CN111187562A - FEVE thermosetting layered fluorocarbon powder coating and preparation method thereof - Google Patents
FEVE thermosetting layered fluorocarbon powder coating and preparation method thereof Download PDFInfo
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- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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- C09D133/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, the oxygen atom being present only as part of the carboxyl radical
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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Abstract
The invention provides an FEVE thermosetting layered fluorocarbon powder coating and a preparation method thereof, wherein after modification treatment is carried out on polymer fibers and carboxylation treatment is carried out on carbon nano tubes, generated active groups such as hydroxyl, carboxyl and the like are favorable for better compatibility and dispersibility with other components in the powder coating, the adhesiveness of a mixed filler in the powder coating is improved, raw materials are sequentially added into a reaction kettle according to the properties of the raw materials, and an ultrasonic generating device and a grinding device are arranged in the reaction kettle, so that the granularity of the raw materials is ensured to be within a specified range, the problem of uneven dispersion of the powder coating in the preparation process is solved, the uniformity and the consistency of the performance of the integral structure of a mixture are improved, and the quality of the powder coating is further ensured. In addition, the prepared powder coating has excellent corrosion resistance, impact resistance, weather resistance, impact toughness, fatigue resistance and adhesion when a coating film is formed.
Description
Technical Field
The invention relates to the field of powder coating preparation, in particular to an FEVE thermosetting layered fluorocarbon powder coating and a preparation method thereof.
Background
The existing oxygen-carbon paint is brittle and easy to age, the corrosion resistance of the oxygen-carbon paint can be improved by adding inorganic nano materials, and the epoxy paint and a cured product thereof show excellent heat resistance because the oxygen-carbon paint contains epoxy groups, ether bonds, carboxyl groups and the like. The cured oxygen-carbon coating has a three-dimensional network structure, so that the cured oxygen-carbon coating has poor impact toughness, brittle property and poor fatigue resistance, and the product performance is greatly influenced, so that the oxygen-carbon coating is generally required to be modified to achieve the required comprehensive performance. In addition, in the prior art, the particle size of the powder coating is difficult to control in the preparation process, raw materials need to be ground in additional equipment and then added, the steps of the preparation process are increased, and the energy consumption is high.
For example, patent No. CN109749492A discloses an epoxy polyester powder coating, but the fatigue resistance is poor. For another example, patent No. CN106893414A discloses an environment-friendly FEVE fluorocarbon coating and a preparation method thereof, which are complicated to prepare and cannot obtain a powder coating with high binding degree and adhesion. For example, WO2015074622A1 discloses a polyester hot melt adhesive for powder coating and a preparation method thereof, but the method has complex process and large labor cost.
In the field of preparing powder coatings, particularly fluorocarbon powder coatings, many practical problems to be treated in practical application still leave no specific solution.
Disclosure of Invention
The invention provides an FEVE thermosetting layered fluorocarbon powder coating and a preparation method thereof to solve the problems.
In order to achieve the purpose, the invention adopts the following technical scheme:
the preparation method of the oxygen-carbon powder comprises the following steps:
(1) weighing materials such as polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol, ethylene glycol butyl ether and the like;
(2) slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and has friction heat generation at the temperature of 35-70 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is (15-40): (15-30): (10-25);
(3) adding the polymer fiber into a formic acid solution with the amount of 2-3 times that of the polymer fiber, heating to 65-90 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 5-8h after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain the modified polymer fiber; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 45-60g/min, stopping stirring after the addition is finished, standing, continuing stirring for 15-20min, and grinding and dispersing until the fineness is less than or equal to 25 micrometers to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 1-3h by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol butyl ether to obtain a mixture C;
(5) mixing the mixture B with the mixture C, dispersing for 15-30min by using a high-speed dispersion machine, and adding the auxiliary agent for spheroidizing and loosening treatment;
(6) adding the mixture subjected to spheroidization and loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
Optionally, the powder coating comprises the following components in parts by weight: 10-45 parts of polyurethane resin, 20-35 parts of polymethyl methacrylate, 1-5 parts of a curing agent, 8-25 parts of a mixed filler, 10-30 parts of FEVE fluorocarbon resin, 1-15 parts of PEVE emulsion, 4-8 parts of a coupling agent, 1-8 parts of a carbon nano tube, 1-5 parts of high polymer fiber, 0.6-1.6 parts of calcium chloride, 1-3 parts of propylene glycol and 1-2 parts of ethylene glycol butyl ether; and the carbon nano tube is a carboxylated carbon nano tube.
