CN118374210B - A high wear-resistant powder coating, its preparation method and application - Google Patents
A high wear-resistant powder coating, its preparation method and applicationInfo
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- CN118374210B CN118374210B CN202410551815.2A CN202410551815A CN118374210B CN 118374210 B CN118374210 B CN 118374210B CN 202410551815 A CN202410551815 A CN 202410551815A CN 118374210 B CN118374210 B CN 118374210B
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- C—CHEMISTRY; METALLURGY
- 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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
- C09D163/10—Epoxy resins modified by unsaturated compounds
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- C—CHEMISTRY; METALLURGY
- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/03—Powdery paints
- C09D5/033—Powdery paints characterised by the additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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Abstract
本发明提供了一种高耐磨性粉末涂料及其制备方法与应用，涉及涂料技术领域。本发明的高耐磨性粉末涂料包含以下原料：改性环氧树脂、改性端羧基饱和聚酯树脂、聚四氟乙烯蜡微粉、煅烧高岭土、钛白粉、石英粉、助剂；其中，改性环氧树脂是双酚A环氧树脂先与植酸反应，然后加入肉桂酸、庚酸反应，最后经胺中和得到改性环氧树脂。所得涂料具有优异的耐磨性和强度，耐候性好，长时间使用后不会脱落破损，使用寿命长。This invention provides a high-wear-resistant powder coating, its preparation method, and its application, relating to the field of coating technology. The high-wear-resistant powder coating of this invention comprises the following raw materials: modified epoxy resin, modified carboxyl-terminated saturated polyester resin, polytetrafluoroethylene wax micropowder, calcined kaolin, titanium dioxide, quartz powder, and additives; wherein, the modified epoxy resin is obtained by first reacting bisphenol A epoxy resin with phytic acid, then adding cinnamic acid and heptanoic acid, and finally neutralizing with amine. The resulting coating exhibits excellent wear resistance and strength, good weather resistance, and will not peel or break after prolonged use, resulting in a long service life.
Description
Technical Field
The invention relates to the technical field of coatings, in particular to a high-wear-resistance powder coating and a preparation method and application thereof.
Background
The powder paint is a pure solid paint without volatile organic solvent, and its recipe mainly contains resin, curing agent, pigment, stuffing, additive, etc. Powder coatings generally comprise a host resin, filler, auxiliary agent, pigment, etc., and are generally classified into thermoplastic powder coatings and thermosetting powder coatings. The main resin of the thermoplastic powder coating is usually polyethylene, polyvinyl chloride, polyester, nylon, polyphenylene sulfide, polyvinyl fluoride and the like, and the thermoplastic powder coating is melted after being heated and leveled to form a coating film, but is remelted at high temperature. The main resin of the thermosetting powder coating is epoxy resin, epoxy resin-polyester, polyurethane, acrylic acid and the like, and the thermosetting powder coating can be solidified and crosslinked in the melting process to form a firm coating film, and can not be melted again at high temperature. The powder coating has the characteristics of no solvent, no pollution, recoverability, environmental protection, energy saving, high mechanical strength of coating film and the like, and is widely applied in various fields at present, including the fields of building materials, household appliances, electronic products, decks of automobiles and ships and the like.
As the application of powder coatings has increased, consumers have placed higher demands on the powder coatings. For example, the powder coating is easily rubbed by air flow, water flow scouring and mechanical force in the application process, so that the abrasion is quite serious, and the coating loses the original protection or aesthetic effect, so that the abrasion resistance of the powder coating is necessary to be improved.
The existing method for improving the wear resistance of the powder coating mainly comprises the steps of selecting main resin with high wear resistance, adding wear-resistant inorganic filler, auxiliary agent and the like. However, in the practical application process, the inorganic filler is difficult to uniformly disperse in the coating, the binding force between the resin and the inorganic filler is weak, the characteristic of enhancing the wear resistance of the inorganic filler is difficult to be exerted, other properties of the coating are easy to be influenced, and the market demand cannot be met.
