CN114032011B - High-brightness electroplating effect imitating powder coating and preparation method thereof - Google Patents
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D167/00—Coating compositions based on polyesters obtained by reactions forming a carboxylic ester link in the main chain; Coating compositions based on derivatives of such polymers
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- C08F230/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and containing phosphorus, selenium, tellurium or a metal
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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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- 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 relates to a high-brightness electroplating effect imitating powder coating and a preparation method thereof, belonging to the technical field of powder coatings, wherein the preparation method comprises the following steps: firstly, weighing raw materials in parts by weight; adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet press, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m; and secondly, binding the base powder by adopting a binding process, and sieving the base powder by a 100-mesh sieve after the binding is finished to obtain the high-brightness electroplating-effect-imitating powder coating. The filler is added into the raw materials, the filler is pretreated diatomite obtained by treating diatomite with a silane coupling agent, the pretreated diatomite and the flame-retardant component are obtained by treating through a chemical grafting method, the flame-retardant component can be uniformly distributed in the diatomite, and the stability of the flame-retardant component is improved through the powder coating obtained by melt extrusion.
Description
Technical Field
The invention belongs to the technical field of powder coatings, and particularly relates to a high-brightness electroplating-effect-imitating powder coating and a preparation method thereof.
Background
The powder coating does not contain an organic solvent, and compared with the conventional coating, the powder coating has the advantages of no pollution, energy and resource saving, high mechanical strength of a coating film, complete recovery of excessive coating and the like, and is increasingly and widely applied to coating of shells of household appliances, automobile エ industry, office appliances, metal materials, outdoor buildings and the like, however, the conventional powder coating basically does not have flame retardant property, and polyester resin and epoxy resin are main components of the powder coating, when the substrate is wood, the powder coating is easy to burn, and has great potential safety hazard.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a high-brightness powder coating with an imitation electroplating effect and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
a high-brightness powder coating with an electroplating-imitated effect comprises the following raw materials in parts by weight: 92-100 parts of polyester resin, 5-6 parts of curing agent, 2-6 parts of filler, 1.2-1.5 parts of flatting agent, 1-1.1 parts of wetting accelerator, 0.3-0.4 part of benzoin, 0.4-1.2 parts of aluminum powder directional arrangement agent and 1-1.2 parts of aluminum powder;
the filler is prepared by the following steps:
mixing the pretreated diatomite, span-80 and the flame-retardant component, adding azobisisobutyronitrile, stirring and reacting for 6 hours at the temperature of 65 ℃ under the protection of nitrogen, and after the reaction is finished, performing suction filtration and drying to obtain a filler; wherein the mass ratio of the pretreated diatomite, span-80, the flame-retardant component and the azobisisobutyronitrile is 2: 0.5: 1: 1.
the preparation method comprises the steps of treating diatomite with a silane coupling agent to obtain pretreated diatomite, treating the pretreated diatomite and a flame-retardant component by a chemical grafting method to obtain a filler, wherein the flame-retardant component can be uniformly distributed in the diatomite, and the stability of the flame-retardant component is improved by a powder coating obtained through melt extrusion.
Further, the flame retardant component is prepared by the steps of:
step S11, mixing hydroxyacetone, p-hydroxybenzaldehyde and ethanol at the temperature of 20 ℃, adding a hydrochloric acid solution, stirring for reaction for 12 hours, and then heating and refluxing for 2 hours to obtain a hydroxyl compound;
step S12, mixing a hydroxyl compound, pyridine and tetrahydrofuran at the temperature of 0 ℃, adding dichlorodimethylsilane under the protection of nitrogen, heating to 20 ℃ after adding, and stirring for reacting for 12 hours to obtain an intermediate 1; the structure of intermediate 1 is shown below:
step S13, mixing the intermediate 1, triethylamine and tetrahydrofuran at the temperature of 0 ℃, then adding acryloyl chloride, heating to 40 ℃ after the addition, and stirring for reacting for 5 hours to obtain a component A;
step S14, mixing 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate and tetrahydrofuran at the temperature of 0 ℃, keeping the temperature unchanged, and stirring for reaction for 12 hours to obtain a component B; mixing the component A and the component B according to the mass ratio of 1: 5, mixing to obtain the flame-retardant component. The flame-retardant component is formed by compounding a component A and a component B, wherein the component A contains siloxane bonds, the high-temperature resistance is improved, meanwhile, the introduction of the siloxane bonds can improve the hydrophobic property, the siloxane bonds are grafted on the pretreated diatomite, the specific component A is a silicon-containing monomer, the component B is a phosphorus-containing monomer, and the prepared polymer chain uniformly contains oxysilane bonds and phosphate groups, so that the flame-retardant effect is achieved.
