for a long time without fading and has long service life.

Drawings

The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:

FIG. 1 is a flow chart of a process for making a low-recession nano thermal insulation slurry according to the present invention;

FIG. 2 is a flow chart of a process for making a low-fade nano thermal barrier coating of the present invention;

FIG. 3 is a flow chart of a process for making the compound glue of the present invention;

FIG. 4 is a graph comparing the heat insulation data of a conventional heat insulation automobile film on the market with the low-fading heat insulation automobile film manufactured according to the embodiment in the ultraviolet aging test box according to the embodiment of the invention;

fig. 5 is a graph comparing the performance of the low-fade, thermally insulating automotive film prepared in this example with a commercially available front barrier film.

Detailed Description

The technical solutions of the present invention will be described clearly and completely in the following embodiments of the present invention, and it should be understood 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.

Referring to fig. 1, fig. 1 is a flow chart of a process for manufacturing a low-degradation nano thermal insulation slurry according to the present invention. As shown in fig. 1, the process for manufacturing the low-recession nano thermal insulation slurry of the present invention comprises the following steps:

s11, adding 18ml of deionized water, 8ml of propanol, 2ml of butyronitrile and 0.4ml of ammonia water into a flask at one time to obtain a heterogeneous solution, then adding 44.0g of gamma-aminopropyl triethoxy siloxane into the flask, heating the solution to 50 ℃ under a stirring state, filtering a precipitated white crystal and washing the white crystal for 3 times by using ice methanol after 12 hours, and finally performing vacuum drying for 24 hours at 800c to synthesize the octa-aminopropyl cage type polysilsesquioxane;

s12, mixing nano silicon dioxide and modified silicon dioxide; for modified silicon dioxide, amino contained in the octaaminopropyl cage-type polysilsesquioxane and hydrogen-containing groups such as hydroxyl or carboxyl contained in the silicon dioxide generate bonding action by removing water molecules. Because the cage type polysilsesquioxane is a nanostructure hybrid system of polyhedral oligomeric silsesquioxane, an inorganic phase is taken as a core, and a shell has an organic group, the compatibility of the cage type polysilsesquioxane is amphiphilic, the surface energy of silicon dioxide particles is reduced, and the stability of a dispersion liquid is improved;

s13, executing a mechanical dispersion program, wherein the power of the used liquid dispersion machine is 11KW, and the rotating speed of a main shaft is 43 r/min; wherein, a large amount of particles are thinned by utilizing shearing force, so that the aggregates are depolymerized, wetted, wrapped and adsorbed, and the nano particles can be effectively and uniformly dispersed.

S14, mixing the dispersed suspension and the high-performance ATO solution. The ATO solution used is a common high-performance heat insulation liquid in the market, and is mixed with the dispersion suspension, so that the high heat insulation performance of the original product is ensured, and the recession rate of the product is slowed down.

S15, executing the mechanical dispersion program again and adjusting the Zeta potential value of the mixed solution to prepare low-fading nano heat-insulating slurry, wherein according to the DLVO theory, when the absolute value of the Zeta potential is larger, the electric double layers on the surfaces of the particles are mainly expressed as repulsive force, namely, the electric double layers have stronger electrostatic effect; while at the isoelectric point this repulsion is minimal and there is little electrostatic repulsion. Generally, when the Zeta potential absolute value is more than 30 mV, the slurry has higher stability. That is, the Zeta potential of the nano thermal insulation slurry can be effectively controlled by adding the flocculating agent, so that the stability of the prepared nano thermal insulation slurry is maintained.

In the embodiment of the invention, because of the chemical bonding effect among molecules, the modified silicon dioxide has compatibility presenting amphipathy, the surface energy of silicon dioxide particles is reduced, and the stability of the dispersion liquid is improved; meanwhile, a large amount of particles are thinned by mechanical dispersion through shearing force, so that the aggregates are depolymerized, wetted, wrapped and adsorbed, and the prepared low-fading nano heat-insulating slurry has stable performance and can be maintained for a long time without agglomeration.

