CN115975471B - Double-coating powder coating and preparation method thereof - Google Patents
Double-coating powder coating and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a double-coating powder coating and a preparation method thereof; the powder coating is formed by combining an inner layer and a surface layer, wherein the surface layer is arranged on the surface of a base material, and the inner layer is covered on the surface of the surface layer; according to the double-coating powder coating prepared by the invention, the service life of the coating can be remarkably prolonged by adopting the double-coating, the surface layer and the base material can be better tightly combined by the characteristic that the inner layer has higher adhesive force, and the inner layer has relatively poorer corrosion resistance, so that the inner layer can be prevented from directly contacting with external corrosion factors by the covering of the surface layer, and the double-coating can be better applied to various environments by the higher corrosion resistance of the surface layer.
Description
Technical Field
The invention belongs to the technical field of powder coating production, and in particular relates to a double-coating powder coating and a preparation method thereof.
Background
Since the seventies of the last century, powder coatings have been widely used because they contain no organic solvent and 100% are solid components, and they have the advantages of no pollution, energy and resource saving, high mechanical strength of coating film, and complete recovery of excessive coating materials, compared with most of the existing solvent-based coatings.
The prior art has the application number of: 2019110148084 the invention relates to the field of powder coatings, and in particular discloses a high-silver-flash corrosion-resistant powder coating, which comprises the following raw materials in parts by mass: 24-35 parts of epoxy resin KD-203L; 36-50 parts of polyester resin SJ 6805; 1.6-9.3 parts of inorganic pigment; 11-33 parts of a secondary film forming filler; 2-5 parts of an auxiliary agent; 3-7 parts of aluminum powder. The invention selects the epoxy resin KD-203L with hydroxyl to make the powder coating have good corrosion resistance, selects the polyester resin SJ6805 with carboxyl to make the powder coating have good leveling property, adds high amount of aluminum powder to make the powder coating have good silver flashing effect ", and has good corrosion resistance, but because the powder coating is a single-layer coating, after long-time use, more abrasion is easy to occur, and after abrasion exposes the base material, the deterioration of the coating is accelerated, so that the service life of the powder coating is greatly reduced.
Accordingly, there is a need for further improvements in the art.
Disclosure of Invention
The invention aims to provide a double-coating powder coating and a preparation method thereof, which are used for solving the defects in the prior art.
The technical scheme adopted by the invention is as follows:
a double-coating powder coating is formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: 65-70 parts of epoxy resin KD2012H, 1-3 parts of ethyl triphenylphosphine bromide, 2-2.8 parts of stearic acid, 2-4 parts of silicon micropowder, 1-2 parts of graphene and 6-7 parts of curing agent;
the surface layer is prepared from the following components in parts by weight: 50-65 parts of polyester resin, 1-4 parts of pigment, 12-20 parts of calcium carbonate, 10-18 parts of graft polymer and 1-1.5 parts of inorganic antibacterial agent.
As a further technical scheme: the mixing weight ratio of the silicon micro powder to the graphene is 2:1.
As a further technical scheme: the mass fraction of silicon dioxide in the silicon micropowder is 97-98%.
As a further technical scheme: the graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring at a rotating speed of 100r/min for 10min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat, stirring for 40min, standing for 1 hour, performing suction filtration, washing to be neutral by adopting clear water, and drying at 60 ℃ for 30min.
As a further technical scheme: the mass fraction of the nitric acid solution is 8-10%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:12-15.
As a further technical scheme: the curing agent is diethylenetriamine.
As a further technical scheme: the preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 112-115 ℃, preserving heat, and stirring for 30min at a rotating speed of 100r/min to obtain a mixed solution;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2-2.5, introducing nitrogen, discharging air in the reaction kettle, stirring for 2 hours at the rotating speed of 150r/min, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
As a further technical scheme: the mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene in the step (1) is 3:18:40;
in the step (2), the mixing mass ratio of maleic anhydride, an initiator and dimethylbenzene is 5:1:30;
the initiator is dicumyl peroxide.