Optionally, the carboxylated carbon nanotube is prepared by dispersing the carbon nanotube in 3 times of hydrochloric acid solution, ultrasonically dispersing for 3-5h, adding distilled water, carrying out vacuum filtration for multiple times, detecting the pH value to be equal to 7, drying the solid obtained after vacuum filtration, repeatedly grinding, dispersing the ground powder into mixed acid, ultrasonically dispersing for 5-8h, adding distilled water again, repeatedly carrying out vacuum filtration to make the pH value within the range of 6-7, and drying in a drying oven at 95-100 ℃ for 10-15 h.
Optionally, the curing agent is any one or a combination of two or more of ethylenediamine, diethylenetriamine, triethylenetetramine, xylylenediamine, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, and β -hydroxyethyl ethylenediamine.
Optionally, the mixed filler is any one or a combination of more than two of titanium dioxide, chrome yellow, calcium carbonate, calcined kaolin, talcum powder and barium sulfate.
Optionally, the auxiliary agent comprises an adhesion promoter and a nano modifier, and is a solid organic silicon-phosphorus auxiliary agent.
Optionally, the coupling agent is prepared by mixing an aluminum zirconium coupling agent and a silane coupling agent according to the proportion of 1-5: 1-9.
Optionally, the reaction kettle comprises a kettle body, an ultrasonic generating device, a stirring device and a grinding device, wherein the stirring device and the grinding device are fixedly arranged in the kettle body, the ultrasonic generating device is composed of ultrasonic pulse units arranged at intervals along the outer side wall of the kettle body, the ultrasonic pulse units are arranged into 10-30 groups from top to bottom, each group is 10-50 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit comprises an ultrasonic generator and an energy converter which are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth.
Optionally, the temperature during the spheroidization loosening treatment is not more than 15 ℃.
Compared with the prior art, the invention has the beneficial technical effects that:
1. according to the fluorocarbon powder coating, after the modification treatment is carried out on the polymer fibers and the carboxylation treatment is carried out on the carbon nano tubes, generated active groups such as hydroxyl, carboxyl and the like are beneficial to having better compatibility and dispersibility with other components in the preparation process of the powder coating, and the dispersibility and the adhesiveness of the mixed filler in the powder coating are improved.
2. In the preparation process of the powder coating, the raw materials are sequentially added into the reaction kettle under different feeding conditions according to the properties of the raw materials, and the ultrasonic generating device and the grinding device are arranged in the reaction kettle, so that the granularity of the raw materials is ensured to be within a specified range, the problem of uneven dispersion of the powder coating in the preparation process is solved, the uniformity of the integral structure of the mixture and the consistency of the properties can be improved, and the quality of the powder coating is further ensured.
3. When a coating film is formed, the powder coating has excellent corrosion resistance, impact resistance, weather resistance, impact toughness resistance and fatigue resistance, and the adhesion of the film layer is good.
4. The powder coating disclosed by the invention is simple to prepare, and can reduce grinding equipment of raw materials, so that the energy consumption and the cost are reduced.
Drawings
The invention will be further understood from the following description in conjunction with the accompanying drawings. The components in the figures are not necessarily to scale, emphasis instead being placed upon illustrating the principles of the embodiments. Like reference numerals designate corresponding parts throughout the different views.
FIG. 1 is a schematic flow chart of a preparation process of an FEVE thermosetting layered fluorocarbon powder coating in one embodiment of the present invention;
FIG. 2 is a schematic structural view of a reaction vessel in one embodiment of the present invention;
fig. 3 is a schematic view of the powder coating forming a coating film.