Further, the mass fraction of the hydrochloric acid solution in step S11 is 37%, and the usage ratio of the hydroxyacetone, the p-hydroxybenzaldehyde, the ethanol and the hydrochloric acid solution is 0.07 mol: 0.07 mol: 300 mL: 2 mL;
in step S12, the ratio of the amount of the hydroxy compound, dichlorodimethylsilane, pyridine and tetrahydrofuran was 3 g: 1 g: 1.6 g: 4 mL;
in the step S13, the dosage ratio of the intermediate 1, acryloyl chloride, triethylamine and tetrahydrofuran is 2 g: 1 g: 0.5 mL: 20 mL;
in step S14, the use amount ratio of 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate to tetrahydrofuran was 2.3 g: 2 g: 2.1 g: 10 mL.
Further, the pretreated diatomaceous earth is prepared by the steps of:
dispersing the diatomite and the mixed solvent, adding gamma-aminopropyltriethoxysilane, stirring at 60 ℃ for 5 hours, filtering, placing in an oven at 80 ℃ and drying to constant weight to obtain the pretreated diatomite.
Further, the volume ratio of the ethanol to the water in the mixed solvent is 9: 1, the dosage ratio of the diatomite, the gamma-aminopropyl triethoxysilane and the mixed solvent is 10 g: 100mL of: 0.3 g.
Further, the polyester resin is a carboxyl-terminated saturated polyester resin and a hydroxyl-terminated saturated polyester resin in a mass ratio of 10: 1, the curing agent is a closed isocyanate curing agent, wherein the content of-NCO is 14-15%.
A preparation method of a high-brightness electroplating effect imitating powder coating comprises the following steps:
firstly, weighing the following raw materials in parts by weight: 92-100 parts of polyester resin, 5-6 parts of curing agent, 2-6 parts of filler, 1.2-1.5 parts of flatting agent, 1-1.1 parts of wetting accelerator, 0.3-0.4 part of benzoin, 0.4-1.2 parts of aluminum powder directional arrangement agent and 1-1.2 parts of aluminum powder;
adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet machine, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m;
and secondly, binding the base powder by adopting a binding process and sieving the base powder by a 100-mesh sieve to obtain the high-brightness electroplating effect imitating powder coating.
Further, the leveling agent is selected from a leveling agent KC758, the wetting accelerator is selected from a wetting accelerator BLC701B, and the aluminum powder aligning agent is selected from an aluminum powder aligning agent SP-1004.
