CN115895404A - Salt-fog-resistant powder coating and preparation method thereof - Google Patents
Salt-fog-resistant powder coating and preparation method thereof Download PDFInfo
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- CN115895404A CN115895404A CN202211455360.1A CN202211455360A CN115895404A CN 115895404 A CN115895404 A CN 115895404A CN 202211455360 A CN202211455360 A CN 202211455360A CN 115895404 A CN115895404 A CN 115895404A
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Abstract
The invention discloses a salt spray resistant powder coating and a preparation method thereof, wherein the salt spray resistant powder coating comprises the following raw materials in percentage by mass: 50-65% of graphene and carbon nanotube modified polyester resin, 10-30% of polyaniline modified layered filler, 4-7% of curing agent, 0.8-1.2% of flatting agent, 0.7-28% of pigment, 10-30% of inorganic filler and 0.5-2% of auxiliary agent; the salt spray resistant powder coating prevents water vapor, oxygen, salt and the like from permeating by utilizing the barrier property of graphene and polyaniline modified layered filler, and can form a compact conductive network on the surface of a matrix, so that free electrons generated by electrochemical reaction are transferred to the surface of the coating and are quenched by the external environment, the electrochemical reaction is obviously inhibited, and the salt spray resistance of the coating is improved.
Description
Technical Field
The invention belongs to the technical field of powder coatings, and particularly relates to a salt spray resistant powder coating and a preparation method thereof.
Background
The coating prepared from the powder coating can be corroded by acid rain, salt and the like in the application process and causes the failure of the coating, so the salt spray resistance is an important index parameter of the powder coating and is used for representing the relative strength of the anticorrosion (corrosion-resistant) capability of a material.
The corrosion principle of the coating is that the surface of a metal substrate such as iron and the like generates electrochemical reaction, in the reaction, metal loses electrons and is oxidized, the reaction process is called as a negative electrode reaction process, and the reaction product is metal ions entering a medium or metal oxide (or metal insoluble salt) covered on the surface of the metal; the material in the medium, such as oxygen, gets electrons from the metal surface and is reduced, and the reaction process is called as a positive electrode reaction process. In the prior art, polyester resin, acrylic resin, epoxy resin and the like are generally adopted to prepare an anticorrosive coating together with a filler to realize the anticorrosive performance of the coating, but the coating has certain anticorrosive performance, but the anticorrosive effect is not ideal.
Graphene has a layered barrier property, and is widely used in a zinc-rich anticorrosive paint for heavy corrosion protection at present, and the main principle is that the graphene-based layer transfer barrier property prevents water vapor and the like from permeating, and a conductive network formed between the graphene and zinc powder quenches free electrons generated by electrochemistry, so that the salt spray resistance is remarkably improved. Experiments show that when the graphene or the carbon nano tube is independently added into the powder coating, the graphene/the carbon nano tube is not uniformly distributed in the powder coating, so that a compact conductive network and a barrier network are not formed in the powder coating, and the improvement effect on the salt spray performance is not obvious.
Disclosure of Invention
In order to solve the technical problems, the invention discloses a salt spray resistant powder coating and a preparation method thereof, wherein the salt spray resistant powder coating is characterized in that a modified layered filler network obtained by mutually coordinating a graphene-formed layered transfer blocking system in a resin phase in the powder coating and a blocking system formed by a polyaniline modified layered filler in a conductive polymer filler phase is utilized to remarkably prevent water vapor, oxygen, salt and other materials from permeating; the conductive network formed by head-tail collision of uniformly distributed carbon nanotubes in the polyester resin and the filler conductive network formed by mutual intersection of polyaniline modified layered fillers in the filler phase form a compact synergistic conductive network in the powder coating body, so that free electrons generated by electrochemical reaction can be transferred to the surface of the coating through the synergistic conductive network in the powder coating and are quenched by the external environment, the electrochemical reaction is remarkably inhibited, and the salt spray resistance of the coating is improved by the synergy of the conductive network and the filler conductive network. .