Therefore, there is a need to develop a novel high abrasion resistant powder coating.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the high-wear-resistance powder coating, the preparation method and the application thereof, and the coating not only has higher wear resistance and strength, but also has excellent weather resistance, and can effectively prevent the coating from falling off and being damaged after long-term use, and has long service life.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a high-wear-resistance powder coating comprises the following raw materials of modified epoxy resin, modified carboxyl-terminated saturated polyester resin, polytetrafluoroethylene wax micropowder, calcined kaolin, titanium dioxide, quartz powder and an auxiliary agent;
the modified epoxy resin is obtained by reacting bisphenol A epoxy resin with phytic acid, then adding cinnamic acid and heptanoic acid for reaction, and finally neutralizing by amine.
The modified epoxy resin and the modified carboxyl-terminated saturated polyester resin are used as main resins, polytetrafluoroethylene wax micropowder and calcined kaolin are added as functional additives, and other auxiliary components are matched to prepare the powder coating, so that the powder coating has high wear resistance and strength, excellent weather resistance, and long service life, and can effectively prevent the coating from falling off and being damaged after long-term use.
Further, in the preparation process of the modified epoxy resin, the dosage of the phytic acid is 8-12% of the weight of the bisphenol A epoxy resin, the dosage of the cinnamic acid is 10-18% of the weight of the bisphenol A epoxy resin, and the dosage of the heptanoic acid is 20-30% of the weight of the bisphenol A epoxy resin.
Preferably, in the preparation process of the modified epoxy resin, the dosage of the phytic acid is 10% of the weight of the bisphenol A epoxy resin, the dosage of the cinnamic acid is 15% of the weight of the bisphenol A epoxy resin, and the dosage of the heptanoic acid is 26% of the weight of the bisphenol A epoxy resin.
Preferably, the modified epoxy resin is prepared by the following method:
Dissolving bisphenol A epoxy resin in absolute ethyl alcohol, heating to 70-80 ℃ after complete dissolution, adding phytic acid for reaction for 3-4h, then adding cinnamic acid and heptanoic acid, heating to 190-200 ℃ for reaction for further 1.5-2h, then cooling to 60-70 ℃, adding amine for neutralization, and finally drying to obtain the modified epoxy resin.
More preferably, in the preparation process of the modified epoxy resin, the mass ratio of the bisphenol A epoxy resin to the absolute ethyl alcohol is 0.5-1:1.
More preferably, in the preparation process of the modified epoxy resin, the amine is at least one of triethylamine, N-dimethylethanolamine and ammonia water.
The invention adopts a stepwise reaction method, firstly, the phosphoric acid group in the phytic acid reacts with the epoxy resin, then the phytic acid is grafted on the epoxy resin, then the cinnamic acid and the heptanoic acid are grafted to finish the modification of the epoxy resin, the modified epoxy resin is introduced into a long-chain structure, the ideal toughness is realized, the crosslinking degree of the coating can be increased, the compactness degree is increased, the wear resistance and the strength are improved, in addition, the dosages of the phytic acid, the cinnamic acid and the heptanoic acid, particularly the dosages of the phytic acid and the cinnamic acid are controlled, the strength and the wear resistance of the coating can be further improved, the friction coefficient of the surface of the coating is reduced, the smoothness is improved, the aging resistance and the weather resistance are also good, and the good covering and protecting capability can be maintained after long-time use.
Further, the calcined kaolin has an average particle size of 1 to 2 μm.
Further, the average particle diameter of the polytetrafluoroethylene wax micro powder is 2-5 mu m.
The modified carboxyl-terminated saturated polyester resin is prepared by dispersing diatomite in concentrated sulfuric acid, stirring, filtering, drying filter residues, calcining to obtain diatomite refined powder, adding bamboo fibers into an alkali solution for activation treatment, washing with water to be neutral after the treatment, drying to obtain activated bamboo fiber powder, adding the activated bamboo fiber powder into the carboxyl-terminated saturated polyester resin, adding a coupling agent, heating to 60-80 ℃, and adding the diatomite refined powder for reaction to obtain the modified carboxyl-terminated saturated polyester resin.