As a further technical scheme: the inorganic antibacterial agent is nano titanium dioxide.
A preparation method of the double-coating powder coating comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the main machine rotating speed of the double-screw extruder is 150r/min.
According to the invention, the inner layer and the surface layer are respectively prepared, and are combined to form the double-layer coating, so that the service life of the coating is greatly prolonged, and when the surface layer is worn greatly, the substrate can be continuously protected through the inner layer, and the protection time of the substrate is prolonged.
In the surface layer powder coating, the graft polymer is introduced and can be combined with polyester resin molecules in a powder coating system to form a stable network structure, so that the stability, particularly the corrosion resistance, of the formed coating is greatly improved, and the stability of chemical bonds is improved through the combination of the graft polymer and the polyester resin molecules, so that the erosion effect of chemicals on the coating can be better avoided, and the prepared coating can be applied to the chemical field.
By introducing a certain amount of inorganic antibacterial agent nano titanium dioxide into the surface layer powder coating, the antibacterial performance of the surface layer can be greatly improved by introducing the nano titanium dioxide, and the antibacterial rate of the surface layer powder coating on escherichia coli, staphylococcus aureus and the like is over 99 percent.
The epoxy resin is adopted as the matrix resin in the inner layer, so that the bearing effect of the inner layer on the surface layer can be remarkably improved, and meanwhile, the epoxy resin can react with the base material to form a chemical bond, so that the adhesive force of the epoxy resin is greatly improved.
Advantageous effects
According to the double-coating powder coating prepared by the invention, the service life of the coating can be remarkably prolonged by adopting the double-coating, the surface layer and the base material can be better tightly combined by the characteristic that the inner layer has higher adhesive force, and the inner layer has relatively poorer corrosion resistance, so that the inner layer can be prevented from directly contacting with external corrosion factors by the covering of the surface layer, and the double-coating can be better applied to various environments by the higher corrosion resistance of the surface layer.
Drawings
FIG. 1 is a bar graph of flexural strength for examples and comparative examples.
Detailed Description
The following description of embodiments of the present invention will be made clearly and fully with reference to the accompanying drawings, in which it is shown, however, only some, but not all embodiments of the invention are shown. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
A double-coating powder coating is formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: epoxy resin KD2012H 65 parts, ethyl triphenylphosphine bromide 1 part, stearic acid 2 parts, silicon micropowder 2 parts, graphene 1 part and curing agent 6 parts;
the surface layer is prepared from the following components in parts by weight: 50 parts of polyester resin, 1 part of pigment, 12 parts of calcium carbonate, 10 parts of graft polymer and 1 part of inorganic antibacterial agent.
The mixing weight ratio of the silicon micro powder to the graphene is 2:1.
The mass fraction of silicon dioxide in the silicon micropowder is 97%.
The graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring at a rotating speed of 100r/min for 10min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat, stirring for 40min, standing for 1 hour, performing suction filtration, washing to be neutral by adopting clear water, and drying at 60 ℃ for 30min.
The mass fraction of the nitric acid solution is 8%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:12.
The curing agent is diethylenetriamine.
The preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 112 ℃, preserving heat, and stirring for 30min at a rotating speed of 100r/min to obtain a mixed solution;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2, introducing nitrogen, discharging air in the reaction kettle, stirring for 2 hours at the rotating speed of 150r/min, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
The mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene in the step (1) is 3:18:40;
in the step (2), the mixing mass ratio of maleic anhydride, an initiator and dimethylbenzene is 5:1:30;
the initiator is dicumyl peroxide.
The inorganic antibacterial agent is nano titanium dioxide.
A preparation method of the double-coating powder coating comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the main machine rotating speed of the double-screw extruder is 150r/min.