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the salt spray resistant powder coating comprises the following raw materials in percentage by mass: 50-65% of graphene and carbon nano tube modified polyester resin, 10-30% of polyaniline modified layered filler, 4-7% of curing agent, 0.8-1.2% of flatting agent, 0.7-28% of pigment, 10-30% of inorganic filler and 0.5-2% of auxiliary agent.
The preparation method of the polyaniline modified layered filler comprises the following steps: uniformly mixing a layered filler, aniline and an inorganic acid aqueous solution, dropwise adding an ammonium persulfate solution under the stirring condition, carrying out in-situ polymerization reaction, filtering after the reaction is finished, and then washing until the layered filler is neutral, wherein the layered filler is one or a mixture of mica powder and nano montmorillonite; the inorganic acid is at least one of sulfuric acid, hydrochloric acid and nitric acid.
The concentration of H + in the inorganic acid aqueous solution is 0.1-2.0mol/L; the molar ratio of ammonium persulfate to aniline is 2-3:1; the mass ratio of the lamellar filler to the aniline is 1: 0.02-0.1.
The reaction temperature of the in-situ polymerization reaction is 15-35 ℃, and the reaction time is not less than half an hour.
The acid value of the graphene and carbon nanotube modified polyester resin is 25-55mgKOH/g resin, the number average molecular weight is 2500-5000g/mol, and the glass transition temperature (Tg) is more than or equal to 55 ℃.
The graphene and carbon nanotube modified polyester resin, the content of graphene is 0.3-5% wt, the content of carbon nanotubes is 0.2-0.9% wt.
The preparation method of the graphene and carbon nanotube modified polyester resin comprises the following steps: putting polyol, a branching agent, graphene dispersion liquid, carbon nano tube dispersion liquid, aromatic polyacid and an esterification catalyst into a reaction kettle at the same time, heating to 235-255 ℃ at the speed of 1-2 ℃/min in a nitrogen atmosphere, maintaining, adding an acidolysis agent when the system is clarified and the sampling detection Acid Value (AV) reaches 5-20mgKOH/g, and maintaining the temperature at 235-250 ℃ for acidolysis and end capping; when the acid value of the polyester is 35-68mgKOH/g, the temperature is reduced to 230-240 ℃ at the speed of 3-5 ℃/min, and the polyester is polycondensed under vacuum of-0.1 mPA, so that the acid value of the polyester reaches 25-55mgKOH/g; then emptying and cooling to 180-230 ℃, adding the curing accelerator according to the formula amount, and discharging after keeping for 5-30 min.
In the preparation method of the graphene and carbon nanotube modified polyester resin, the weight percentages of the raw materials are as follows: 8-44% by weight of polyols; 44-65% by weight of an aromatic polyacid; 0.0-2% by weight of branching agent; 2.3-30% of graphene dispersion liquid; 4-18% of carbon nano tube dispersion liquid; 8-15% by weight of acidolysis agent; 0.03-0.15% by weight of an esterification catalyst; 0.01-1% by weight of a curing accelerator.
Wherein the polyol is one or more of neopentyl glycol (NPG), ethylene Glycol (EG), methyl propylene glycol (MPO), ethyl butyl propylene glycol (BEPD) and Cyclohexanedimethanol (CHDM); the aromatic polybasic acid is one or a mixture of terephthalic acid (PTA) and isophthalic acid (IPA); the branching agent adopts one or two of Trimethylolpropane (TMP) and Trimethylolethane (TME) to be mixed; the acidolysis agent is one or a mixture of more of isophthalic acid (IPA), adipic acid (ADA), 1,4 cyclohexanedicarboxylic acid (CHDA), fumaric acid (FCC) and trimellitic anhydride; the esterification catalyst is a tin catalyst, preferably one or more of dibutyltin oxide, tributyltin oxide, dihydroxybutyltin chloride, stannous oxalate or monobutyltin oxide; the curing accelerator is one or more of tetraethylammonium bromide, tetramethylammonium bromide, benzyltriethylammonium chloride and triphenyl ethyl phosphine bromide and dibutyltin dilaurate.