Preferably, the mass ratio of the diatomite to the concentrated sulfuric acid is 1:1-2, and the mass concentration of the concentrated sulfuric acid is 60-80%.
Preferably, the calcination temperature is 600-800 ℃ and the time is 30-40min.
Preferably, the stirring operation is to stir at 1000-1500r/min for 10min, then to reduce the rotation speed to 500-600r/min for 30-40min, and repeating the operation once again.
Preferably, the volume ratio of the bamboo fibers to the alkali solution is 1:1.5-2, and the alkali solution is sodium hydroxide solution with the mass fraction of 5-10%.
Preferably, the mass ratio of the carboxyl-terminated saturated polyester resin to the activated bamboo fiber powder to the diatomite refined powder is 1:0.3-0.5:0.2-0.4.
Preferably, the coupling agent is an organosilicon coupling agent selected from silane coupling agents or titanate coupling agents, including but not limited to at least one of KH550, KH560, KH570 and triisostearyl isopropyl titanate, and the amount of the silane coupling agent is 0.5-1% of the weight of the carboxyl-terminated saturated polyester resin.
Further, the auxiliary agent is at least one selected from curing agents, leveling agents, accelerators, antioxidants and coupling agents.
Preferably, the curing agent is a substance capable of accelerating the curing of the powder coating, and comprises at least one of 2-methylimidazole, 2-ethylimidazole, 2-ethyl-4-methylimidazole, dibutyltin dilaurate, triglycidyl isocyanurate, beta-hydroxyalkylamide and phenolic curing agent, wherein the adding amount of the curing agent is 0.1-3% of the total weight of the powder coating.
Preferably, the leveling agent can enable the paint to form a flat, smooth and uniform coating film in the drying film forming process, can effectively reduce the surface tension of finishing liquid and improve the leveling property and uniformity of the finishing liquid, and comprises at least one of polydimethylsiloxane, polymethylphenylsiloxane, alkyl modified organosiloxane, end group modified organosilicon, acrylic resin, urea resin and melamine formaldehyde resin, wherein the addition amount of the leveling agent is 0.1-3% of the total weight of the powder paint.
Preferably, the accelerator comprises at least one of methylimidazole, dimethyl imidazole, fumed silica and alumina, and the addition amount of the accelerator is 0.1-3% of the total weight of the powder coating.
Preferably, the antioxidant can improve the ageing resistance and durability of the coating, the antioxidant can be phosphite antioxidant, and the addition amount of the antioxidant is 0.5-2% of the total weight of the powder coating.
Preferably, the coupling agent is a silane coupling agent and/or a titanate coupling agent, and the addition amount of the coupling agent is 0.1-1% of the total weight of the powder coating.
Further, pigments can be added into the high-wear-resistance powder coating according to the requirements of customers. The pigments may impart color to the powder coating while improving the associated mechanical properties of the powder coating. The powder coating according to the invention may comprise a high temperature resistant metal matrix composite pigment. By "high temperature resistant" is meant a pigment that does not change its physicochemical properties at 250 ℃. Pigments suitable for use in the powder coating of the present invention may include, for example, titanium dioxide, carbon black, copper chrome black, and any mixtures thereof, added in an amount of 0.5 to 10% by weight of the total powder coating.
Further, fillers can be added into the high-wear-resistance powder coating, and the fillers suitable for the powder coating comprise at least one of mica powder, wollastonite, glass powder and talcum powder, wherein the addition amount of the fillers is 0.5-5% of the total weight of the powder coating.
Further, the high-wear-resistance powder coating comprises, by weight, 25-35 parts of modified epoxy resin, 28-32 parts of modified carboxyl-terminated saturated polyester resin, 5-8 parts of polytetrafluoroethylene wax micropowder, 16-20 parts of calcined kaolin, 5-6 parts of titanium dioxide, 6-8 parts of quartz powder and 1-4 parts of auxiliary agent.
