CN112680016A - Automobile paint component and preparation method thereof - Google Patents
Automobile paint component and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of water-based paint, and particularly relates to an automobile paint component and a preparation method thereof. The product developed by the invention comprises acrylate-epoxy resin emulsion and graphene oxide; the acrylate-epoxy resin emulsion contains emulsion particles, and the particle size distribution range of the emulsion particles is 1-10 nm; the emulsion particles are at least partially dispersed between graphene oxide layers. The preparation method comprises the steps of mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating for reaction under the protection of inert gas, cooling when the epoxy equivalent value reaches 1200-1300g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 80-90 ℃, stirring for mixing, adding cationic acrylate, a crosslinking agent and modified graphene oxide, and continuing heating and stirring for reaction after ultrasonic dispersion; and (3) after the reaction is finished, adding an acid solution, adjusting the acid value to be 40-50mgKOH/g, and stirring and mixing uniformly to obtain the automobile paint component.
Description
Technical Field
The invention belongs to the technical field of water-based paint. And more particularly to an automotive paint component and a method of making the same.
Background
In the field of traditional automobile coating, most automobile manufacturers mainly adopt solvent-based coatings for automobile coating, and the solvent-based coatings easily generate a large amount of volatile organic compounds in the using process, so that the environment is polluted, and the health of people is harmed. With the continuous improvement of living standard, people's environmental awareness is also continuously strengthened, and in order to reduce the environmental pollution caused by VOC (volatile organic compounds) in the automobile coating process, water-based paint is more and more applied. Compared with solvent-based automobile coatings, the water-based automobile coating has the characteristics of high technical content, high added value and the like, is green and environment-friendly, and has the advantages of various aspects such as bright color, high glossiness, good impact resistance, hard coating, strong wear resistance, good adhesion capacity, good heat resistance, quick drying, simple construction and the like. Therefore, the adoption of green and environment-friendly water-based paint instead of solvent-based paint has become an important trend in the field of automobile coating. Waterborne automotive coatings have some common drawbacks compared to solvent-based coatings: (1) the water-based paint has higher requirement on the cleanliness of a construction surface, and because the surface tension of water is higher, shrinkage cavities are more easily generated on the construction surface if pollutants exist; (2) the water-based paint has higher corrosivity to a construction surface, so the spraying work of the anticorrosion primer must be done on the construction surface, and if the spraying of the anticorrosion primer is not tight, pits are easy to generate on a coating film; (3) the water-based paint has higher requirements on construction environments (temperature and humidity) in the automobile coating process, and the investment of environment maintaining equipment is increased; (4) the water resistance of the water-based paint is poorer, the pH value of the water-based paint is generally between 8.3 and 8.8, the water-based paint is alkalescent, and ester bonds in the paint are easy to hydrolyze in water to damage molecular chains, so that the stability of a coating film is influenced. Due to the defects, the water-based paint is difficult to be widely used in the field of automobile coating.
Disclosure of Invention
The invention aims to overcome the defects and shortcomings that a water-based paint used for the existing automobile coating is used as an automobile body primer, a tight coating film is difficult to form on the metal surface of an automobile body in the using process, the appearance of the coating film is poor, and the binding force between the coating film and the automobile body is not firm, and provides an automobile paint component and a preparation method thereof.
The invention aims to provide an automobile paint component.
It is another object of the present invention to provide a method for preparing an automotive vehicle paint component.
The above purpose of the invention is realized by the following technical scheme:
the automobile paint component comprises acrylate-epoxy resin emulsion and graphene oxide;
the acrylate-epoxy resin emulsion contains emulsion particles, and the particle size distribution range of the emulsion particles is 1-10 nm;
the emulsion particles are at least partially dispersed between graphene oxide layers.