The carbon nanotube dispersion was selected from LB217-54 water series conductive paste of Jiangsu Tiannai technology, in which the diameter of the carbon nanotube was 5 to 7nm and the mass concentration was 5% by weight.
The preparation method of each 100g of graphene dispersion liquid comprises the following steps:
1) Adding 100-200g of graphene into a dispersion tank, adjusting the rotating speed of a high-speed shearing dispersion machine to 800-1000rpm, then adding 7-25g of graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 1200-2000rpm, and dispersing for 1-3 hours to obtain a graphene suspension;
2) Transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 15-21kHz, and the ultrasonic time is 10-30min;
3) Centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking the lower layer slurry-like substance, mixing with 100-200g of water, and then carrying out ultrasonic treatment; the ultrasonic frequency is 15-21kHz, and the ultrasonic time is 10-30min; and repeating the step for 2-3 times, mixing the slurry-like substance obtained after the ultrasonic treatment with 50-72g of organic polyol, and stirring until the mixture is uniform to obtain the graphene dispersion liquid. Wherein the organic polyol is one or more of neopentyl glycol (NPG), ethylene Glycol (EG), methyl propylene glycol (MPO), ethyl butyl propylene glycol (BEPD) or cyclohexane dimethanol (CHDM).
The curing agent is triglycidyl isocyanurate; the leveling agent is a GLP588 leveling agent; the auxiliary agent is any one or more of benzoin and a wetting agent 701B.
The inorganic filler is any one or a mixture of several of nano silicon dioxide, talcum powder and barium sulfate, and is mainly used for improving the mechanical property of the powder coating.
The preparation method of the salt spray resistant powder coating comprises the following steps: proportioning raw materials according to a formula → fully premixing in a mixing tank → extruding by an extruder → tabletting → crushing → grinding → sieving → packaging a finished product.
The formula of the salt spray resistant powder coating provided by the invention mainly has the following innovation points: 1) The graphene and carbon nanotube modified polyester resin is used as the main resin, the graphene and carbon nanotubes can be uniformly distributed in a coating formed by the polyester resin and the powder coating after modification, the problem of nonuniform distribution of the graphene and the carbon nanotubes in the powder coating caused by directly adding the graphene and the carbon nanotubes as raw materials of the powder coating is avoided, and simultaneously, a uniformly distributed layered barrier system consisting of the graphene and a three-dimensional conductive network consisting of the carbon nanotubes exist in a resin phase; 2) The graphene forming layer in the resin phase in the powder coating is cooperated with the barrier system formed by the polyaniline modified layered filler in the filler phase, so that the permeation of materials such as water vapor, oxygen, salt and the like is obviously prevented; 3) The conductive network formed by head-tail collision of carbon nanotubes uniformly distributed in a resin phase of the powder coating and the filler conductive network formed by mutual intersection of polyaniline modified layered fillers in the filler phase enable a compact synergistic conductive network to be formed inside a powder coating body, so that free electrons generated by electrochemical reaction can be transferred to the surface of a coating through the synergistic conductive network inside the powder coating and are quenched by the external environment, the electrochemical reaction is remarkably inhibited, and the salt spray resistance of the coating is improved by the synergy of the conductive network and the filler conductive network.
Compared with the conventional powder coating, the salt spray resistant powder coating provided by the invention has the advantages that the copper-accelerated acetate spray test time of the coating obtained after baking and curing is increased from 150 hours to 300-400 hours, and the salt spray resistance of the powder coating is obviously improved.
Detailed Description
The present invention will be described in detail with reference to examples.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
The carbon nanotube dispersion was selected from LB217-54 water series conductive paste of Jiangsu Tiannai technology, in which the diameter of the carbon nanotube was 5 to 7nm and the mass concentration was 5% by weight.
