CN105062330A - High-performance thermosetting polyester powder coating - Google Patents
High-performance thermosetting polyester powder coating Download PDFInfo
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- CN105062330A CN105062330A CN201510438619.5A CN201510438619A CN105062330A CN 105062330 A CN105062330 A CN 105062330A CN 201510438619 A CN201510438619 A CN 201510438619A CN 105062330 A CN105062330 A CN 105062330A
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Abstract
The discloses a high-performance thermosetting polyester powder coating which comprises the raw materials: pure polyester resin, fluorinated polyester resin, epoxy resin, terminal carboxyl nitrile rubber, N,N,N,N'-tetra(2-ethoxyl) adipamide, tetramethoxyl methyl glycoluril, triglycidyl isocyanurate, amino resin, phenyl-2-imidazoline, 2-methylimidazole, chitosan, sodium lignin sulfonate, starch, polyethylene, polyvinyl butyral, nano titanium dioxide, aluminium oxide, zinc borate, mica iron oxide, montmorillonite, nanosilver, activated carbon powder, lanthanum oxide and auxiliaries. The high-performance thermosetting polyester powder coating disclosed by the invention is good in water resistance, oil resistance and heat resistance and excellent in weather resistance, acid and alkaline corrosion resistance and pollution resistance, and is good in comprehensive performance and long in service life if being used as an outdoor coating.
Description
Technical field
The present invention relates to technical field of coatings, particularly relate to a kind of high-performance thermosetting polyester type powder paint.
Background technology
Powder coating is that one does not contain solvent, and forms the new coating of film after carrying out construction application with powder morphology.Compared with traditional solvent based coating, the discharge of powder coating organic solvent volatile matter (VOC) when solidifying is almost nil, avoids the pollution to environment; Meanwhile, it is high that powder coating has utilization ratio, and coating property is good and be convenient to realize the advantages such as automation paint, obtains in recent years and develops faster.
Powder coating can be divided into thermoplastic powder coating and thermosetting powder coating(s) by the character according to powder coating filmogen, wherein polyester powder coating is the thermosetting powder coating(s) of a kind of excellent performance that development in recent years is got up, there is weathering resistance and excellent heat resistance, raw material sources be abundant, coating performance is good, the advantage such as low price, being widely used in the aspects such as hard shoulder, freeway guardrail, outdoor transformer, automobile, traffic sign, is a kind of important weather-resistance powder coatings for open air.But when it is for outdoor environment, often be subject to the impact of the climatic factor such as rainwater, humidity, cause the mechanical properties decrease of film, occur crackle and embrittlement, water easily diffuses into the ester group hydrolyses making vibrin in the film of polyester powder coating simultaneously, thus shortens the work-ing life of film.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of high-performance thermosetting polyester type powder paint, its water tolerance, oil-proofness and good heat resistance, weathering resistance, acid-alkali-corrosive-resisting and anti-pollution characteristic are excellent, be used as outdoor application, good combination property, long service life.
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: pure polyester resin 40-55 part, fluorine-containing vibrin 3-8 part, epoxy resin 5-15 part, nbr carboxyl terminal 5-15 part, N, N, N ', N '-four (2-hydroxyethyl) adipamide 1-5 part, four methoxy methyl glycoluril 2-10 parts, isocyanuric acid three-glycidyl ester 1-5 part, aminoresin 1-5 part, 2-benzylimidazoline 1-5 part, glyoxal ethyline 3-10 part, chitosan 1-8 part, sodium lignosulfonate 1-5 part, starch 2-5 part, polyethylene 2-5 part, polyvinyl butyral acetal 3-10 part, nano titanium oxide 5-15 part, aluminum oxide 2-10 part, zinc borate 1-5 part, iron mica 2-10 part, polynite 1-5 part, nanometer silver 2-10 part, activity charcoal powder 1-5 part, lanthanum trioxide 2-6 part, auxiliary agent 1-5 part.
Preferably, in its raw material, the weight ratio of pure polyester resin, fluorine-containing vibrin, epoxy resin, nbr carboxyl terminal is 45-53:5-8:6-12:7-13.