Example 2
A double-coating powder coating is formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: epoxy resin KD2012H 66 parts, ethyl triphenylphosphine bromide 2 parts, stearic acid 2.1 parts, silicon micropowder 3 parts, graphene 1.5 parts and curing agent 6.2 parts;
the surface layer is prepared from the following components in parts by weight: 52 parts of polyester resin, 2 parts of pigment, 13 parts of calcium carbonate, 12 parts of graft polymer and 1.2 parts of inorganic antibacterial agent.
The mixing weight ratio of the silicon micro powder to the graphene is 2:1.
The mass fraction of silicon dioxide in the silicon micropowder is 97.5%.
The graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring at a rotating speed of 100r/min for 10min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat, stirring for 40min, standing for 1 hour, performing suction filtration, washing to be neutral by adopting clear water, and drying at 60 ℃ for 30min.
The mass fraction of the nitric acid solution is 8.2%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:13.
The curing agent is diethylenetriamine.
The preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 113 ℃, preserving heat, and stirring for 30min at a rotating speed of 100r/min to obtain a mixed solution;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2.1, introducing nitrogen, discharging air in the reaction kettle, stirring for 2 hours at the rotating speed of 150r/min, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
The mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene in the step (1) is 3:18:40;
in the step (2), the mixing mass ratio of maleic anhydride, an initiator and dimethylbenzene is 5:1:30;
the initiator is dicumyl peroxide.
The inorganic antibacterial agent is nano titanium dioxide.
A preparation method of the double-coating powder coating comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the main machine rotating speed of the double-screw extruder is 150r/min.
Example 3
A double-coating powder coating is formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: epoxy resin KD2012H 68 parts, ethyl triphenylphosphine bromide 2 parts, stearic acid 2.5 parts, silicon micropowder 3 parts, graphene 1.5 parts and curing agent 6.4 parts;
the surface layer is prepared from the following components in parts by weight: 58 parts of polyester resin, 3 parts of pigment, 18 parts of calcium carbonate, 15 parts of graft polymer and 1.2 parts of inorganic antibacterial agent.
The mixing weight ratio of the silicon micro powder to the graphene is 2:1.
The mass fraction of silicon dioxide in the silicon micropowder is 97.8%.
The graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring at a rotating speed of 100r/min for 10min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat, stirring for 40min, standing for 1 hour, performing suction filtration, washing to be neutral by adopting clear water, and drying at 60 ℃ for 30min.
The mass fraction of the nitric acid solution is 9%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:14.
The curing agent is diethylenetriamine.
The preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 113 ℃, preserving heat, and stirring for 30min at a rotating speed of 100r/min to obtain a mixed solution;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2.4, introducing nitrogen, discharging air in the reaction kettle, stirring for 2 hours at the rotating speed of 150r/min, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
The mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene in the step (1) is 3:18:40;
in the step (2), the mixing mass ratio of maleic anhydride, an initiator and dimethylbenzene is 5:1:30;
the initiator is dicumyl peroxide.
The inorganic antibacterial agent is nano titanium dioxide.
A preparation method of the double-coating powder coating comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the main machine rotating speed of the double-screw extruder is 150r/min.
Example 4
A double-coating powder coating is formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: epoxy resin KD2012H 70 parts, ethyl triphenylphosphine bromide 3 parts, stearic acid 2.8 parts, silicon micropowder 4 parts, graphene 2 parts and curing agent 7 parts;
the surface layer is prepared from the following components in parts by weight: 65 parts of polyester resin, 4 parts of pigment, 20 parts of calcium carbonate, 18 parts of graft polymer and 1.5 parts of inorganic antibacterial agent.
The mixing weight ratio of the silicon micro powder to the graphene is 2:1.
The mass fraction of silicon dioxide in the silicon micropowder is 98%.
The graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring at a rotating speed of 100r/min for 10min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat, stirring for 40min, standing for 1 hour, performing suction filtration, washing to be neutral by adopting clear water, and drying at 60 ℃ for 30min.
The mass fraction of the nitric acid solution is 10%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:15.