The preparation method of the graphene dispersion used in the following examples and comparative examples is as follows: adding 150g of water into a dispersion tank, adjusting the rotating speed of a high-speed shearing dispersion machine to 1000rpm, then adding 15g of graphene, stirring and uniformly dispersing, adjusting the rotating speed of the dispersion machine to 2000rpm, and dispersing for 3 hours to obtain a graphene suspension; 2) Transferring the graphene suspension into an ultrasonic container for ultrasonic treatment, wherein the ultrasonic frequency is 20kHz, and the ultrasonic time is 30min; 3) Centrifuging the graphene suspension subjected to ultrasonic treatment, removing supernatant, taking a lower-layer slurry-like substance, mixing with 120g of water, and performing ultrasonic treatment; after repeating this step 2 to 3 times, 35g of a slurry-like substance (a mixed system of 10g of graphene and 25g of water) obtained after the ultrasonic treatment was mixed with 65g of neopentyl glycol with stirring until uniform. That is, 100g of a graphene dispersion was obtained, in which the mass fraction of graphene was 10% by weight and the concentration of the organic polyol neopentyl glycol was 65% by weight.
The modified polyester resin B used in the following examples was prepared by the following method: preparing raw materials according to the following table 1, putting a formula amount of polyol, the prepared graphene dispersion liquid, the carbon nano tube dispersion liquid, a branching agent, an esterification catalyst and aromatic polybasic acid into a 5-liter glass reaction kettle, heating and melting the raw materials, then slowly heating up to 235-255 ℃ at 1-2 ℃/min in nitrogen atmosphere and maintaining the temperature, sampling and detecting that the Acid Value (AV) reaches 5-15 (unit mgKOH/g resin, the same applies hereinafter) after the system is clarified, adding an acidolysis agent and the like and maintaining the temperature at 235-250 ℃ for acidolysis and end capping, cooling to 230-240 ℃ at the rate of 3-5 ℃/min when the acid value of the polyester is 35-68mgKOH/g, and carrying out vacuum polycondensation for a period of time in vacuum-0.1 MPA so that the acid value of the polyester reaches 25-55mgKOH/g. Finally, the temperature is reduced to 180-230 ℃, the curing accelerator and the coupling agent are dosed according to the formula amount, and the materials are discharged after the materials are maintained for 5-30 min. Two samples of the modified polyester resin B prepared above are respectively marked as graphene and carbon nanotube modified polyester resin B1 and graphene and carbon nanotube modified polyester resin B2.
The preparation method of the polyester resin A1 used in the following comparative example was the same as the preparation method of the modified polyester resin B except that the graphene dispersion and the carbon nanotube dispersion were not added in the preparation process.
The polyester resin A2 used in the following comparative examples was prepared in the same manner as the modified polyester resin B except that the carbon nanotube dispersion was not added during the preparation.
The polyester resin A3 used in the following comparative examples was prepared in the same manner as the modified polyester resin B except that the graphene dispersion was not added during the preparation.
Polyester resins A1, A2 and A3 are used as reference samples and raw materials are used as comparative examples; the graphene and carbon nanotube modified polyester resins B1 and B2 are prepared by the method
Modified polyester resins in which the indices for controlling the acid value at the various stages are likewise indicated in Table 1.