Description of reference numerals: 1-a material guide plate; 2-grinding roller; 3-an ultrasonic pulse unit; 4-stirring device.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to embodiments thereof; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. Other systems, methods, and/or features of the present embodiments will become apparent to those skilled in the art upon review of the following detailed description. It is intended that all such additional systems, methods, features and advantages be included within this description, be within the scope of the invention, and be protected by the accompanying claims. Additional features of the disclosed embodiments are described in, and will be apparent from, the detailed description that follows.
The same or similar reference numerals in the drawings of the embodiments of the present invention correspond to the same or similar components; in the description of the present invention, it should be understood that if there is an orientation or positional relationship indicated by the terms "upper", "lower", "left", "right", etc. based on the orientation or positional relationship shown in the drawings, it is only for convenience of describing the present invention and simplifying the description, but it is not intended to indicate or imply that the device or component referred to must have a specific orientation, be constructed in a specific orientation, and be operated, and therefore, the terms describing the positional relationship in the drawings are only used for illustrative purposes and are not to be construed as limiting the present patent, and the specific meaning of the terms described above will be understood by those of ordinary skill in the art according to the specific circumstances.
The invention relates to a FEVE thermosetting layered fluorocarbon powder coating and a preparation method thereof, which teach the following embodiments according to the description of the attached drawings:
example 1:
according to the figure 1, the invention provides an FEVE thermosetting layered fluorocarbon powder coating, and the preparation method of the oxygen-carbon powder comprises the following steps:
(1) weighing materials such as polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol, ethylene glycol butyl ether and the like;
(2) slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and has friction heat generation at the temperature of 35-70 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is (15-40): (15-30): (10-25);
(3) adding the polymer fiber into a formic acid solution with the amount of 2-3 times that of the polymer fiber, heating to 65-90 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 5-8h after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain the modified polymer fiber; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 45-60g/min, stopping stirring after the addition is finished, standing, continuing stirring for 15-20min, and grinding and dispersing until the fineness is less than or equal to 25 micrometers to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 1-3h by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol butyl ether to obtain a mixture C;
(5) mixing the mixture B and the mixture C, dispersing for 15-30min by using a high-speed dispersion machine, adding the aid for spheroidizing and loosening treatment, wherein the temperature during the spheroidizing and loosening treatment is not more than 15 ℃;
(6) adding the mixture subjected to spheroidization loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
The powder coating comprises, by weight, 10-45 parts of polyurethane resin, 20-35 parts of polymethyl methacrylate, 1-5 parts of a curing agent, 8-25 parts of a mixed filler, 10-30 parts of FEVE fluorocarbon resin, 1-15 parts of PEVE emulsion, 4-8 parts of a coupling agent, 1-8 parts of carbon nanotubes, 1-5 parts of polymer fibers, 0.6-1.6 parts of calcium chloride, 1-3 parts of propylene glycol and 1-2 parts of ethylene glycol butyl ether, wherein the carbon nanotubes are carboxylated carbon nanotubes, the carboxylated carbon nanotubes are dispersed in a hydrochloric acid solution in an amount which is 3 times that of the amount of the carbon nanotubes, distilled water is added after ultrasonic dispersion for 3-5 hours, the mixture is subjected to vacuum filtration for many times and is detected to have a pH value of 7, the solid obtained after the vacuum filtration is dried and repeatedly ground, the ground powder is dispersed in mixed acid and subjected to ultrasonic dispersion for 5-8 hours, the distilled water is added again subjected to repeated vacuum filtration to make the pH value within a range of 6-7, the mixture is placed in a drying box for drying for 10-15 hours, the mixture of m-phenylenediamine, the mixture of the carboxyl-diaminobenzene coupling agent, the modified ethylene diamine, the additive, the ethylene diamine and the additive is calcined, the mixture of ethylene diamine, the additive is prepared by mixing of ethylene diamine, the additive of propylene diamine and the additive, the additive is one or more than two additives of the additive, the additive of propylene diamine coupling additive is prepared by mixing additive.
In addition, in this embodiment, the reaction kettle includes a kettle body, an ultrasonic generating device, a stirring device and a grinding device, the stirring device and the grinding device are fixedly arranged in the kettle body, the ultrasonic generating device is composed of ultrasonic pulse units arranged at intervals along the outer side wall of the kettle body, the ultrasonic pulse units are arranged into 10-30 groups from top to bottom, each group is 10-50 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit includes an ultrasonic generator and a transducer which are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth.