In the step of adjusting the zeta potential value of the dispersion in this example, the zeta potential value of the dispersion is adjusted by means of a flocculating agent, and the weight percentage of the flocculating agent must not exceed 2%. In the experiment, under the environment that the pH value is 7, the dosage of the polymeric flocculant is increased from 50mg/L to 300mg/L, the zeta value of the dispersed suspension is increased rapidly at first and reaches the optimal value at 100mg/L, then the dosage of the flocculant is increased continuously, and the zeta value is increased slowly.

The stability and functionality of the nano-insulation slurry prepared by the present invention were tested by several experiments.

(1) Sedimentation test:

the nano-sized insulating slurry prepared in example was poured into a 15 ml graduated tube, and after standing for 7 days, the height of the upper clear water column was measured. In detail, a higher height of the clear water column indicates a less stable nanoparticle. The clear water column of the nano thermal insulation slurry of the embodiment is at least 20% lower than that of the prior art.

(2) Ultraviolet-visible spectrophotometer test:

the nano-sized thermal insulating slurry dispersion prepared in this example was placed on a centrifuge and centrifuged at 3000rpm for 10 minutes. The supernatant was taken and placed in a cuvette, and its light transmittance at a wavelength of 600 nm was measured with a Hitachi U-3010 ultraviolet-visible spectrophotometer. The lower the light transmittance, the better the dispersion stability of the dispersion. The light transmittance of the nano thermal insulation slurry of the embodiment is at least 25% lower than that of the prior art.

According to the manufacturing process of the low-fading nano heat insulation slurry disclosed by the embodiment of the invention, the prepared nano heat insulation slurry is detected by a BT-9300H laser particle size analyzer, the particle size of the nano particles is between 20 and 40 nanometers, and the nano particles can be maintained in a stable state for a long time.

The following describes a process for preparing the low-recession nano thermal insulation coating from the low-recession nano thermal insulation slurry prepared in the embodiment. Referring to fig. 2, fig. 2 is a flow chart of a process for manufacturing the low-fading nano thermal insulation coating of the present invention. The manufacturing process of the low-recession nano heat-insulating coating comprises the following steps of:

s21, mixing the low-fading nano heat insulation slurry with a solvent; in this example, the solvent used was toluene, and the weight ratio of low-fade nano insulation slurry to solvent was 2: 1. In this step, the mixture is stirred for 1 hour at 500rpm to achieve uniform mixing.

S22, mixing the solution and the compound glue; the solution prepared in step S21 is mixed with the compound glue and stirred for 10 minutes to achieve the effect of thorough mixing. Wherein, the weight percentage of the composite glue is 10-15%. Specifically, the weight percentage of the pH adjuster is, for example, 11%, 12%, 13%, 14%, 15%.

S23, mixing the solution and a curing agent; curing agent 3pt was added and stirred for 20 minutes.

Referring to fig. 3, the preparation of the composite adhesive in this embodiment is shown, and fig. 3 is a flow chart of the manufacturing process of the composite adhesive of the present invention. The composite adhesive is prepared by the following steps:

s31, mixing the glue and the solvent. In this example, the solvent used was toluene, and the weight ratio of glue to solvent was 1: 1; in this step, stirring was carried out at 500rpm for 1 hour for uniform mixing.

S32, mixing the solution and the siloxane coupling agent. In detail, the percentage by weight of the siloxane coupling agent is between 1% and 5%, for example between 1%, 2%, 3%, 4%, 5%. To form a silicone resin modified acrylic emulsion, which is then used as a film forming material.

In this embodiment, the glue is polyurethane glue. So as to achieve better bonding effect.

Then, in this embodiment, the nanometer thermal insulation coating stirred uniformly is uniformly coated on the surface of the 23 μm PET base film by a slit coating process. Wherein the thickness of the coating is substantially 8 microns, and a semi-finished product material with heat insulation performance is prepared after precision compounding. After 24 hours and after curing at 60 ℃, the high-transparency acrylic pressure-sensitive adhesive is precisely coated and compounded with a release film. And UV precision coating is carried out on the back surface, and the thickness is about 2 microns substantially through ultraviolet light curing. Thus, the nano heat insulation coating of the embodiment can be prepared into the car membrane.