Preferably, the high-wear-resistance powder coating comprises, by weight, 32 parts of modified epoxy resin, 30 parts of modified carboxyl-terminated saturated polyester resin, 7.5 parts of polytetrafluoroethylene wax micropowder, 16.6 parts of calcined kaolin, 5.2 parts of titanium dioxide, 7 parts of quartz powder and 1.7 parts of an auxiliary agent.
On the other hand, the invention also provides a preparation method of the high-wear-resistance powder coating, which comprises the following steps of uniformly mixing modified epoxy resin and modified carboxyl-terminated saturated polyester resin to obtain mixed resin, adding polytetrafluoroethylene wax micropowder, calcined kaolin, titanium dioxide, quartz powder and an auxiliary agent into the mixed resin in a stirring state, extruding, crushing and sieving after uniformly mixing to obtain the high-wear-resistance powder coating.
Further, the stirring speed is 500-800r/min.
Further, the sieving refers to sieving through a 150-200 mesh sieve.
Preferably, in order to further improve the wear resistance of the powder coating, polytetrafluoroethylene wax micropowder is added into isopropanol with the weight of 5-8 times at room temperature to be uniformly dispersed, then calcined kaolin is added into the powder coating in a stirring state, the temperature is reduced to 5-10 ℃ and kept at the temperature for 20-50min after uniform dispersion, then the temperature is increased to 60-70 ℃ and kept at the temperature for 60-100min, stirring is kept in the heat-preserving process, and finally the powder coating is dried, crushed and then added into mixed resin. According to the invention, polytetrafluoroethylene wax micropowder and calcined kaolin are treated, the polytetrafluoroethylene micropowder can be adsorbed on the surface of the calcined kaolin, and then the polytetrafluoroethylene micropowder is added into resin, so that the binding property with the resin is improved, the characteristic of enhancing the wear resistance can be better exerted, and compared with the method that two materials are directly added into the resin, the two materials are mixed and then added into the resin, and the weather resistance of the powder coating can be improved.
The invention also provides application of the high-wear-resistance powder coating in preparing wear-resistant materials.
Compared with the prior art, the invention has the following beneficial effects:
1. The modified epoxy resin and the modified carboxyl-terminated saturated polyester resin are used as matrix resin, and then a plurality of fillers and additives are added to prepare the powder coating, so that the obtained powder coating has excellent wear resistance, good toughness and weather resistance on the basis of ensuring coating coverage, and the service life is effectively prolonged, so that the powder coating cannot fall off and be damaged in the long-time use process.
2. According to the invention, the modified epoxy resin is added into the powder coating, so that the strength of the coating is effectively improved, the wear resistance of the coating is greatly improved, the friction coefficient of the surface of the coating is reduced, the smoothness is improved, the weather resistance of the coating is improved, and the service life is greatly prolonged compared with the unmodified epoxy resin.
3. In addition, the two materials are mixed and treated before being added into the powder coating, so that the weather resistance of the powder coating can be improved.
4. The invention has the characteristics of simple operation, strong safety, strong practicability and suitability for popularization and use.
Drawings
FIG. 1 is an infrared spectrum of a modified epoxy resin, wherein A represents an unmodified epoxy resin and B represents a modified epoxy resin.
Detailed Description
The following non-limiting examples will enable those of ordinary skill in the art to more fully understand the invention and are not intended to limit the invention in any way. The following is merely exemplary of the scope of the invention as claimed and many variations and modifications of the invention will be apparent to those skilled in the art in light of the disclosure, which are intended to be within the scope of the invention as claimed.