The invention has the beneficial effects that:
the filler is added into the high-brightness electroplating-imitated powder coating, the filler is obtained by treating diatomite with a silane coupling agent to obtain pretreated diatomite, the pretreated diatomite and a flame-retardant component are treated by a chemical grafting method to obtain the filler, the flame-retardant component is formed by compounding a component A and a component B, wherein the component A contains siloxane bonds, the high-temperature resistance is improved, meanwhile, the introduction of the siloxane bonds can improve the hydrophobic property, the siloxane bonds are grafted on the pretreated diatomite, the specific component A is a silicon-containing monomer, the component B is a phosphorus-containing monomer, and a prepared polymer chain uniformly contains oxysilane bonds and phosphate groups, so that the flame-retardant effect is achieved. The flame-retardant component can be uniformly distributed in the diatomite, and the stability of the flame-retardant component is improved by the powder coating obtained by melt extrusion. The addition of the flame retardant component can prevent further degradation of the underlying polymeric material and inhibit the release of toxic gases.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing a flame-retardant component:
step S11, mixing hydroxyacetone, p-hydroxybenzaldehyde and ethanol at the temperature of 20 ℃, adding a hydrochloric acid solution, stirring for reaction for 12 hours, and then heating and refluxing for 2 hours to obtain a hydroxyl compound; wherein the mass fraction of the hydrochloric acid solution is 37 percent, the dosage ratio of the hydroxyacetone, the p-hydroxybenzaldehyde, the ethanol and the hydrochloric acid solution is controlled to be 0.07 mol: 0.07 mol: 300 mL: 2 mL;
step S12, mixing a hydroxyl compound, pyridine and tetrahydrofuran at the temperature of 0 ℃, adding dichlorodimethylsilane under the protection of nitrogen, heating to 20 ℃ after adding, and stirring for reacting for 12 hours to obtain an intermediate 1; controlling the dosage ratio of the hydroxyl compound, dichlorodimethylsilane, pyridine and tetrahydrofuran to be 3 g: 1 g: 1.6 g: 4 mL;
step S13, mixing the intermediate 1, triethylamine and tetrahydrofuran at the temperature of 0 ℃, then adding acryloyl chloride, heating to 40 ℃ after the addition, and stirring for reacting for 5 hours to obtain a component A; controlling the dosage ratio of the intermediate 1, acryloyl chloride, triethylamine and tetrahydrofuran to be 2 g: 1 g: 0.5 mL: 20 mL;
step S14, mixing 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate and tetrahydrofuran at the temperature of 0 ℃, keeping the temperature unchanged, and stirring for reaction for 12 hours to obtain a component B; mixing the component A and the component B according to the mass ratio of 1: 5, mixing to obtain a flame-retardant component; controlling the dosage ratio of 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate and tetrahydrofuran to be 2.3 g: 2 g: 2.1 g: 10 mL.
Example 2
Preparing a filler:
dispersing diatomite and a mixed solvent, adding gamma-aminopropyltriethoxysilane, stirring for 5 hours at 60 ℃, filtering, placing in an oven at 80 ℃ and drying to constant weight to obtain pretreated diatomite; wherein the volume ratio of the ethanol to the water in the mixed solvent is 9: 1, the dosage ratio of the diatomite, the gamma-aminopropyl triethoxysilane and the mixed solvent is 10 g: 100mL of: 0.3 g;
mixing the pretreated diatomite, span-80 and the flame-retardant component prepared in the example 1, adding azobisisobutyronitrile, stirring and reacting for 6 hours at the temperature of 65 ℃ under the protection of nitrogen, and after the reaction is finished, performing suction filtration and drying to obtain the filler. Wherein the mass ratio of the pretreated diatomite, span-80, the flame-retardant component and the azodiisobutyronitrile is 2: 0.5: 1: 1.
example 3
Preparing a high-brightness electroplating effect imitating powder coating:
firstly, weighing the following raw materials in parts by weight: 92 parts of polyester resin, 5 parts of curing agent, 2 parts of filler prepared in example 2, 1.2 parts of leveling agent, 1 part of wetting accelerator, 0.3 part of benzoin, 0.4 part of aluminum powder aligning agent and 1 part of aluminum powder; adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet press, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m; wherein, the leveling agent is selected from a leveling agent KC758, the wetting accelerant is selected from a wetting accelerant BLC701B, and the aluminum powder aligning agent is selected from an aluminum powder aligning agent SP-1004. The polyester resin is a carboxyl-terminated saturated polyester resin and a hydroxyl-terminated saturated polyester resin according to a mass ratio of 10: 1, and the curing agent is a closed isocyanate curing agent.
Secondly, bonding the base powder by adopting a bonding process, adding the base powder into a bonding machine, slowly stirring, stirring at 1000rmp, heating to 45 ℃, then stirring at 900rmp, heating to 50 ℃, and then stirring at 800rmp, heating to 54 ℃; continuing stirring at 700rmp and heating to 57 ℃; then stirring and heating to 60 ℃ by 650 rmp; and finally, stirring at 600rmp, heating to 61 ℃ of a preset bonding temperature, regulating the rotating speed to 400rmp after the preset bonding temperature is reached, opening a valve to feed the metal powder pigment into a bonding pot for bonding for 80s, stirring at 350rmp, cooling to below 40 ℃, and sieving with a 100-mesh sieve to obtain the high-brightness powder coating with the electroplating-imitating effect.