Example 2:
as can be seen from fig. 1, in this embodiment, there is provided a FEVE thermosetting layered fluorocarbon powder coating, and the preparation method of the oxygen-carbon powder includes the following steps:
(1) weighing materials such as polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol, ethylene glycol butyl ether and the like; and the carbon nano tube is a carboxylated carbon nano tube, the carboxylated carbon nano tube is prepared by dispersing the carbon nano tube in 3 times of hydrochloric acid solution, ultrasonically dispersing for 3 hours, adding distilled water, carrying out vacuum filtration for multiple times, detecting the pH value to be equal to 7, drying the solid obtained after the vacuum filtration, repeatedly grinding, dispersing the ground powder into mixed acid, ultrasonically dispersing for 5-8 hours, adding distilled water again, repeatedly carrying out vacuum filtration for 5-8 hours, keeping the pH value within 6, and drying in a drying oven at 95-100 ℃ for 10 hours to obtain the carboxylated carbon nano tube.
(2) Slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and has frictional heat generation at the temperature of 35-70 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is 15: 15: 10;
(3) adding polymer fibers into a formic acid solution with the amount being 2 times that of the polymer fibers, heating to 65 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 5 hours after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain modified polymer fibers; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 45-60g/min, stopping stirring after the addition is finished, standing, continuing stirring for 15min, and grinding and dispersing until the fineness is less than or equal to 25 micrometers to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 1h by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol monobutyl ether to obtain a mixture C;
(5) mixing the mixture B and the mixture C, dispersing for 15min by using a high-speed dispersion machine, adding the auxiliary agent for spheroidizing and loosening treatment, wherein the temperature during the spheroidizing and loosening treatment is not more than 15 ℃;
(6) adding the mixture subjected to spheroidization and loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
In this embodiment, the powder coating comprises the following components in parts by weight: 10 parts of polyurethane resin, 20 parts of polymethyl methacrylate, 1 part of curing agent, 25 parts of mixed filler, 10 parts of FEVE fluorocarbon resin, 1 part of PEVE emulsion, 4 parts of coupling agent, 1 part of carbon nano tube, 1 part of polymer fiber, 0.6 part of calcium chloride, 1 part of propylene glycol and 1 part of ethylene glycol butyl ether.
Wherein the curing agent is ethylenediamine; the mixed filler is titanium dioxide; the auxiliary agent comprises an adhesion promoter and a nano modifier, and is a solid organic silicon-phosphorus auxiliary agent; the coupling agent is prepared by mixing an aluminum zirconium coupling agent and a silane coupling agent according to the proportion of 1: 1.
As can be seen from fig. 2, in this embodiment, the reaction kettle includes a kettle body, an ultrasonic generating device, a stirring device, and a grinding device, where the stirring device and the grinding device are fixedly disposed in the kettle body, the ultrasonic generating device is formed by ultrasonic pulse units disposed at intervals along an outer side wall of the kettle body, the ultrasonic pulse units are disposed in 10 groups from top to bottom, each group is 10 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit includes an ultrasonic generator and a transducer that are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth.