According to the technical scheme, the acrylate-epoxy resin emulsion particles with specific nanometer sizes and particle size distribution ranges are used as one of the components of the automobile paint, and in the electrophoresis process, firstly, the emulsion particles with smaller particle sizes are easier to uniformly deposit on the surface of an automobile body to form a flat coating film; secondly, the emulsion particles with a specific particle size distribution range are selected, and because of the monodisperse emulsion particles, pores formed when the particles are stacked are also uniform, so that the unevenness of a coating film caused by nonuniform local shrinkage in a drying process due to nonuniform particle stacking pores can be effectively avoided; moreover, an acrylate-epoxy resin emulsion system is selected, wherein the epoxy resin can endow the coating film with relatively better corrosion resistance, and the acrylate can provide more excellent aging resistance;
according to the technical scheme, the graphene oxide is used, and partial emulsion particles are dispersed among layers of the graphene oxide, in the using process of a product, as moisture among the emulsion particles is gradually volatilized, the particles are continuously condensed with each other, and cohesion is formed, and the emulsion particles embedded among the graphene oxide layers can be used as a 'bearing' for relative sliding among the layers, in the process, the internal stress generated by the cohesion can enable the stacking result of the graphene oxide layers to be damaged and converted into a monolithic layer structure, in the emulsion drying process, the emulsion particles are self-assembled among the emulsion particles, in the assembling process, the emulsion particles with small particle sizes are adsorbed and condensed, and the defect that the coating thickness is increased disadvantageously due to the fact that the emulsion particles are too small is avoided.
Further, the graphene oxide molecular structure comprises a conjugate region and an edge region; the conjugated region is distributed in hydroxyl and epoxy groups; the epoxy groups are at least partially converted to amino groups.
According to the technical scheme, amino is further introduced between graphene oxide layers, and in the using process, due to the influence of an acidic environment of a system, amino groups in graphene oxide conjugated regions can be protonated by hydrogen ions, and due to the fact that the graphene oxide conjugated regions have the same positive charges, electrostatic repulsion is formed between layers, so that relative slippage is easily generated under the action of internal stress in the drying process of a paint film.
Further, the liquid also comprises ionic liquid; the ionic liquid is selected from any one of 1-alkyl-3-methyl imidazole bromide and N-alkyl-N-methyl pyrrole bromide.
The technical proposal further introduces ionic liquid into the system; the ionic liquid has the advantages that the ionic liquid has the characteristics of belonging to a compound composed of anions and cations, and can play a role in balancing charges among all components of an emulsion system in the electrophoretic deposition process, so that all the components in a product are deposited on the surface of a vehicle body more uniformly, the conductivity of the system can be further improved by introducing the ionic liquid, the rapid deposition on the surface of the vehicle body in the electrophoretic deposition process is facilitated, and the processing efficiency is improved.
The preparation method of the automobile paint component comprises the following specific preparation steps:
modification of graphene oxide:
mixing graphene oxide and a sodium azide aqueous solution, carrying out ultrasonic reaction, filtering, washing and drying to obtain pretreated graphene oxide;
dispersing the pretreated graphene oxide in N-methyl pyrrolidone, adding lithium aluminum tetrahydride, and carrying out heating reduction reaction to obtain modified graphene oxide;
preparation of the automotive paint component:
mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating for reaction under the protection of inert gas, cooling when the epoxy equivalent value reaches 1200-1300g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 80-90 ℃, stirring for mixing, adding cationic acrylate, a crosslinking agent and modified graphene oxide, performing ultrasonic dispersion, and continuing heating and stirring for reaction;
and (3) after the reaction is finished, adding an acid solution, adjusting the acid value to be 40-50mgKOH/g, uniformly stirring and mixing, and discharging to obtain the automobile paint component.
Further, the specific preparation steps further comprise:
after the acid value is adjusted, adding ionic liquid; the ionic liquid is selected from any one of 1-alkyl-3-methyl imidazole bromide and N-alkyl-N-methyl pyrrole bromide.
Further, the epoxy resin is selected from any one of epoxy resin E-42, epoxy resin E-44 and epoxy resin E-51.
