CN103275597A - High temperature-resistant ultralow temperature-cured epoxy polyester powdery coating - Google Patents
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Abstract
The invention discloses a high temperature-resistant ultralow temperature-cured epoxy polyester powdery coating. The high temperature-resistant ultralow temperature-cured epoxy polyester powdery coating solves the problem that the existing low temperature-cured epoxy polyester powdery coating has poor heat resistance and poor thermal conductivity so that in curing, temperatures in a coating film prepared from the existing low temperature-cured epoxy polyester powdery coating are not different and coating curing rates are not different and thus the coating film produces orange peel phenomenon and even crazes and coating film surface-effects are influenced. The high temperature-resistant ultralow temperature-cured epoxy polyester powdery coating is prepared from 30 to 40wt% of epoxy resin, 15 to 20wt% of polyester resin, 0.5 to 1.5wt% of polyarylene sulfide resin, 10 to 15wt% of titanium dioxide, 2 to 5wt% of nano-metal powder subjected to surface treatment, 0.5 to 1wt% of dibutyltin dilaurate, 1 to 3wt% of an assistant, 1 to 5wt% of sodium fluoride, 15 to 20wt% of a filling material and 10 to 15wt% of a pigment. The high temperature-resistant ultralow temperature-cured epoxy polyester powdery coating has a low curing temperature, good heat resistance, and physical and mechanical properties and chemical resistance satisfying industrial requirements.
Description
Technical field
The present invention relates to a kind of powder coating, especially relate to a kind of high temperature resistant cryogenic curing epoxy polyester powder coating.
Background technology
Heat curing-type epoxy/polyester powder coating is to be a kind of powder coating of main film forming substance with vibrin and Resins, epoxy.This powder coating is solvent-free, pollution-free, but traditional heat curing-type epoxy/polyester powder coating is 180 ~ 200 ℃ in solidification value normally, be to solidify under 15 ~ 30min condition set time, too high solidification value is the energy consumption height on the one hand, can the base material of poor heat resistance be impacted again, limit its application on the thermo-sensitivity base material, caused its range of application narrower; In addition, can only bear 200 ℃ of heatproofs by filming of forming of traditional heat curing-type epoxy/polyester powder coating, resistance toheat is relatively poor, when temperature surpasses 200 ℃, filming can cracking, efflorescence, fade, and this has just limited the application on the workpiece that heat curing-type epoxy/polyester powder coating uses in some high temperature field again; Of paramount importancely be, traditional heat curing-type epoxy/polyester powder coating heat transfer efficiency is poor, if the coating thickness of spraying is thinner, then when solidifying, the surface effect of filming there is not influence, if the coating thickness of spraying is thicker, when solidifying, easily causes the temperature in filming inconsistent, thereby make solidification rate inconsistent, be easy to cause the orange peel phenomenon of filming, the surface effect that influence is filmed.
Chinese patent publication number CN101289592A discloses a kind of ultra-low temperature epoxy resin and vibrin hybrid powder coatings open day on October 22nd, 2008, and by weight percentage, each components contents is respectively: Resins, epoxy 32 ~ 38%; Polyester 32 ~ 37%; Titanium dioxide 18 ~ 22%; Flow agent 0.2 ~ 1.8%; Defoamer 0.3 ~ 0.5%; Static inhibitor 1 ~ 1.2%; St-yrax 1%; Pigment 0.7 ~ 2%; Optical brightener 0.8 ~ 1%; Filler 2 ~ 5%.This powder coating does not still solve the problem of heat curing-type epoxy/polyester powder coating resistance toheat difference, can only use at a lower temperature, range of application is narrower, simultaneously, if the coating thickness of spraying is thicker, when solidifying, easily cause the temperature in filming inconsistent, the formation temperature gradient, thereby make that the solidification rate of filming is inconsistent, be easy to cause orange peel phenomenon even the cracking of filming, the surface effect that influence is filmed.
Summary of the invention
The present invention be for the temperature curing epoxy low polyester powder coating resistance toheat that solves prior art poor, range of application is narrower, heat conductivility is poor simultaneously, when coating thickness is thicker, when solidifying, easily cause the temperature in filming inconsistent, the formation temperature gradient, thereby make that the solidification rate of filming is inconsistent, easily cause orange peel phenomenon even the cracking of filming, the problem of the surface effect that influence is filmed provides a kind of high temperature resistant cryogenic curing epoxy polyester powder coating, and condition of cure of the present invention is 120 ℃ of solidification values, set time 15min, reduce the solidification value of powder coating greatly, enhance productivity, energy-saving effect is obvious, solved coating thickness inconsistent problem of solidification rate when thicker simultaneously, physical and mechanical properties of the present invention, chemical resistance all can satisfy industrial requirements, can be at plastics, use on the surface of thermo-sensitivity base materials such as timber, also has excellent heat resisting simultaneously, can use in the high temperature field, widen Application Areas and the range of application of powder coating.