Example 3:
as can be seen from fig. 1, in this embodiment, there is provided a FEVE thermosetting layered fluorocarbon powder coating, and the preparation method of the oxygen-carbon powder includes the following steps:
(1) weighing materials such as polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol, ethylene glycol butyl ether and the like; dispersing the carbon nano tube in 3 times of hydrochloric acid solution, ultrasonically dispersing for 3 hours, adding distilled water, performing vacuum filtration for multiple times, detecting the pH value to be equal to 7, drying the solid obtained after the vacuum filtration, repeatedly grinding, dispersing the ground powder into the mixed acid, ultrasonically dispersing for 5-8 hours, adding distilled water again, repeatedly performing vacuum filtration for 5-8 hours to enable the pH value to be within 6, and drying in a drying box at 95 ℃ for 10 hours to obtain the carboxylated carbon nano tube;
(2) slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and generates heat by friction at the temperature of 70 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is 40: 30: 25;
(3) adding polymer fibers into a formic acid solution with the amount being 3 times that of the polymer fibers, heating to 90 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 8 hours after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain modified polymer fibers; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 60g/min, stopping stirring after the addition is finished, standing, continuing stirring for 20min, and grinding and dispersing until the fineness is less than or equal to 25 mu m to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 3 hours by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol monobutyl ether to obtain a mixture C;
(5) mixing the mixture B and the mixture C, dispersing for 30min by using a high-speed dispersion machine, adding the auxiliary agent for spheroidizing and loosening treatment, wherein the temperature during the spheroidizing and loosening treatment is not more than 15 ℃;
(6) adding the mixture subjected to spheroidization and loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
The powder coating comprises the following components in parts by weight: 45 parts of polyurethane resin, 35 parts of polymethyl methacrylate, 5 parts of curing agent, 25 parts of mixed filler, 30 parts of FEVE fluorocarbon resin, 15 parts of PEVE emulsion, 8 parts of coupling agent, 1 part of carbon nano tube, 5 parts of high polymer fiber, 1.6 parts of calcium chloride, 1 part of propylene glycol and 2 parts of ethylene glycol butyl ether; the curing agent is prepared by mixing ethylenediamine and diethylenetriamine in a ratio of 1: 1; the mixed filler is obtained by mixing titanium dioxide, chrome yellow and calcium carbonate according to the proportion of 1:2: 1; the auxiliary agent comprises an adhesion promoter and a nano modifier, and is a solid organic silicon phosphorus auxiliary agent; the coupling agent is prepared by mixing an aluminum zirconium coupling agent and a silane coupling agent according to the proportion of 5: 9.
As can be seen from fig. 2, in this embodiment, the reaction kettle includes a kettle body, an ultrasonic generating device, a stirring device, and a grinding device, where the stirring device and the grinding device are fixedly disposed in the kettle body, the ultrasonic generating device is formed by ultrasonic pulse units disposed at intervals along an outer side wall of the kettle body, the ultrasonic pulse units are disposed in 30 groups from top to bottom, each group is 10 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit includes an ultrasonic generator and a transducer that are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth.
Example 4:
as can be seen from fig. 1, in this embodiment, there is provided a FEVE thermosetting layered fluorocarbon powder coating, and the preparation method of the oxygen-carbon powder includes the following steps:
(1) weighing materials such as polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol, ethylene glycol butyl ether and the like; dispersing the carbon nano tube in 3 times of hydrochloric acid solution, ultrasonically dispersing for 3 hours, adding distilled water, performing vacuum filtration for multiple times, detecting the pH value to be equal to 7, drying the solid obtained after the vacuum filtration, repeatedly grinding, dispersing the ground powder into the mixed acid, ultrasonically dispersing for 5-8 hours, adding distilled water again, repeatedly performing vacuum filtration for 5-8 hours to enable the pH value to be within 6, and drying in a drying box at 100 ℃ for 10 hours to obtain the carboxylated carbon nano tube;
(2) slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and generates heat by friction at the temperature of 60 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is 20: 20: 20;
(3) adding polymer fibers into a formic acid solution with the amount being 2-3 times that of the polymer fibers, heating to 80 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 6 hours after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain modified polymer fibers; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 50g/min, stopping stirring after the addition is finished, standing, continuing stirring for 20min, and grinding and dispersing until the fineness is less than or equal to 25 mu m to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 3 hours by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol monobutyl ether to obtain a mixture C;
(5) mixing the mixture B and the mixture C, dispersing for 30min by using a high-speed dispersion machine, adding the auxiliary agent for spheroidizing and loosening treatment, wherein the temperature during the spheroidizing and loosening treatment is not more than 15 ℃;
(6) adding the mixture subjected to spheroidization and loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
The powder coating comprises the following components in parts by weight: 25 parts of polyurethane resin, 25 parts of polymethyl methacrylate, 3 parts of curing agent, 15 parts of mixed filler, 20 parts of FEVE fluorocarbon resin, 12 parts of PEVE emulsion, 6 parts of coupling agent, 5 parts of carbon nano tube, 3 parts of high polymer fiber, 0.8 part of calcium chloride, 2 parts of propylene glycol and 2 parts of ethylene glycol butyl ether; the curing agent is xylylenediamine; the mixed filler is calcined kaolin; the auxiliary agent comprises an adhesion promoter and a nano modifier, and is a solid organic silicon phosphorus auxiliary agent; the coupling agent is prepared by mixing an aluminum zirconium coupling agent and a silane coupling agent according to the proportion of 3: 5.