Further, the acid solution is selected from any one of a lactic acid solution, an acetic acid solution, an oxalic acid solution, a citric acid solution, and a succinic acid solution.
Detailed Description
The present invention is further illustrated by the following specific examples, which are not intended to limit the invention in any way. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Unless otherwise indicated, reagents and materials used in the following examples are commercially available.
Example 1
Modification of graphene oxide:
according to the mass ratio of 1: 3, mixing graphene oxide and a 15 mass percent sodium azide aqueous solution, pouring the mixture into a reactor, carrying out heat preservation ultrasonic reaction for 3 hours at the ultrasonic frequency of 50kHz and the temperature of 65 ℃, filtering, collecting a filter cake, washing the filter cake for 3 times by deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight at the temperature of 80 ℃ to obtain pretreated graphene oxide;
according to the mass ratio of 1: dispersing the pretreated graphene oxide in N-methyl pyrrolidone, adding lithium aluminum hydride accounting for 5% of the mass of the pretreated graphene oxide, heating, stirring and reducing for 2 hours at the temperature of 80 ℃ and the stirring speed of 300r/min, filtering, collecting a filter cake, washing for 3 times by using the N-methyl pyrrolidone, and then drying the washed filter cake in vacuum to obtain modified graphene oxide;
preparation of the automotive paint component:
according to the weight parts, 100 parts of epoxy resin, 4 parts of dodecylphenol, 5 parts of xylene, 3 parts of dimethylbenzylamine, 10 parts of ethylene glycol monobutyl ether, 8 parts of xylene, 10 parts of isobutanol, 3 parts of hydroxymethylethanolamine, 30 parts of cationic acrylate, 3 parts of crosslinking agent EGDMA and 10 parts of modified graphene oxide are taken in sequence; mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating and stirring for reaction at the temperature of 120 ℃ and the stirring speed of 400r/min under the protection of inert gas, cooling when the equivalent value of epoxy reaches 1200g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 80 ℃, stirring and mixing for 10min at the speed of 400r/min by using a stirrer, adding cationic acrylate 6305, a crosslinking agent EGDMA and modified graphene oxide, performing ultrasonic dispersion for 10min at the frequency of 60kHz, and continuing heating and stirring for reaction for 3h at the temperature of 80 ℃ and the speed of 600 r/min;
after the reaction is finished, adding an acid solution, adjusting the acid value to be 40mgKOH/g, adding an ionic liquid accounting for 5% of the mass of the epoxy resin, stirring and mixing uniformly, and discharging to obtain the automobile paint component;
the ionic liquid is selected from 1-alkyl-3-methyl imidazole bromide; the epoxy resin is selected from epoxy resin E-42; the acid solution is selected from lactic acid solutions.
Example 2
Modification of graphene oxide:
according to the mass ratio of 1: mixing graphene oxide and a sodium azide aqueous solution with the mass fraction of 20% and pouring the mixture into a reactor, carrying out heat preservation ultrasonic reaction for 5 hours at the ultrasonic frequency of 60kHz and the temperature of 68 ℃, filtering, collecting a filter cake, washing the filter cake for 4 times by deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight at the temperature of 90 ℃ to obtain pretreated graphene oxide;
according to the mass ratio of 1: dispersing the pretreated graphene oxide in N-methyl pyrrolidone, adding lithium aluminum hydride accounting for 8% of the mass of the pretreated graphene oxide, heating, stirring and reducing for 4 hours at the temperature of 85 ℃ and the stirring speed of 400r/min, filtering, collecting a filter cake, washing for 4 times by using the N-methyl pyrrolidone, and then drying the washed filter cake in vacuum to obtain the modified graphene oxide;
preparation of the automotive paint component:
according to the weight parts, 120 parts of epoxy resin, 8 parts of dodecylphenol, 6 parts of xylene, 5 parts of dimethylbenzylamine, 15 parts of ethylene glycol monobutyl ether, 9 parts of xylene, 12 parts of isobutanol, 5 parts of hydroxymethyl ethanolamine, 35 parts of cationic acrylate, 5 parts of crosslinking agent EGDMA and 16 parts of modified graphene oxide are taken in sequence; mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating and stirring for reaction at the temperature of 130 ℃ and the stirring speed of 600r/min under the protection of inert gas, cooling when the equivalent value of epoxy reaches 1250g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 85 ℃, stirring and mixing for 20min at the speed of 500r/min by using a stirrer, adding cationic acrylate 6305, a crosslinking agent EGDMA and modified graphene oxide, performing ultrasonic dispersion for 15min at the frequency of 70kHz, and continuing heating and stirring for reaction for 4h at the temperature of 85 ℃ and the speed of 800 r/min;
after the reaction is finished, adding an acid solution, adjusting the acid value to be 45mgKOH/g, adding an ionic liquid accounting for 8% of the mass of the epoxy resin, stirring and mixing uniformly, and discharging to obtain the automobile paint component;
the ionic liquid is selected from N-alkyl-N-methyl pyrrole bromide; the epoxy resin is selected from epoxy resin E-51; the acid solution is selected from acetic acid solution.