TABLE 1 polyester resin A and graphene polyester resin B formulations, control of acid number and Performance during production
The preparation method of the polyaniline modified layered filler used in the following examples and comparative examples comprises the following steps:
the preparation method of the polyaniline modified mica powder comprises the following steps: 100g of mica powder, 5g of aniline and 1L of 0.2mol/L hydrochloric acid aqueous solution are uniformly mixed, 0.2mol/L ammonium sulfate aqueous solution 670mL is dropwise added at 30 ℃ under the stirring condition of 150rpm, in-situ polymerization reaction is carried out for 3-5 h at 30 ℃, after the reaction is finished, filtration treatment is carried out, polyaniline modified mica powder is collected, and the polyaniline modified mica powder is washed to be neutral by deionized water, so that 103g of polyaniline modified mica powder is obtained. The preparation method of the polyaniline modified nano montmorillonite comprises the following steps: 100g of nano montmorillonite, 5g of aniline and 1L of 0.18mol/L hydrochloric acid aqueous solution are uniformly mixed, 0.2mol/L of ammonium sulfate aqueous solution 600ml is dropwise added at 30 ℃ under the stirring condition of 150rpm, in-situ polymerization reaction is carried out for 3-5 h at 30 ℃, filtration treatment is carried out after the reaction is finished, polyaniline modified mica powder is collected and washed to be neutral by deionized water, and 104g of polyaniline modified mica powder is obtained.
The prepared polyester resins A1, A2 and A3, the graphene and carbon nano tube modified polyester resins B1 and B2, the polyaniline modified mica powder, the polyaniline modified nano montmorillonite, the curing agent, the leveling agent, the pigment, the inorganic filler, the auxiliary agent and the like are utilized to prepare the salt spray resistant powder coating, and the specific formula is shown in the following table.
TABLE 2 powder coating formulations for the examples and comparative examples
The preparation method of the powder coating of each of the above examples and comparative examples was: the different raw materials are weighed out in a compounding tank with reference to the formulation in table 2 and thoroughly premixed → coextruded by means of an extruder → tableted → comminuted → ground → sieved → packed into a finished product. Then the powder coating is sprayed on the surface of a standard salt spray test phosphated plate of Q-Lab company by electrostatic spraying, and the different performances of the coating are tested after baking at 200 ℃ for 10min, and the results are shown in Table 3.
TABLE 3 Properties of powder coatings for the respective examples and comparative formulations
Remarks are as follows: leveling grades PCI from 1 to 10 represent an improvement in leveling performance, where PCI-10 represents the same leveling performance as a mirror, and there are currently standard boards in commercial use for evaluating PCI grades.
As can be seen from Table 3, the salt spray resistant powder coating prepared from the modified polyester resin and the polyaniline modified layered filler has excellent salt spray resistance, the unilateral corrosion width of 250h in a copper-accelerated acetate spray test is less than 1.2mm, and the unilateral corrosion width of 400h in a copper-accelerated acetate spray test is less than 2mm.
The raw materials of the powder coating provided by the comparative example 1 are only added with common polyester resin and are not added with polyaniline modified layered filler, so that the corrosion resistance is poor, the single-sided corrosion width reaches 2.3mm when the copper is subjected to an accelerated acetate spray test for 250 hours, and the single-sided corrosion width reaches 3.7mm when the copper is subjected to an accelerated acetate spray test for 400 hours; the polyester resin added to the raw materials of the powder coatings provided in comparative examples 2 and 3 only undergoes single modification of graphene or carbon nanotubes, resulting in significantly weaker corrosion resistance of the powder coatings than the respective examples; comparative example 4 also provided a powder coating that was significantly less corrosion resistant than the examples, since the modification of the layered filler was not performed.
The above detailed description of a salt spray resistant powder coating and the method of preparing the same with reference to the examples is illustrative and not restrictive, and several examples are set forth in the limits of the invention, so that variations and modifications thereof without departing from the general inventive concept are intended to be within the scope of the invention.
Claims (10)
1. The salt spray resistant powder coating is characterized by comprising the following raw materials in percentage by mass: 50-65% of graphene and carbon nano tube modified polyester resin, 10-30% of polyaniline modified layered filler, 4-7% of curing agent, 0.8-1.2% of flatting agent, 0.7-28% of pigment, 10-30% of inorganic filler and 0.5-2% of auxiliary agent.
2. The salt spray resistant powder coating as claimed in claim 1, wherein the polyaniline-modified layered filler is prepared by the following method: uniformly mixing the layered filler, aniline and an inorganic acid aqueous solution, dropwise adding an ammonium persulfate solution under the stirring condition, carrying out in-situ polymerization reaction, filtering after the reaction is finished, and then washing with water to be neutral.