To achieve these goals, the present invention is by the following technical solutions:
A kind of high temperature resistant cryogenic curing epoxy polyester powder coating, raw material by following mass percent is made: Resins, epoxy 30 ~ 40%, vibrin 15 ~ 20%, poly arylidene thio-ester resinoid 0.5 ~ 1.5%, titanium dioxide 10 ~ 15%, Nano metal powder 2 ~ 5% after surface treatment, dibutyltin dilaurate 0.5 ~ 1%, auxiliary agent 1 ~ 3%, Sodium Fluoride 1 ~ 5%, filler 15 ~ 20%, pigment 10 ~ 15%.Film-forming resin of the present invention is Resins, epoxy and vibrin, an inventive point of the present invention is to sneak into the poly arylidene thio-ester resinoid in film-forming resin, polyarylene sulfide resin and Resins, epoxy, the consistency of vibrin is good, and has outstanding high temperature resistance, can improve the cross-linking density of filming during curing, not only can improve physicals and the corrosion resistance nature of filming, can also improve the resistance to elevated temperatures of filming, but the resinoid melt viscosity that adds the whole system of affiliation change of poly arylidene thio-ester, influence levelling property, though can add the melt viscosity that flow agent improves whole system, but need to add a large amount of flow agents like this, and the consistency of flow agent and resin is poor, and the flow agent add-on is too much, can influence the over-all properties of filming; Another inventive point of the present invention is to have added dibutyltin dilaurate, the contriver finds in process of production, if when preparation is of the present invention, add dibutyltin dilaurate, the powder coating solidification temperature that obtains can reduce by 10 ~ 20 ℃, make solidification value of the present invention can be low to moderate 120 ℃, more be conducive to the reduction of energy consumption, tracing it to its cause may be the effect that dibutyltin dilaurate has played curing catalyst, reduced solidification value, the adding of dibutyltin dilaurate simultaneously can also improve the melt viscosity of whole system, reduces the influence that the adding because of polyarylene sulfide resin produces whole system melt viscosity greatly; Added the Nano metal powder after surface treatment among the present invention again, Nano metal powder has good heat conductance, and the one, can play good thermolysis, improve the resistance to elevated temperatures of filming greatly; The 2nd, can play good conductive force, flash heat transfer, reduce thermograde, make and to film that the temperature at each position can be consistent when solidifying, thereby the solidification rate at each position of filming is consistent, the surface effect that assurance is filmed, Nano metal powder is carried out surface treatment, overcome its agglomeration, it is more even that it is disperseed in resin, simultaneously to improve the consistency of itself and resin, can well soak into mutually with resin and increase bonding strength, film coated surface is smooth more smooth, in addition, the adding of Nano metal powder also can improve the intensity of filming, but the affiliation that adds of Nano metal powder influences powder coating greatly at the sticking power of workpiece surface, reduce film and workpiece between cohesive force, making films easily throws off, and in order to address this problem, the contriver adds Sodium Fluoride in powder coating, and Sodium Fluoride has corrodibility, in the process of coating baking heating, can destroy the structure of workpiece surface, make its roughen, so just be conducive to improve the cohesive force of filming with workpiece surface, be difficult for throwing off.Pigment among the present invention must be selected heatproof＞180 ℃, and kind then can be selected arbitrarily according to color.The present invention fills a prescription rationally, cost is low, solidification value is low, can enhance productivity, energy-saving effect is obvious, have good meltbility, flowability and solidified nature, physical and mechanical properties, chemical resistance all can satisfy industrial requirements, strong adhesion can use on the surface of thermo-sensitivity base materials such as plastics, timber, also has excellent heat resisting, can use in the high temperature field, widened Application Areas and the range of application of powder coating, it is inconsistent to efficiently solve the thicker temperature of filming when solidifying of thickness, easily causes the orange peel phenomenon of filming or the problem of cracking.