The curing agent is diethylenetriamine.
The preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 115 ℃, preserving heat, and stirring for 30min at a rotating speed of 100r/min to obtain a mixed solution;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2.5, introducing nitrogen, discharging air in the reaction kettle, stirring for 2 hours at the rotating speed of 150r/min, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
The mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene in the step (1) is 3:18:40;
in the step (2), the mixing mass ratio of maleic anhydride, an initiator and dimethylbenzene is 5:1:30;
the initiator is dicumyl peroxide.
The inorganic antibacterial agent is nano titanium dioxide.
A preparation method of the double-coating powder coating comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the main machine rotating speed of the double-screw extruder is 150r/min.
Comparative example 1: no graft polymer was added as distinguished from example 1.
Comparative example 2: the difference from example 1 is that the graft polymer is replaced by ethylene propylene diene monomer.
Test
The chemical corrosion resistance of the surface powder coatings of the examples and the comparative examples is tested; chemical corrosion resistance: according to GB/T18593-2001;
TABLE 1
| Resistance to chemical attack | |
| Example 1 | The coating has no foaming and no cracking |
| Example 2 | The coating has no foaming and no cracking |
| Example 3 | The coating has no foaming and no cracking |
| Example 4 | The coating has no foaming and no cracking |
| Comparative example 1 | Foaming and cracking of the coating |
| Comparative example 2 | Foaming and cracking of the coating |
As can be seen from Table 1, the surface coating prepared by the invention has excellent corrosion resistance after being cured, and particularly has obviously improved chemical corrosion resistance.
The following tests were carried out on the two-layer coating materials after the inner layer and the surface layer coating materials of the examples and the comparative examples were combined:
flexural strength: the test was performed according to GB/T6742-1986 assay;
TABLE 2
| Flexural Strength/mm | |
| Example 1 | 4.3 |
| Example 2 | 4.6 |
| Example 3 | 4.5 |
| Example 4 | 4.2 |
| Comparative example 1 | 3.1 |
| Comparative example 2 | 3.2 |
From table 2, it can be seen that the double-layer coating formed by the powder coating prepared by the invention has excellent mechanical properties, and the mechanical properties of the coating, especially the bending strength, can be effectively improved by introducing the graft polymer.
Performance tests were performed on the example and comparative powder coatings;
adhesion measurement: measured according to SY/T0315-2005 assay;
TABLE 3 Table 3
| Adhesion/grade | |
| Example 1 | 1 |
| Example 2 | 1 |
| Example 3 | 1 |
| Example 4 | 1 |
| Comparative example 1 | 3 |
As can be seen from Table 3, the powder coating prepared by the invention has excellent adhesion and can be more firmly combined with the surface of a substrate after being cured to form a double-layer coating.
Flexural strength bar graphs of examples and comparative examples are shown in fig. 1.
The foregoing description of the preferred embodiments of the invention should not be taken as limiting the scope of the invention, which is defined by the appended claims, but rather by the description of the preferred embodiments, all changes and modifications that come within the meaning and range of equivalency of the claims are intended to be embraced therein.