Example 3
Modification of graphene oxide:
according to the mass ratio of 1: 5, mixing graphene oxide and a 30% sodium azide aqueous solution, pouring the mixture into a reactor, carrying out heat preservation ultrasonic reaction for 6 hours at the ultrasonic frequency of 80kHz and the temperature of 75 ℃, filtering, collecting a filter cake, washing the filter cake for 5 times by deionized water, transferring the washed filter cake into a drying oven, and drying the filter cake to constant weight at the temperature of 100 ℃ to obtain pretreated graphene oxide;
according to the mass ratio of 1: 8, dispersing the pretreated graphene oxide in N-methyl pyrrolidone, adding lithium aluminum hydride accounting for 10% of the mass of the pretreated graphene oxide, heating, stirring and reducing for 6 hours at the temperature of 90 ℃ and at the stirring speed of 500r/min, filtering, collecting a filter cake, washing for 5 times by using the N-methyl pyrrolidone, and then drying the washed filter cake in vacuum to obtain modified graphene oxide;
preparation of the automotive paint component:
according to the weight parts, 150 parts of epoxy resin, 10 parts of dodecylphenol, 8 parts of xylene, 6 parts of dimethylbenzylamine, 20 parts of ethylene glycol monobutyl ether, 10 parts of xylene, 15 parts of isobutanol, 6 parts of hydroxymethyl ethanolamine, 50 parts of cationic acrylate, 6 parts of crosslinking agent EGDMA and 20 parts of modified graphene oxide are taken in sequence; mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating and stirring for reaction at 140 ℃ and the stirring speed of 800r/min under the protection of inert gas, cooling when the equivalent value of epoxy reaches 1300g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 90 ℃, stirring and mixing for 30min at the rotation speed of 600r/min by using a stirrer, adding cationic acrylate 6305, a crosslinking agent EGDMA and modified graphene oxide, performing ultrasonic dispersion for 30min at the frequency of 80kHz, and continuing heating and stirring for reaction for 6h at the temperature of 90 ℃ and the rotation speed of 900 r/min;
after the reaction is finished, adding an acid solution, adjusting the acid value to be 50mgKOH/g, adding an ionic liquid accounting for 10% of the mass of the epoxy resin, stirring and mixing uniformly, and discharging to obtain the automobile paint component;
the ionic liquid is selected from 1-alkyl-3-methyl imidazole bromide; the epoxy resin is selected from epoxy resin E-44; the acid solution is selected from citric acid solutions.
Comparative example 1
This comparative example differs from example 1 in that: the graphene oxide is directly used without modification treatment, and the rest conditions are kept unchanged.
Comparative example 2
This comparative example differs from example 1 in that: graphene oxide is not added, and the other conditions are kept unchanged;
because of the lack of graphene oxide, the emulsion particles are easily agglomerated to form emulsion particles with larger particle size during the formation of the emulsion particles, and thus, the actual emulsion particle size distribution range of the comparative example is 50-300 nm.