Example 4
Preparing a high-brightness electroplating effect imitating powder coating:
firstly, weighing the following raw materials in parts by weight: 96 parts of polyester resin, 5 parts of curing agent, 4 parts of filler prepared in example 2, 1.3 parts of flatting agent, 1 part of wetting accelerator, 0.3 part of benzoin, 0.8 part of aluminum powder aligning agent and 1.1 part of aluminum powder; adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet machine, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m; wherein, the leveling agent is selected from a leveling agent KC758, the wetting accelerant is selected from a wetting accelerant BLC701B, and the aluminum powder aligning agent is selected from an aluminum powder aligning agent SP-1004. The polyester resin is a carboxyl-terminated saturated polyester resin and a hydroxyl-terminated saturated polyester resin according to a mass ratio of 10: 1, and the curing agent is a closed isocyanate curing agent.
And secondly, binding the base powder by adopting a binding process, wherein the specific process is as shown in example 3, and sieving the base powder by a 100-mesh sieve to obtain the high-brightness electroplating-simulated powder coating.
Example 5
Preparing a high-brightness electroplating effect imitating powder coating:
firstly, weighing the following raw materials in parts by weight: 100 parts of polyester resin, 6 parts of curing agent, 6 parts of filler prepared in example 2, 1.5 parts of leveling agent, 1.1 parts of wetting accelerator, 0.4 part of benzoin, 1.2 parts of aluminum powder aligning agent and 1.2 parts of aluminum powder; adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet machine, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m; wherein, the leveling agent is selected from a leveling agent KC758, the wetting accelerant is selected from a wetting accelerant BLC701B, and the aluminum powder aligning agent is selected from an aluminum powder aligning agent SP-1004. The polyester resin is a carboxyl-terminated saturated polyester resin and a hydroxyl-terminated saturated polyester resin according to a mass ratio of 10: 1, and the curing agent is a closed isocyanate curing agent.
And secondly, binding the base powder by adopting a binding process, wherein the specific process is as shown in example 3, and sieving the base powder by a 100-mesh sieve to obtain the high-brightness electroplating-simulated powder coating.
Comparative example 1
The filler in example 4 was replaced by diatomaceous earth, and the remaining raw materials and preparation process were kept unchanged.
The samples from examples 3-5 and all of comparative example 1 were tested and the results are shown in table 1 below:
preparing a coating layer: the powder coatings of examples 3-5 and comparative example 1 were sprayed on the medium density fiberboard substrate after surface treatment by an electrostatic spray gun, and cured at 140 ℃/30min to obtain a coating, the index of which was measured according to: CB/T21776-2008 Standard guidelines for testing powder coatings and coatings thereof; the sample plate flame retardant property and the oxygen index obtained in the examples and the comparative examples of the application are detected according to the following steps: GB8624-2012 grading the combustion performance of building materials and products.
TABLE 1
| Flame-retardant effect | Example 3 | Example 4 | Example 5 | Comparative example 1 |
| Oxygen index (%) | 46 | 46 | 46 | 21 |
| Flame retardant rating | B1 | B1 | B1 | B3 |
As can be seen from the above Table 1, the powder coating sample prepared by the invention has good flame retardant effect, excellent flame retardant effect, no halogen and environmental friendliness.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (5)
1. The high-brightness powder coating with the electroplating-imitated effect is characterized by comprising the following raw materials in parts by weight: 92-100 parts of polyester resin, 5-6 parts of curing agent, 2-6 parts of filler, 1.2-1.5 parts of flatting agent, 1-1.1 parts of wetting accelerator, 0.3-0.4 part of benzoin, 0.4-1.2 parts of aluminum powder directional arrangement agent and 1-1.2 parts of aluminum powder; the filler is prepared by the following steps:
mixing the pretreated diatomite, span-80 and the flame-retardant component, adding azobisisobutyronitrile, stirring and reacting for 6 hours at the temperature of 65 ℃ under the protection of nitrogen, and after the reaction is finished, performing suction filtration and drying to obtain a filler;
the flame retardant component is prepared by the following steps:
step S11, mixing hydroxyacetone, p-hydroxybenzaldehyde and ethanol at the temperature of 20 ℃, adding a hydrochloric acid solution, stirring for reaction for 12 hours, and then heating and refluxing for 2 hours to obtain a hydroxyl compound;
step S12, mixing a hydroxyl compound, pyridine and tetrahydrofuran at the temperature of 0 ℃, adding dichlorodimethylsilane under the protection of nitrogen, heating to 20 ℃ after adding, and stirring for reacting for 12 hours to obtain an intermediate 1;
step S13, mixing the intermediate 1, triethylamine and tetrahydrofuran at the temperature of 0 ℃, then adding acryloyl chloride, heating to 40 ℃ after the addition, and stirring for reacting for 5 hours to obtain a component A;
step S14, mixing 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate and tetrahydrofuran at the temperature of 0 ℃, keeping the temperature unchanged, and stirring for reaction for 12 hours to obtain a component B; mixing the component A and the component B according to the mass ratio of 1: 5, mixing to obtain a flame-retardant component;
the pretreated diatomite is prepared by the following steps:
dispersing the diatomite and the mixed solvent, adding gamma-aminopropyltriethoxysilane, stirring at 60 ℃ for 5 hours, filtering, placing in an oven at 80 ℃ and drying to constant weight to obtain the pretreated diatomite.
2. The high-brightness imitation electroplating powder coating as claimed in claim 1, wherein the mass fraction of the hydrochloric acid solution in step S11 is 37%, and the usage ratio of the hydroxyacetone, the p-hydroxybenzaldehyde, the ethanol and the hydrochloric acid solution is 0.07 mol: 0.07 mol: 300 mL: 2 mL; in step S12, the ratio of the amount of the hydroxy compound, dichlorodimethylsilane, pyridine and tetrahydrofuran was 3 g: 1 g: 1.6 g: 4 mL; in the step S13, the dosage ratio of the intermediate 1, acryloyl chloride, triethylamine and tetrahydrofuran is 2 g: 1 g: 0.5 mL: 20 mL; in the step S14, the use amount ratio of 2-hydroxyethyl acrylate, triethylamine, phenyl dichlorophosphate and tetrahydrofuran was 2.3 g: 2 g: 2.1 g: 10 mL.
3. The high-brightness electroplating-like powder coating as claimed in claim 1, wherein the volume ratio of ethanol to water in the mixed solvent is 9: 1, the dosage ratio of the diatomite, the gamma-aminopropyl triethoxysilane and the mixed solvent is 10 g: 100mL of: 0.3 g.
4. The high-brightness electroplating-effect-simulating powder coating as claimed in claim 1, wherein the polyester resin is a carboxyl-terminated saturated polyester resin and a hydroxyl-terminated saturated polyester resin in a mass ratio of 10: 1, and the curing agent is a closed isocyanate curing agent.
5. The method for preparing the powder coating with the high-brightness imitation electroplating effect according to claim 1, which is characterized by comprising the following steps:
firstly, weighing raw materials in parts by weight; adding the weighed raw materials into a high-speed mixer, premixing for 4min, performing melt extrusion through a double-screw extruder, cooling by a tablet machine, performing coarse crushing, then performing air classification grinding, and screening to obtain base powder with the particle size of 30-40 mu m;
and secondly, binding the base powder by adopting a binding process, and sieving the base powder by a 100-mesh sieve after the binding is finished to obtain the high-brightness electroplating-effect-imitating powder coating.
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| CN111876098B (en) * | 2020-07-02 | 2021-10-22 | 广东泰强化工实业有限公司 | Amphiphilic ionomer-reinforced healthy environment-friendly hot melt adhesive and preparation and application thereof |
| CN111662620A (en) * | 2020-07-06 | 2020-09-15 | 阜南县民安人防工程设备有限公司 | Preparation method of powder coating for fireproof door |
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| CN104231849A (en) * | 2014-08-22 | 2014-12-24 | 安徽博大纤维素科技有限公司 | Flame-retardant power coating |
| CN107936786A (en) * | 2017-12-20 | 2018-04-20 | 青岛豪元晟五金塑胶有限公司 | Bonding Pearlescent powder paint and its preparation process |
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