In the following specific embodiments, the modified carboxyl-terminated saturated polyester resin is specifically prepared by the following method:
(1) Adding concentrated sulfuric acid with the weight of 1.5 times and the mass fraction of 70% into diatomite powder, stirring and filtering, adding concentrated sulfuric acid with the weight of 1.5 times and the mass fraction of 80% into the diatomite powder, stirring and filtering, drying the filter residue, calcining at 800 ℃ for 30min to obtain diatomite refined powder, wherein the stirring operation is that stirring is carried out for 10min at 1000r/min, then the rotating speed is reduced to 500r/min, stirring is continued for 40min, and repeating the operation once;
(2) Adding sodium hydroxide aqueous solution with the weight of 2 times of the volume and the mass fraction of 8% into bamboo fibers, stirring for 1h at 1000r/min, washing with water to be neutral, filtering and drying to obtain activated bamboo fiber powder;
(3) Adding the activated bamboo fiber powder prepared in the step (2) into carboxyl-terminated saturated polyester resin, stirring for 30min under the condition of inert gas, adding isopropyl triisostearoyl titanate with the dosage of 1% of the carboxyl-terminated saturated polyester resin, heating to 80 ℃, adding diatomite refined powder, continuously stirring for 2h, cooling and discharging to obtain the modified carboxyl-terminated saturated polyester resin, wherein the mass ratio of the carboxyl-terminated saturated polyester resin to the activated bamboo fiber powder to the diatomite refined powder is 1:0.5:0.4.
In the present invention, unless otherwise indicated, the numerical range "a-b" represents an abbreviated representation of any combination of real numbers between a and b, and is intended to include all subranges subsumed therein. For example, the numerical range "1-10" means that all real numbers between "1-10" have been listed herein, e.g., can be 1.1, 1.2, 1.5, 2. This range is intended to include all subranges between (and including) the minimum value of 1 and the maximum value of 10, i.e., having a minimum value equal to or greater than 1 and a maximum value equal to or less than 10.
The invention is further illustrated by means of the following specific examples. The various chemical reagents used in the examples of the present invention were obtained by conventional commercial means unless otherwise specified.
Example 1:
The embodiment provides a preparation method of a high-wear-resistance powder coating, which comprises the following steps:
Mixing 25kg of modified epoxy resin and 32kg of modified carboxyl-terminated saturated polyester resin uniformly to obtain mixed resin, adding 8kg of polytetrafluoroethylene wax micropowder (average particle size of 5 mu m), 20kg of calcined kaolin (average particle size of 2 mu m), 6kg of titanium dioxide, 8kg of quartz powder and 1kg of auxiliary agent (0.5 kg of triglycidyl isocyanurate and 0.5kg of polydimethylsiloxane) into the mixed resin under stirring, extruding, crushing and sieving with a 200-mesh sieve to obtain the high-wear-resistance powder coating.
The modified epoxy resin is prepared by dissolving 25kg of bisphenol A epoxy resin in absolute ethyl alcohol according to the weight ratio of 0.5:1, heating to 70 ℃ after complete dissolution, adding 2kg of phytic acid for reaction for 4 hours, then adding 2.5kg of cinnamic acid and 7.5kg of heptanoic acid, heating to 190 ℃ for reaction for 2 hours, then cooling to 60 ℃, adding ammonia water for neutralization, and finally drying to obtain the modified epoxy resin.
The infrared spectrogram of the modified epoxy resin is shown in fig. 1, wherein a curve A represents unmodified epoxy resin, a curve B represents modified epoxy resin, and it can be seen that a characteristic peak of C-O-P appears near 1040cm -1 and an absorption peak of C=C double bond near 1953cm -1 relative to the curve A, which indicates that the modified epoxy resin is successfully prepared.
Example 2
The embodiment provides another preparation method of the high-wear-resistance powder coating, which comprises the following steps:
Mixing 32kg of modified epoxy resin and 30kg of modified carboxyl-terminated saturated polyester resin uniformly to obtain mixed resin, adding 7.5kg of polytetrafluoroethylene wax micropowder (average particle size of 2 mu m), 16.6kg of calcined kaolin (average particle size of 1 mu m), 5.2kg of titanium pigment, 7kg of quartz powder and 1.7kg of auxiliary agent (1 kg of beta-hydroxyalkylamide and 0.7kg of polymethylphenylsiloxane) into the mixed resin under stirring, extruding, crushing and sieving with a 180-mesh sieve to obtain the high-wear-resistance powder coating.