Comparative example 3
This comparative example differs from example 1 in that: no ionic liquid was added and the remaining conditions were kept constant.
The products obtained in examples 1 to 3 and comparative examples 1 to 3 were subjected to performance tests, and the specific test methods and test results were as follows:
and (3) respectively mixing the products of the examples and the comparative examples with mortar according to a mass ratio of 5: 1 preparing a primer, curing for 24 hours, and testing a swimming plate; the mortar comprises the following raw materials in parts by weight: 80 parts of water-based acrylic resin, 3 parts of lactic acid, 60 parts of water, 3 parts of titanium dioxide, 2 parts of carbon black and 3 parts of aluminum silicate;
a QUV artificial aging machine is adopted to test the accelerated aging performance index of the paint film, a neutral salt fog machine is adopted to test the salt fog resistance of the paint film, and the specific test results are as follows:
in addition, after the coating is finished, the observation of the surface of the coating shows that the products obtained by the examples 1 to 3 have more excellent flatness compared with the comparative product; and the combination of the test results shows that the product of the invention obtains more excellent corrosion resistance.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (7)
1. The automobile paint component is characterized by comprising acrylic ester-epoxy resin emulsion and graphene oxide;
the acrylate-epoxy resin emulsion contains emulsion particles, and the particle size distribution range of the emulsion particles is 1-10 nm;
the emulsion particles are at least partially dispersed between graphene oxide layers.
2. The automotive vehicle paint component of claim 1, wherein the graphene oxide comprises a conjugated region and an edge region in a molecular structure; the conjugated region is distributed in hydroxyl and epoxy groups; the epoxy groups are at least partially converted to amino groups.
3. The automotive vehicle paint component of claim 1, further comprising an ionic liquid; the ionic liquid is selected from any one of 1-alkyl-3-methyl imidazole bromide and N-alkyl-N-methyl pyrrole bromide.
4. The preparation method of the automobile paint component is characterized by comprising the following specific preparation steps:
modification of graphene oxide:
mixing graphene oxide and a sodium azide aqueous solution, carrying out ultrasonic reaction, filtering, washing and drying to obtain pretreated graphene oxide;
dispersing the pretreated graphene oxide in N-methyl pyrrolidone, adding lithium aluminum tetrahydride, and carrying out heating reduction reaction to obtain modified graphene oxide;
preparation of the automotive paint component:
mixing epoxy resin, dodecylphenol, xylene and dimethylbenzylamine, heating for reaction under the protection of inert gas, cooling when the epoxy equivalent value reaches 1200-1300g/eq, adding ethylene glycol monobutyl ether, xylene, isobutanol and hydroxymethylethanolamine when the temperature is reduced to 80-90 ℃, stirring for mixing, adding cationic acrylate, a crosslinking agent and modified graphene oxide, performing ultrasonic dispersion, and continuing heating and stirring for reaction;
and (3) after the reaction is finished, adding an acid solution, adjusting the acid value to be 40-50mgKOH/g, uniformly stirring and mixing, and discharging to obtain the automobile paint component.
5. The method of preparing an automotive paint component of claim 4, wherein the specific steps further comprise:
after the acid value is adjusted, adding ionic liquid; the ionic liquid is selected from any one of 1-alkyl-3-methyl imidazole bromide and N-alkyl-N-methyl pyrrole bromide.
6. The method for preparing the automobile paint component according to claim 4, wherein the epoxy resin is any one selected from the group consisting of epoxy resin E-42, epoxy resin E-44, and epoxy resin E-51.
7. The method of preparing the automobile paint component according to claim 4, wherein the acid solution is any one selected from the group consisting of a lactic acid solution, an acetic acid solution, an oxalic acid solution, a citric acid solution, and a succinic acid solution.
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Cited By (1)
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Application publication date: 20210420 |