As can be seen from fig. 2, in this embodiment, the reaction kettle includes a kettle body, an ultrasonic generating device, a stirring device, and a grinding device, where the stirring device and the grinding device are fixedly disposed in the kettle body, the ultrasonic generating device is formed by ultrasonic pulse units disposed at intervals along an outer side wall of the kettle body, the ultrasonic pulse units are disposed in 20 groups from top to bottom, each group is 30 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit includes an ultrasonic generator and a transducer that are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth. Certainly, the feed inlet is arranged at the upper part of the reaction kettle in the embodiment, the discharge outlet is arranged at the bottom of the reaction kettle, one end of the stirring device is driven by the driving motor, and when the reaction kettle works, the step (3) can be set to stand, and the stirring speed in the stirring process is continued. In the specific operation, raw materials enter from the feeding hole, the end parts of the guide plates are contacted, a closed grinding cavity is formed at the upper part of the reaction kettle, the grinding rollers repeatedly grind the raw materials until the required granularity is achieved, the rear guide plates are opened, the ground raw materials are introduced into the lower part of the reaction kettle and are mixed with other components under the action of a stirring device; and meanwhile, the ultrasonic generating device is started, and the ultrasonic generating device can intermittently generate ultrasonic vibration by setting, so that the combination degree of the mixture in the reaction kettle and the mixing uniformity are promoted, and the production quality is ensured. It should be noted that, in the present invention, the connection of the components in the reaction kettle is an electrical connection, which can be solved by the circuit design in the electrical field, and is not described in detail in the present invention.
Comparative example 1:
the only difference from example 4 is that the raw material is not ground and that there is no requirement for the fineness of mixture B and the mixed filler.
Comparative example 2:
the only difference from example 4 is that no ultrasonic generator was provided in the reaction vessel.
Comparative example 3:
the only difference from example 4 is that no milling device was provided in the reaction vessel.
Using an electrostatic spray gun, the powder coatings prepared in examples 2 to 4 and comparative examples 1 to 3 were applied to the metal surface, and the properties of the coating film were measured after baking, and Table 1 below is a table of property test data for each example and comparative example:
TABLE 1
From the analysis of the experimental results in table 1 above, it can be seen that: as seen from the comparison of the test results of examples 2-4 and comparative examples 1-3 in the table of the powder coatings of examples 2-4 and comparative examples 1-3, respectively, using an electrostatic spray gun, under the conditions of aging and salt spray resistance for 4000 hours and 10% hydrochloric acid resistance for 15 minutes, the powder coatings obtained by using the components and the preparation method of the invention obtain excellent test results in performance tests such as boiling water resistance, impact resistance (recoil), cupping test, salt spray resistance test, artificial accelerated aging resistance test, humidity resistance and the like, and the comprehensive performance of the powder coatings is obviously superior to that of the existing powder coatings. And as can be seen from the attached figure 3, the powder coating of the invention can form a smooth coating.
In addition, the following comparative examples 4 to 6 were also provided:
comparative example 4:
comparative example 4 is different from example 4 only in that the added polymer fiber is not modified, and the carbon nanotube is carboxylated.
Comparative example 5:
comparative example 5 is different from example 4 only in that the added polymer fiber is modified and the carbon nanotube is not carboxylated.
Comparative example 6:
comparative example 6 is different from example 4 only in that the added polymer fiber is not subjected to the modification treatment, and the carbon nanotube is not subjected to the carboxylation treatment.
Experimental observations of dispersibility, compatibility and adhesion of comparative example 4, comparative example 5 and comparative example 6 and example 4 were made, and comparative example 4, comparative example 5 and comparative example 6 were compared with example 4, and the results are shown in table 2 below.