The modified epoxy resin is prepared by dissolving 32kg of bisphenol A epoxy resin in absolute ethyl alcohol according to the weight ratio of 0.5:1, heating to 80 ℃ after the bisphenol A epoxy resin is completely dissolved, adding 3.2kg of phytic acid for reaction for 3 hours, then adding 4.8kg of cinnamic acid and 8.32kg of heptanoic acid, heating to 200 ℃ for reaction for 1.5 hours, then cooling to 70 ℃, adding triethylamine for neutralization, and finally drying to obtain the modified epoxy resin.
Example 3
The embodiment provides another preparation method of the high-wear-resistance powder coating, which comprises the following steps:
Mixing 35kg of modified epoxy resin and 28kg of modified carboxyl-terminated saturated polyester resin uniformly to obtain mixed resin, adding 5kg of polytetrafluoroethylene wax micropowder (average particle size of 2 mu m), 16kg of calcined kaolin (average particle size of 1 mu m), 5kg of titanium dioxide, 7kg of quartz powder and 4kg of auxiliary agent (2 kg of beta dibutyltin dilaurate and 2kg of polydimethylsiloxane) into the mixed resin under stirring, extruding, crushing and sieving with a 180-mesh sieve to obtain the high-wear-resistance powder coating.
The modified epoxy resin is prepared by dissolving 35kg of bisphenol A epoxy resin in absolute ethyl alcohol according to the weight ratio of 0.5:1, heating to 80 ℃ after complete dissolution, adding 4.2kg of phytic acid for reaction for 3 hours, then adding 6.3kg of cinnamic acid and 7kg of heptanoic acid, heating to 200 ℃ for reaction for 1.5 hours, then cooling to 70 ℃, adding triethylamine for neutralization, and finally drying to obtain the modified epoxy resin.
Example 4
The embodiment provides another preparation method of the high-wear-resistance powder coating, which comprises the following steps:
Mixing 32kg of modified epoxy resin and 30kg of modified carboxyl-terminated saturated polyester resin uniformly to obtain mixed resin, adding 7.5kg of polytetrafluoroethylene wax micropowder (average particle size of 2 mu m) into isopropanol with the weight of 8 times at room temperature, dispersing uniformly, adding 16.6kg of calcined kaolin (average particle size of 1 mu m) under stirring, cooling to 5 ℃ after dispersing uniformly, preserving heat for 50min, heating to 60 ℃ and preserving heat for 100min, preserving heat, drying and crushing, adding the obtained mixture into the mixed resin, mixing uniformly, adding 5.2kg of titanium dioxide, 7kg of quartz powder and 1.7kg of auxiliary agent (1 kg of beta-hydroxyalkylamide and 0.7kg of polymethylphenylsiloxane), extruding, crushing, and sieving by a 180-mesh sieve to obtain the high-wear-resistance powder coating.
The preparation method of the modified epoxy resin is the same as in example 2.
Comparative example 1
This comparative example provides another method of preparing a high abrasion resistant powder coating, differing from example 2 in that the modified epoxy resin is replaced with an equivalent amount of bisphenol a epoxy resin.
Comparative example 2
The present comparative example provides another method for preparing a high abrasion resistant powder coating material, which is different from example 2 in that the modified epoxy resin in the present comparative example is prepared by the following method:
32kg of bisphenol A epoxy resin is dissolved in absolute ethyl alcohol according to the weight ratio of 0.5:1, heated to 80 ℃ after being completely dissolved, added with 2kg of phytic acid for reaction for 3 hours, then added with 3kg of cinnamic acid and 10kg of heptanoic acid, heated to 200 ℃ for reaction for 1.5 hours, cooled to 70 ℃, added with triethylamine for neutralization, and finally dried to obtain the modified epoxy resin.
Comparative example 3
The present comparative example provides another method for preparing a high abrasion resistant powder coating material, which is different from example 2 in that the modified epoxy resin in the present comparative example is prepared by the following method:
And (3) dissolving 32kg of bisphenol A epoxy resin in absolute ethyl alcohol according to a weight ratio of 0.5:1, heating to 80 ℃ after the bisphenol A epoxy resin is completely dissolved, adding 4kg of phytic acid for reaction for 3 hours, then adding 6kg of cinnamic acid and 6kg of heptanoic acid, heating to 200 ℃ for reaction for 1.5 hours, then cooling to 70 ℃, adding triethylamine for neutralization, and finally drying to obtain the modified epoxy resin.