As preferably, make by the following method through the Nano metal powder after the surface treatment: Nano metal powder is used frequency 15 ~ 20KHz in treating compound, the ultrasonic echography of power 200 ~ 300W is handled behind 30 ~ 60min 70 ~ 80 ℃ of following oven dry and is namely got Nano metal powder after surface treatment, described treating compound is made up of following component by mass percent: polyoxyethylene 3 ~ 5%, silane coupling agent 0.1 ~ 0.5%, vitamins C 1 ~ 5%, surplus are water.Silane coupling agent is conducive to the dispersion of Nano metal powder in resin, polyoxyethylene can improve the consistency of Nano metal powder and resin, and vitamins C can effectively be avoided Nano metal powder blackening when oven dry, thereby influence outward appearance and the color and luster of filming ultrasonicly then are conducive to the dispersion of nano metal powder in treating compound.
As preferably, the Nano metal powder particle diameter after surface treatment is 10 ~ 30 μ m.Excessive or the too small over-all properties that all can influence powder coating of the particle diameter of Nano metal powder, the Nano metal powder particle diameter is 10 ~ 30 μ m, the over-all properties of powder coating is good.
As preferably, Nano metal powder is nanometer aluminium powder or copper nanoparticle.Nanometer aluminium powder and copper nanoparticle cost are low, be easy to get, and heat-conducting effect are good, and be little to the aberration influence of coating.
As preferably, described Resins, epoxy is 88～93 ℃ of softening temperatures, and oxirane value is at 0.11 ~ 0.14 bisphenol A type epoxy resin.The bisphenol A type epoxy resin cost is low, adopts bisphenol A type epoxy resin and vibrin adapted, not only makes the overall performance of filming good, and cost also relatively rationally.
As preferably, described vibrin be acid number at 70～75mgKOH/g, softening temperature is 85 ~ 95 ℃ terminal carboxyl polyester resin.
As preferably, described poly arylidene thio-ester resinoid is polyphenylene sulfide.
As preferably, described auxiliary agent is made up of flow agent, optical brightener and air release agent, and the mass percent of each component is respectively in the auxiliary agent: flow agent 20 ~ 30%, optical brightener 25 ~ 35%, air release agent 30 ~ 40%.
As preferably, described flow agent is cellulose acetate butyrate (CAB), and optical brightener is butyl acrylate, and air release agent is st-yrax.
As preferably, the mixed fillers that described filler mixes for active micro silicon powder and process white by mass ratio 1:2 ~ 3.The chemical constitution difference of different fillers, physical propertiess such as density, hardness, size-grade distribution and oil number are different, this will influence reactive behavior and the melt viscosity of polyester epoxy powder coating, also influence the performances such as levelling property, gloss, shock-resistance and pencil hardness of filming simultaneously, the present invention is by constantly screening and optimization, it is the active micro silicon powder of 1:2 ~ 3 and the mixed fillers that process white mixes that filler adopts by mass ratio, when guaranteeing performance powder coating, and can be greatly through low cost.
Therefore, the present invention has following beneficial effect:
(1) prescription is reasonable, and solidification value is low, good heat resistance, and cost is low, good combination property;
(2) add polyarylene sulfide resin, improve the resistance to elevated temperatures of filming;
(3) add dibutyltin dilaurate, reduced solidification value, reduced simultaneously the influence that the adding because of polyarylene sulfide resin produces whole system melt viscosity greatly;
(4) add Nano metal powder after surface treatment, improved the resistance to elevated temperatures of filming greatly, made simultaneously and film that the temperature at each position can be consistent when solidifying, thereby the solidification rate at each position of filming is consistent, guaranteed the surface effect of filming;
(5) Nano metal powder has been carried out surface treatment, overcome its agglomeration, it is more even that it is disperseed in resin, simultaneously to improve itself and the consistency of resin, can well soak into the increase bonding strength mutually with resin;
(6) add Sodium Fluoride, effectively solve the Nano metal powder that adds after the surface treatment caused film and workpiece surface between the problem that reduces of cohesive force.
Embodiment
The present invention will be further described below by concrete embodiment.
In the present invention, if not refer in particular to, all per-cents are weight unit, all devices and raw material all can be buied from market or the industry is commonly used, wherein, Nano metal powder is all available from Jiaozhuo companion's nano material Engineering Co., Ltd, and silane coupling agent is available from Nanjing really chemical industry company limited difficult to understand, model KH550.Method among the following embodiment if no special instructions, is this area ordinary method.
Embodiment 1
(1) be that the nanometer aluminium powder of 10 μ m is used frequency 15KHz with particle diameter in treating compound, the ultrasonic echography of power 300W is dried down at 70 ℃ after handling 30min, nanometer aluminium powder that must be after surface treatment, described treating compound is made up of following component by mass percent: polyoxyethylene 5%, silane coupling agent 0.1%, vitamins C 1%, surplus are water.