Claims (8)
1. The double-coating powder coating is characterized by being formed by combining an inner layer and a surface layer;
the inner layer is prepared from the following components in parts by weight: 65-70 parts of epoxy resin KD2012H, 1-3 parts of ethyl triphenylphosphine bromide, 2-2.8 parts of stearic acid, 2-4 parts of silicon micropowder, 1-2 parts of graphene and 6-7 parts of curing agent;
the surface layer is prepared from the following components in parts by weight: 50-65 parts of polyester resin, 1-4 parts of pigment, 12-20 parts of calcium carbonate, 10-18 parts of graft polymer and 1-1.5 parts of inorganic antibacterial agent;
the preparation method of the graft polymer comprises the following steps:
(1) Firstly, sequentially adding rosin glyceride, ethylene propylene diene monomer and dimethylbenzene into a reaction kettle, then adjusting the temperature in the reaction kettle to 112-115 ℃, preserving heat, and stirring at a rotating speed of 100r/min for 30min to obtain a mixed solution; the mixing mass ratio of the rosin glyceride to the ethylene propylene diene monomer to the dimethylbenzene is 3:18:40;
(2) Adding maleic anhydride and an initiator into dimethylbenzene, and uniformly stirring to obtain a dispersion liquid; the mixing mass ratio of maleic anhydride, initiator and dimethylbenzene is 5:1:30; the initiator is dicumyl peroxide;
(3) Dropwise adding the dispersion liquid prepared in the step (2) into the mixed liquid in the step (1) according to the mass ratio of 5:2-2.5, introducing nitrogen, discharging air in the reaction kettle, stirring at the rotating speed of 150r/min for 2 hours, naturally cooling, and standing for 1 hour to obtain a reaction liquid;
(4) Adding absolute ethyl alcohol into the reaction liquid obtained in the step (3), wherein the mixing mass ratio of the absolute ethyl alcohol to the reaction liquid is 1:1, stirring for 30min at the rotating speed of 500r/min, standing for 4 hours, and separating to obtain a reactant;
(5) And (3) cleaning and drying the reactant obtained in the step (4) to obtain the graft polymer.
2. A dual-coat powder coating as set forth in claim 1, wherein: the mixing weight ratio of the silicon micro powder to the graphene is 2:1.
3. A dual-coat powder coating as set forth in claim 2, wherein: the mass fraction of silicon dioxide in the silicon micropowder is 97-98%.
4. A dual-coat powder coating as set forth in claim 2, wherein: the graphene is subjected to oxidation treatment:
firstly, adding nitric acid into deionized water, and stirring for 10min at a rotating speed of 100r/min to obtain a nitric acid solution;
adding graphene into a nitric acid solution, regulating the temperature to 78 ℃, preserving heat and stirring for 40min, standing for 1 h, performing suction filtration, washing to neutrality by adopting clear water, and drying at the temperature of 60 ℃ for 30min.
5. A dual-coat powder coating as recited in claim 4, wherein: the mass fraction of the nitric acid solution is 8-10%;
the mixing mass ratio of the graphene and the nitric acid solution is 1:12-15.
6. A dual-coat powder coating as set forth in claim 1, wherein: the curing agent is diethylenetriamine.
7. A dual-coat powder coating as set forth in claim 1, wherein: the inorganic antibacterial agent is nano titanium dioxide.
8. A method of preparing a dual-coat powder coating according to any one of claims 1 or 7, characterized in that: the method comprises the following steps:
(1) Weighing epoxy resin KD2012H, ethyl triphenylphosphine bromide, stearyl, silicon micropowder, graphene and curing agent according to parts by weight, sequentially adding the components into a high-speed mixer for mixing, adding the components into a double-screw extruder for melt extrusion, then slicing, crushing, grinding and sieving to obtain inner-layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 120 ℃, the temperature of the second area is 125 ℃, the temperature of the third area is 125 ℃, the temperature of the fourth area is 120 ℃, the temperature of the fifth area is 120 ℃, and the temperature of the machine head is 122 ℃;
the rotating speed of the main machine of the double-screw extruder is 90r/min;
(2) Weighing polyester resin, pigment, calcium carbonate, graft polymer and inorganic antibacterial agent according to parts by weight, sequentially adding into a high-speed mixer for mixing, adding into a double-screw extruder for melt extrusion, slicing, crushing, grinding and sieving to obtain surface layer powder;
wherein, the temperature of each zone of the double-screw extruder is set as follows: the temperature of the first area is 145 ℃, the temperature of the second area is 145 ℃, the temperature of the third area is 150 ℃, the temperature of the fourth area is 155 ℃, the temperature of the fifth area is 150 ℃, and the temperature of the machine head is 145 ℃;
the rotating speed of the main machine of the double-screw extruder is 150r/min.
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