The surface hardness of the prepared car film is more than 3H through testing; the infrared ray blocking rate is more than 90 percent, haze is less than or equal to 1.3, (QUV 1000hrs test) Delta E is less than or equal to 0.5; the LED lamp does not have the adverse phenomena of blue light, white fog and the like under the irradiation of an LED light source with the color temperature of 10000K, and can be maintained for a long time without fading.

As shown in fig. 4, in the ultraviolet aging test box, when the irradiation time is the same, the comparison between the heat insulation data of the ordinary heat insulation automobile film on the market and the low-fading heat insulation automobile film manufactured by the experiment shows that the fading rate of the product is much slower. Fig. 5 shows the performance of the product compared with the common front barrier film on the market. As described above, the car membrane made of the low-fading nano heat-insulating coating according to the embodiment has a remarkably long heat-insulating effect, and is a perfect car membrane product which is free from oxidation, fading, blocking of the GPS, high in heat insulation, high in light transmission, low in light reflection, long in color and luster, and long in service life.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims

1. The preparation process of the low-fading nano heat insulation slurry is characterized by comprising the following steps of: the preparation process of the low-recession nano heat insulation slurry comprises the following steps of: mixing and dispersing the nano silicon dioxide and the modified silicon dioxide to generate bonding effect to form uniform dispersed suspension;

mixing the dispersion suspension and a high-performance ATO solution by a liquid disperser, wherein the ATO solution is a high-performance heat insulation liquid, adjusting the zeta potential value of the mixed solution, adjusting the zeta potential value of the dispersion suspension by a flocculating agent, and preparing the low-fading nano heat insulation slurry, wherein the weight percentage of the flocculating agent is not more than 2% of the weight of the dispersion suspension.

2. The preparation process of the low-fading nano heat insulation slurry as claimed in claim 1, wherein the preparation process comprises the following steps: the power of the liquid dispersion machine is 8-15KW, and the rotating speed of the main shaft is 40-45 r/min.

3. The preparation process of the low-fading nano heat insulation slurry as claimed in claim 1, wherein the preparation process comprises the following steps: the modified silicon dioxide is prepared by blending and dispersing octa-aminopropyl cage type polysilsesquioxane accounting for 0.05-1 wt% of the mass of the nano silicon dioxide.

4. A manufacturing process of a low-fading nano heat-insulating coating is characterized by comprising the following steps: comprises the following steps: mixing the prepared low-fading nano heat-insulating slurry with a solvent, wherein the solvent is toluene, stirring for 0.5-1.5 hours at the rotation speed of 550rpm of a mixing stirrer, adding the composite adhesive, mixing for 10-15 minutes, then adding the curing agent, and continuously stirring uniformly to prepare the low-fading nano heat-insulating coating.

5. The manufacturing process of the low-fading nano heat insulation coating as claimed in claim 4, wherein the manufacturing process comprises the following steps: the weight ratio of the low-fading nano heat insulation slurry to the solvent is 2: 1.

6. The manufacturing process of the low-fading nano heat insulation coating as claimed in claim 4, wherein the manufacturing process comprises the following steps: the composite adhesive accounts for 10-15% of the weight of the low-fading nano heat-insulating slurry.

7. The manufacturing process of the low-fading nano heat insulation coating as claimed in claim 4, wherein the manufacturing process comprises the following steps: the composite adhesive is prepared by the following steps: mixing glue and a solvent, then adding a siloxane coupling agent to prepare the silicone resin modified acrylic emulsion, wherein the used solvent is toluene, the weight ratio of the glue to the solvent is 1:1, and stirring for 1 hour at the rotating speed of 500rpm to achieve the aim of uniform mixing.

8. The manufacturing process of the low-fading nano heat insulation coating as claimed in claim 4, wherein the manufacturing process comprises the following steps: the siloxane coupling agent accounts for 1-5% of the weight of the composite adhesive.

9. The application of the low-recession nano thermal insulation coating of claim 4, wherein the low-recession nano thermal insulation coating is coated on the surface of a PET base film for preparing a nano thermal insulation automobile film.