(2) proportioning according to table 1 takes by weighing Resins, epoxy, vibrin, the poly arylidene thio-ester resinoid, titanium dioxide, nanometer aluminium powder after surface treatment, dibutyltin dilaurate, auxiliary agent, Sodium Fluoride, filler, pigment, wherein, Resins, epoxy is 88 ℃ of softening temperatures, oxirane value is at 0.14 bisphenol A type epoxy resin, vibrin is that acid number is at 75mgKOH/g, softening temperature is 95 ℃ terminal carboxyl polyester resin, the poly arylidene thio-ester resinoid is polyphenylene sulfide, auxiliary agent is by flow agent, optical brightener and air release agent are formed, flow agent is cellulose acetate butyrate (CAB), optical brightener is butyl acrylate, air release agent is st-yrax, and the mass percent of each component sees Table 2 in the auxiliary agent, and filler is mixed by active micro silicon powder and the process white of mass ratio 1:2, pigment is lemon orange H10G, comes this trade mark 149.
(3) each component pre-mixing is finished the back melt extrude by twin screw extruder, extrude sheet stock and after cooling off, pulverize, sieving, namely get high temperature resistant cryogenic curing epoxy polyester powder coating.
Embodiment 2
(1) be that the nanometer aluminium powder of 20 μ m is used frequency 16KHz with particle diameter in treating compound, the ultrasonic echography of power 260W is dried down at 75 ℃ after handling 40min, nanometer aluminium powder that must be after surface treatment, described treating compound is made up of following component by mass percent: polyoxyethylene 4%, silane coupling agent 0.2%, vitamins C 3%, surplus are water.
(2) proportioning according to table 1 takes by weighing Resins, epoxy, vibrin, the poly arylidene thio-ester resinoid, titanium dioxide, nanometer aluminium powder after surface treatment, dibutyltin dilaurate, auxiliary agent, Sodium Fluoride, filler, pigment, wherein, Resins, epoxy is 90 ℃ of softening temperatures, oxirane value is at 0.12 bisphenol A type epoxy resin, vibrin is that acid number is at 72mgKOH/g, softening temperature is 90 ℃ terminal carboxyl polyester resin, the poly arylidene thio-ester resinoid is polyphenylene sulfide, auxiliary agent is by flow agent, optical brightener and air release agent are formed, flow agent is cellulose acetate butyrate (CAB), optical brightener is butyl acrylate, air release agent is st-yrax, the mass percent of each component sees Table 2 in the auxiliary agent, and filler is mixed by active micro silicon powder and the process white of mass ratio 1:2.5, and pigment is barba hispanica.
Embodiment 3
(1) be that the nanometer aluminium powder of 30 μ m is used frequency 20KHz with particle diameter in treating compound, the ultrasonic echography of power 200W is dried down at 80 ℃ after handling 60min, nanometer aluminium powder that must be after surface treatment, described treating compound is made up of following component by mass percent: polyoxyethylene 3%, silane coupling agent 0.5%, vitamins C 5%, surplus are water.
(2) proportioning according to table 1 takes by weighing Resins, epoxy, vibrin, the poly arylidene thio-ester resinoid, titanium dioxide, nanometer aluminium powder after surface treatment, dibutyltin dilaurate, auxiliary agent, Sodium Fluoride, filler, pigment, wherein, Resins, epoxy is 93 ℃ of softening temperatures, oxirane value is at 0.11 bisphenol A type epoxy resin, vibrin is that acid number is at 70mgKOH/g, softening temperature is 85 ℃ terminal carboxyl polyester resin, the poly arylidene thio-ester resinoid is polyphenylene sulfide, auxiliary agent is by flow agent, optical brightener and air release agent are formed, flow agent is cellulose acetate butyrate (CAB), optical brightener is butyl acrylate, air release agent is st-yrax, the mass percent of each component sees Table 2 in the auxiliary agent, and filler is mixed by active micro silicon powder and the process white of mass ratio 1:3, and pigment is red iron oxide.