Comparative example 4
The present comparative example provides another method for preparing a high abrasion resistant powder coating material, which is different from example 2 in that the modified epoxy resin in the present comparative example is prepared by the following method:
32kg of bisphenol A epoxy resin is dissolved in absolute ethyl alcohol according to the weight ratio of 0.5:1, heated to 80 ℃ after being completely dissolved, added with 3.2kg of phytic acid for reaction for 3 hours, then added with 8.32kg of heptanoic acid, heated to 200 ℃ for reaction for 1.5 hours, then cooled to 70 ℃, added with triethylamine for neutralization, and finally dried to obtain the modified epoxy resin.
Comparative example 5
The present comparative example provides another method for preparing a high abrasion resistant powder coating material, which is different from example 2 in that the modified epoxy resin in the present comparative example is prepared by the following method:
32kg of bisphenol A epoxy resin is dissolved in absolute ethyl alcohol according to the weight ratio of 0.5:1, heated to 80 ℃ after being completely dissolved, added with 4.8kg of cinnamic acid and 8.32kg of heptanoic acid, heated to 200 ℃ for reaction for 1.5 hours, cooled to 70 ℃, added with triethylamine for neutralization, and finally dried to obtain the modified epoxy resin.
Comparative example 6
This comparative example provides another method for preparing a high abrasion-resistant powder coating material, which is different from example 2 in that polytetrafluoroethylene wax fine powder is not added in this comparative example, and the composition is unchanged.
Comparative example 7
This comparative example provides another method of preparing a high abrasion resistant powder coating, differing from example 2 in that no calcined kaolin is added in this comparative example, which is unchanged in composition.
Comparative example 8
The comparative example provides another preparation method of the high-wear-resistance powder coating, which comprises the following steps of uniformly mixing 28kg of epoxy resin and 34kg of modified carboxyl-terminated saturated polyester resin, sequentially adding 0.5kg of hydroxyalkylamide, 20kg of Al 2O3 kg, 10kg of titanium dioxide, 6.5kg of quartz powder and 1kg of polymethylphenylsiloxane, continuously mixing at 300r/min for 50min, extruding, crushing and sieving with a 180-mesh sieve.
Test example 1
The powder coatings obtained in the examples and the comparative examples were subjected to the following tests after electrostatic spraying, and the coating thickness was 70. Mu.m;
(1) Film hardness A film hardness was measured by pencil test method with reference to the film hardness specified in GB/T6739-2006.
(2) Film impact resistance the film impact resistance was tested with reference to the film impact resistance test method specified in GB/T1732-2020.
(3) And (3) abrasion resistance, namely selecting S-33 sand paper as a friction material, converting the new sand paper into 100 pieces of sand paper in each test, measuring the abrasion loss of 200 pieces of coating by using the test load of 500 g.
(5) Salt spray resistance is tested by referring to a method for measuring neutral salt spray resistance of colored paint and varnish specified in GB/T1771-2007.
(6) Humidity test-test by referring to the film resistance to humidity and heat assay specified in GB/T1740-2007.
(7) Accelerated aging test, wherein the test item is a QUV-B test, the test condition is that the CUV is irradiated for 4 hours at 50 ℃ and the water vapor circulation test is carried out for 4 hours at 40 ℃.
The test results are shown in tables 1 and 2 below.