3. The salt fog resistant powder coating as claimed in claim 2, wherein the layered filler is one or a mixture of mica powder and nano montmorillonite; the inorganic acid is at least one of sulfuric acid, hydrochloric acid and nitric acid.
4. Root of herbaceous plantThe salt spray resistant powder coating composition as claimed in claim 2 or 3, wherein the inorganic acid aqueous solution contains H + The concentration of (A) is 0.1-2.0mol/L; the molar ratio of ammonium persulfate to aniline is 2-3:1; the mass ratio of the lamellar filler to the aniline is 1.02-0.1.
5. The salt spray resistant powder coating according to claim 2 or 3, wherein the in-situ polymerization reaction is carried out at a reaction temperature of 15 to 35 ℃ for a reaction time of not less than half an hour.
6. The salt spray resistant powder coating as claimed in claim 1 or 2, wherein the graphene and carbon nanotube modified polyester resin has an acid value of 25-55mgKOH/g resin, a number average molecular weight of 2500-5000g/mol, and a glass transition temperature (Tg) of 55 ℃ or higher.
7. The salt spray resistant powder coating as claimed in claim 1 or 2, wherein the graphene and carbon nanotube modified polyester resin has a graphene content of 0.3-5% by weight and a carbon nanotube content of 0.2-0.9% by weight.
8. The salt spray resistant powder coating of claim 1 or 2, wherein the curing agent is triglycidyl isocyanurate; the leveling agent is a GLP588 leveling agent; the auxiliary agent is any one or more of benzoin and a wetting agent 701B.
9. The salt spray resistant powder coating as claimed in claim 1 or 2, wherein the inorganic filler is one or a mixture of several of nano silica, talc and barium sulfate.
10. The method for preparing a salt spray resistant powder coating according to any one of claims 1 to 9, comprising the steps of: proportioning raw materials according to a formula → fully premixing in a mixing tank → extruding by an extruder → tabletting → crushing → grinding → sieving → packaging a finished product.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910752A (en) * | 2015-06-10 | 2015-09-16 | 华南理工大学 | Polyaniline graphene nano composite anticorrosion paint and preparation method thereof |
| CN105400373A (en) * | 2015-12-16 | 2016-03-16 | 常州大学 | Graphene/deimpurity polyaniline-containing anticorrosive coating and preparation method thereof |
| CN105482451A (en) * | 2016-01-18 | 2016-04-13 | 西安科技大学 | Organic montmorillonite/polyaniline composite material and preparation method thereof |
| CN112625225A (en) * | 2020-12-28 | 2021-04-09 | 常州市碳索新材料科技有限公司 | High-heat-dissipation powder coating and preparation method thereof |
| CN114539891A (en) * | 2022-04-06 | 2022-05-27 | 安徽舜邦精细化工有限公司 | High-weather-resistance and corrosion-resistance outdoor powder coating |
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- 2022-11-21 CN CN202211455360.1A patent/CN115895404A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104910752A (en) * | 2015-06-10 | 2015-09-16 | 华南理工大学 | Polyaniline graphene nano composite anticorrosion paint and preparation method thereof |
| CN105400373A (en) * | 2015-12-16 | 2016-03-16 | 常州大学 | Graphene/deimpurity polyaniline-containing anticorrosive coating and preparation method thereof |
| CN105482451A (en) * | 2016-01-18 | 2016-04-13 | 西安科技大学 | Organic montmorillonite/polyaniline composite material and preparation method thereof |
| CN112625225A (en) * | 2020-12-28 | 2021-04-09 | 常州市碳索新材料科技有限公司 | High-heat-dissipation powder coating and preparation method thereof |
| CN114539891A (en) * | 2022-04-06 | 2022-05-27 | 安徽舜邦精细化工有限公司 | High-weather-resistance and corrosion-resistance outdoor powder coating |
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