High temperature resistant each feed composition mass percent of cryogenic curing epoxy polyester powder coating among table 1 embodiment
| Component | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Resins, epoxy | 40% | 30.50% | 30% |
| Vibrin | 15% | 15.50% | 20% |
| The poly arylidene thio-ester resinoid | 0.50% | 0.60% | 1.50% |
| Titanium dioxide | 10% | 15% | 11% |
| Nanometer aluminium powder after surface treatment | 2% | 5% | 3% |
| Dibutyltin dilaurate | 0.50% | 0.60% | 1% |
| Auxiliary agent | 1% | 1.10% | 3% |
| Sodium Fluoride | 1% | 1.20% | 5% |
| Filler | 20% | 15.50% | 15% |
| Pigment | 10% | 15% | 10.50% |
Each constituent mass per-cent in each embodiment auxiliary agent of table 2
| Auxiliary agent | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Cellulose acetate butyrate (CAB) | 30% | 35% | 40% |
| Butyl acrylate | 30% | 35% | 25% |
| St-yrax | 40% | 30% | 35% |
High temperature resistant cryogenic curing epoxy polyester powder coating of the present invention is 120 ℃ of solidification values, set time 15min condition of cure under solidify after, filming of obtaining has following characteristic properties:
| Performance index | Standard or method | Detected result |
| 60 ° of gloss | GB/T9754-1988 | ＞90% |
| Sticking power (cross-hatching) | GB/T9286-1998 | ≤ 1 grade |
| Pencil hardness | GB/T6739-1996 | 2 |
| Shock resistance (Kg.cm) | GB/T1732-1993 | 50 |
| Pliability test (mm) | GB/T6742-1986 | 2 |
| Salt-fog test | GB/T1771-1991 | ＞500h |
| Humid heat test | GB/T1740-1979 | ＞1000h |
| Thermotolerance | Gloss retention can be excellent, E≤0.3-0.4 | 250 ℃/24h(white) |
Condition of cure of the present invention is 120 ℃, 15min, more existing epoxy polyester powder coating is capable of reducing energy consumption more than 30%, the energy-saving effect highly significant, physical and mechanical properties of the present invention, chemical resistance all can satisfy industrial requirements simultaneously, can use on the surface of thermo-sensitivity base materials such as plastics, timber, also has excellent heat resisting, the upper limit temperature of heat tolerance reaches 300 ℃, can use in the high temperature field, has widened Application Areas and the range of application of powder coating.
Above-described embodiment is a kind of preferable scheme of the present invention, is not that the present invention is done any pro forma restriction, also has other variant and remodeling under the prerequisite that does not exceed the technical scheme that claim puts down in writing.
Claims (10)
1. high temperature resistant cryogenic curing epoxy polyester powder coating, it is characterized in that, made by the raw material of following mass percent: Resins, epoxy 30 ~ 40%, vibrin 15 ~ 20%, poly arylidene thio-ester resinoid 0.5 ~ 1.5%, titanium dioxide 10 ~ 15%, the Nano metal powder 2 ~ 5% after surface treatment, dibutyltin dilaurate 0.5 ~ 1%, auxiliary agent 1 ~ 3%, Sodium Fluoride 1 ~ 5%, filler 15 ~ 20%, pigment 10 ~ 15%.
2. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1, it is characterized in that, make by the following method through the Nano metal powder after the surface treatment: Nano metal powder is used frequency 15 ~ 20KHz in treating compound, the ultrasonic echography of power 200 ~ 300W is handled behind 30 ~ 60min 70 ~ 80 ℃ of following oven dry and is namely got Nano metal powder after surface treatment, described treating compound is made up of following component by mass percent: polyoxyethylene 3 ~ 5%, silane coupling agent 0.1 ~ 0.5%, vitamins C 1 ~ 5%, surplus are water.
3. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1 and 2 is characterized in that the Nano metal powder particle diameter after surface treatment is 10 ~ 30 μ m.
4. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 3 is characterized in that Nano metal powder is nanometer aluminium powder or copper nanoparticle.
5. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1 is characterized in that described Resins, epoxy is 88～93 ℃ of softening temperatures, and oxirane value is at 0.11 ~ 0.14 bisphenol A type epoxy resin.
6. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1 is characterized in that, described vibrin be acid number at 70～75mgKOH/g, softening temperature is 85 ~ 95 ℃ terminal carboxyl polyester resin.
7. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1 is characterized in that described poly arylidene thio-ester resinoid is polyphenylene sulfide.
8. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1, it is characterized in that described auxiliary agent is made up of flow agent, optical brightener and air release agent, the mass percent of each component is respectively in the auxiliary agent: flow agent 30 ~ 40%, optical brightener 25 ~ 35%, air release agent 30 ~ 40%.
9. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 8 is characterized in that described flow agent is cellulose acetate butyrate (CAB), and optical brightener is butyl acrylate, and air release agent is st-yrax.
10. a kind of high temperature resistant cryogenic curing epoxy polyester powder coating according to claim 1 is characterized in that, the mixed fillers that described filler mixes for active micro silicon powder and process white by mass ratio 1:2 ~ 3.
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