TABLE 1
| Group of | Hardness (2H) | Impact strength (kg/cm) | Wearing capacity (mg) |
| Example 1 | Scratch-free | 81 | 85.1 |
| Example 2 | Scratch-free | 86 | 83.0 |
| Example 3 | Scratch-free | 82 | 83.7 |
| Example 4 | Scratch-free | 87 | 80.4 |
| Comparative example 1 | Scratch-free | 70 | 94.2 |
| Comparative example 2 | Scratch-free | 73 | 91.6 |
| Comparative example 3 | Scratch-free | 75 | 90.5 |
| Comparative example 4 | Scratch-free | 74 | 92.8 |
| Comparative example 5 | Scratch-free | 75 | 93.0 |
| Comparative example 6 | Scratch-free | 60 | 99.8 |
| Comparative example 7 | Scratch-free | 65 | 97.0 |
| Comparative example 8 | Scratch-free | 63 | 101.7 |
As can be seen from the results in Table 1, the coating film formed by the powder coating obtained by the invention is smooth and flat, and has no scratch, abrasion loss of 80-86mg, good abrasion resistance and high impact resistance through 2H hardness test.
The abrasion loss of the coating film obtained in example 4 was lower than that of example 2, and it was found that the abrasion resistance of the coating material could be further improved by adding the polytetrafluoroethylene wax fine powder and calcined kaolin to the resin after mixing treatment.
As can be seen from the results of comparative examples 1 to 5, the epoxy resin in comparative example 1 was not modified, the impact resistance of the obtained coating film was significantly lower than that of example 2, the abrasion amount was higher than that of example 2, and the impact resistance and abrasion resistance of the coating films obtained in comparative examples 2 to 5 were also inferior to those of example 2, and it was found that the modification treatment of the epoxy resin helped to improve the strength and abrasion resistance of the coating.
From the results of comparative examples 6 and 7, it is understood that the polytetrafluoroethylene wax fine powder and the calcined kaolin simultaneously in the powder coating contribute to the improvement of the strength and abrasion resistance of the powder coating.
TABLE 2
| Group of | Salt spray resistance | Humidity test | Light retention after 1000h of accelerated aging (%) |
| Example 1 | >1000h | >2000h | 78.6 |
| Example 2 | >1000h | >2200h | 81.4 |
| Example 3 | >1000h | >2200h | 80.3 |
| Example 4 | >1000h | >2400h | 84.0 |
| Comparative example 1 | >800h | >1500h | 68.1 |
| Comparative example 2 | >1000h | >1800h | 69.7 |
| Comparative example 3 | >1000h | >2000h | 71.4 |
| Comparative example 4 | >1000h | >1800h | 70.7 |
| Comparative example 5 | >800h | >1800h | 70.1 |
| Comparative example 6 | >1000h | >2000h | 70.8 |
| Comparative example 7 | >1000h | >2000h | 72.2 |
| Comparative example 8 | >600h | >1400h | 67.5 |
As can be seen from the results in Table 2, the powder coating obtained by the invention can still maintain the light retention rate of more than 78% after accelerated aging for 1000 hours (the light retention rate in the test refers to the ratio of the glossiness of the coating after aging to the glossiness before aging), and the phenomena of cracking, foaming and peeling of the coating do not occur in the salt spray resistance test for 1000 hours and the humidity test for 2000 hours, so that the powder coating obtained by the invention has excellent weather resistance and effectively prolongs the service life.
The humidity test result and the aging resistance test result of the coating obtained in the example 4 are superior to those of the coating obtained in the example 2, and the weather resistance of the powder coating can be improved to a certain extent by adding the polytetrafluoroethylene wax micropowder and the calcined kaolin into the resin after the polytetrafluoroethylene wax micropowder and the calcined kaolin are mixed.
From the results of the salt spray resistance test, the humidity test and the accelerated aging test of the powder coating obtained in comparative example 1, it can be seen that the modification treatment of the epoxy resin contributes to the improvement of the weather resistance of the powder coating.
From the test results of the accelerated aging of comparative examples 2 to 5, it can be seen that the amount of the modifier used in the modification treatment of the epoxy resin affects the aging resistance of the paint and affects the service life thereof.
The test results of the accelerated aging of the comparative examples 6 and 7 show that the polytetrafluoroethylene wax micropowder and the calcined kaolin have a certain synergistic effect, and are beneficial to improving the aging resistance of the powder coating.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (9)
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| CN105062332A (en) * | 2015-09-08 | 2015-11-18 | 福建万安实业有限公司 | Powder coating with high wear resistance |
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