TABLE 2
As can be seen from the analysis in table 2, compared with example 4, the polymer fiber of the present invention, after being modified and carboxylated, has better compatibility with other components and better dispersibility during the preparation of the powder coating, and improves the dispersibility and adhesiveness of the mixed filler in the powder coating.
In conclusion, when a coating film is formed, the powder coating has excellent corrosion resistance, impact resistance, weather resistance, impact toughness and fatigue resistance, the adhesion of the film layer is good, the preparation is simple, grinding equipment of raw materials can be reduced, and further, the energy consumption and the cost are reduced.
Although the invention has been described above with reference to various embodiments, it should be understood that many changes and modifications may be made without departing from the scope of the invention. That is, the methods, systems, and devices discussed above are examples. Various configurations may omit, substitute, or add various procedures or components as appropriate. For example, in alternative configurations, the methods may be performed in an order different than that described, and/or various components may be added, omitted, and/or combined. Moreover, features described with respect to certain configurations may be combined in various other configurations, as different aspects and elements of the configurations may be combined in a similar manner. Further, elements therein may be updated as technology evolves, i.e., many elements are examples and do not limit the scope of the disclosure or claims.
Specific details are given in the description to provide a thorough understanding of the exemplary configurations including implementations. However, configurations may be practiced without these specific details, e.g., well-known circuits, processes, algorithms, structures, and techniques have been shown without unnecessary detail in order to avoid obscuring the configurations. This description provides example configurations only, and does not limit the scope, applicability, or configuration of the claims. Rather, the foregoing description of the configurations will provide those skilled in the art with an enabling description for implementing the described techniques. Various changes may be made in the function and arrangement of elements without departing from the spirit or scope of the disclosure.
It is intended that the foregoing detailed description be regarded as illustrative rather than limiting, and that it be understood that it is the following claims, including all equivalents, that are intended to define the spirit and scope of this invention. The above examples are to be construed as merely illustrative and not limitative of the remainder of the disclosure. After reading the description of the invention, the skilled person can make various changes or modifications to the invention, and these equivalent changes and modifications also fall into the scope of the invention defined by the claims.
Claims (9)
1. The FEVE thermosetting layered fluorocarbon powder coating is characterized in that the preparation method of the fluorocarbon powder coating comprises the following steps:
(1) weighing polyurethane resin, polymethyl methacrylate, FEVE fluorocarbon resin, PEVE emulsion, a coupling agent, a curing agent, a mixed filler, a carbon nano tube, an auxiliary agent, high-molecular fibers, calcium chloride, propylene glycol and ethylene glycol butyl ether materials;
(2) slowly adding polyurethane resin, polymethyl methacrylate and FEVE fluorocarbon resin into a reaction kettle which is dispersed at a high speed and has friction heat generation at the temperature of 35-70 ℃, stirring for 1-5h to obtain a mixture A, wherein the solid content ratio of the polyurethane resin, the polymethyl methacrylate and the FEVE fluorocarbon resin in the FEVE thermosetting layered fluorocarbon powder coating is (15-40): (15-30): (10-25);
(3) adding the polymer fiber into a formic acid solution with the amount of 2-3 times that of the polymer fiber, heating to 65-90 ℃, dropwise adding a proper amount of hydrogen peroxide while stirring, stirring for 5-8h after dropwise adding, then adding ammonia water, cooling, then adding ethyl acetate, standing for layering, taking a lower layer, then washing with water to be neutral, and distilling under reduced pressure to obtain the modified polymer fiber; sequentially adding modified polymer fibers and calcium chloride into a reaction kettle to be subjected to ultrasonic dispersion mixing with the mixture A, then sequentially adding a coupling agent and PEVE emulsion and stirring, simultaneously sequentially adding a curing agent and carbon nanotubes at a constant speed of 45-60g/min, stopping stirring after the addition is finished, standing, continuing stirring for 15-20min, and grinding and dispersing until the fineness is less than or equal to 25 micrometers to obtain a mixture B;
(4) mixing the mixed filler, ultrasonically dispersing for 1-3h by using a high-speed dispersion machine, adding a dispersing agent, grinding and dispersing until the fineness is less than or equal to 10 mu m to obtain the dispersed mixed filler, and then sequentially adding propylene glycol and ethylene glycol butyl ether to obtain a mixture C;
(5) mixing the mixture B with the mixture C, dispersing for 15-30min by using a high-speed dispersion machine, and adding the auxiliary agent for spheroidizing and loosening treatment;
(6) adding the mixture subjected to spheroidization and loosening treatment into a double-screw extruder for melting and mixing, wherein the temperature of a zone 1 is 50-70 ℃, the temperature of a zone 2 is 70-95 ℃, the temperature of a zone 3 is 95-110 ℃, the temperature of a zone 4 is 100-; and crushing, grinding and screening the sheet-shaped objects by a fine crusher to obtain the required powder coating.
2. A FEVE thermosetting layered fluorocarbon powder coating according to claim 1, characterized by comprising the following ingredients in parts by weight: 10-45 parts of polyurethane resin, 20-35 parts of polymethyl methacrylate, 1-5 parts of a curing agent, 8-25 parts of a mixed filler, 10-30 parts of FEVE fluorocarbon resin, 1-15 parts of PEVE emulsion, 4-8 parts of a coupling agent, 1-8 parts of a carbon nano tube, 1-5 parts of high polymer fiber, 0.6-1.6 parts of calcium chloride, 1-3 parts of propylene glycol and 1-2 parts of ethylene glycol butyl ether; and the carbon nano tube is a carboxylated carbon nano tube.
3. The FEVE thermosetting layered fluorocarbon powder coating as claimed in claim 2, wherein the carboxylated carbon nanotubes are prepared by dispersing carbon nanotubes in 3 times of hydrochloric acid solution, ultrasonically dispersing for 3-5h, adding distilled water, performing vacuum filtration for many times, detecting pH to be equal to 7, drying the solid obtained after the vacuum filtration, repeatedly grinding, dispersing the ground powder in mixed acid, ultrasonically dispersing for 5-8h, adding distilled water again, repeatedly performing vacuum filtration to make pH within 6-7, drying in a drying oven at 95-100 ℃ for 10-15 h.
4. A FEVE thermosetting layered fluorocarbon powder coating as claimed in claim 1, wherein said curing agent is any one or combination of two or more of ethylenediamine, diethylenetriamine, triethylenetetramine, xylylenediamine, m-phenylenediamine, diaminodiphenylmethane, diaminodiphenylsulfone, β -hydroxyethylethylenediamine.
5. A FEVE thermosetting layered fluorocarbon powder coating as claimed in claim 1, characterized in that the mixed filler is any one or combination of more than two of titanium dioxide, chrome yellow, calcium carbonate, calcined kaolin, talc and barium sulfate.
6. The FEVE thermosetting layered fluorocarbon powder coating of claim 1, wherein the additives include adhesion promoter and nano modifier, being solid organosilicon phosphorus type additives.
7. The FEVE thermosetting layered fluorocarbon powder coating of claim 1, wherein the coupling agent is an aluminum zirconium coupling agent and a silane coupling agent mixed in a ratio of 1-5: 1-9.
8. An FEVE thermosetting layered fluorocarbon powder coating as claimed in claim 1, wherein the reaction kettle comprises a kettle body, an ultrasonic generating device, a stirring device and a grinding device, the stirring device and the grinding device are fixedly arranged in the kettle body, the ultrasonic generating device is composed of ultrasonic pulse units arranged at intervals along the outer side wall of the kettle body, the ultrasonic pulse units are arranged into 10-30 groups from top to bottom, each group is 10-50 and is circumferentially distributed around the kettle body, and each ultrasonic pulse unit comprises an ultrasonic generator and a transducer which are electrically connected; the stirring device is transversely arranged; the grinding device is arranged above the stirring device and comprises two groups of grinding rollers and material guide plates which are symmetrically arranged, the material guide plates are obliquely arranged below the two groups of grinding rollers, and a channel is arranged between the material guide plates below the two groups of grinding rollers; the grinding roller is also evenly provided with a plurality of groups of convex teeth.
9. A FEVE thermosetting layered fluorocarbon powder coating according to claim 1 wherein the temperature of said spheroidizing loosening treatment does not exceed 15 ℃.
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