Preferably, its raw material comprises following component by weight: pure polyester resin 48-52 part, fluorine-containing vibrin 7-8 part, epoxy resin 8-10 part, nbr carboxyl terminal 10-12 part, N, N, N ', N '-four (2-hydroxyethyl) adipamide 3-5 part, four methoxy methyl glycoluril 6-8 parts, isocyanuric acid three-glycidyl ester 2.5-4 part, aminoresin 3-4.5 part, 2-benzylimidazoline 3-4.5 part, glyoxal ethyline 6-9 part, chitosan 5-7 part, sodium lignosulfonate 3-4 part, starch 3-4.5 part, polyethylene 3-4 part, polyvinyl butyral acetal 7-9 part, nano titanium oxide 8-12 part, aluminum oxide 6-8 part, zinc borate 3-4 part, iron mica 6-7 part, polynite 2-3 part, nanometer silver 6-9 part, activity charcoal powder 2-3.8 part, lanthanum trioxide 4-6 part, auxiliary agent 2-3.5 part.
Preferably, its raw material comprises following component by weight: pure polyester resin 50 parts, 7.6 parts, fluorine-containing vibrin, epoxy resin 9 parts, nbr carboxyl terminal 11 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 4 parts, four methoxy methyl glycoluril 7 parts, isocyanuric acid three-glycidyl ester 3 parts, 3.6 parts, aminoresin, 2-benzylimidazoline 4 parts, glyoxal ethyline 7 parts, chitosan 6.5 parts, sodium lignosulfonate 3.8 parts, starch 4 parts, polyethylene 3.5 parts, polyvinyl butyral acetal 8.2 parts, nano titanium oxide 10 parts, 7 parts, aluminum oxide, zinc borate 3.8 parts, iron mica 6.5 parts, polynite 2.6 parts, nanometer silver 7 parts, activity charcoal powder 3.2 parts, lanthanum trioxide 5.3 parts, auxiliary agent 3 parts.
Preferably, described pure polyester resin is the combination of a kind of in terminal carboxyl polyester resin and hydroxyl telechelic polyester resin or two kinds.
Preferably, the acid number of described terminal carboxyl polyester resin is 400-550mgKOH/g, and molecular weight is 3000-5000, and second-order transition temperature is 60-65 DEG C; The molecular weight of described hydroxyl telechelic polyester resin is 4000-5500, and second-order transition temperature is 60-65 DEG C.
Preferably, described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 1-3:3-8:1-3.
Preferably, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by epoxy chloropropane and sodium hydroxide, then hexafluoroisopropanol and Dimethylsilanediol is added, be warming up to 55-60 DEG C, reaction 4-6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; Cyclohexyl dimethanol, pyromellitic dianhydride, Mono-n-butyltin, epoxy chloropropane and glycidyl ether are added in dimethyl formamide and mixes, then under the protection of nitrogen, 105-130 DEG C is warming up to, reaction 2-4h, acetone is added after reaction terminates, then the mixed solvent of second alcohol and water is added, leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin; In the preparation process of fluorine-containing vibrin, hexafluoroisopropanol and Dimethylsilanediol is introduced in system, improve water-resistant coating and thermotolerance, in addition, have selected cyclohexyl dimethanol and the pyromellitic dianhydride raw material as reaction, the fluorine-containing vibrin hydrophobicity obtained is good, improves water tolerance and the weathering resistance of coating.
Preferably, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 25-35 part epoxy chloropropane and 2-3 part sodium hydroxide by weight, then 5-15 part hexafluoroisopropanol and 5-15 part Dimethylsilanediol is added, be warming up to 55-60 DEG C, reaction 4-6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates, by weight by 1-3 part cyclohexyl dimethanol, 8-15 part pyromellitic dianhydride, 1-2 part Mono-n-butyltin, 30-45 part epoxy chloropropane and 25-50 part glycidyl ether add in 8-15 part dimethyl formamide and mix, then under the protection of nitrogen, 105-130 DEG C is warming up to, reaction 2-4h, 10-25 part acetone is added after reaction terminates, then the mixed solvent of 50-100 part second alcohol and water is added, in the mixed solvent of wherein second alcohol and water, the ratio of the volume of second alcohol and water is 1:3-5, leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Preferably, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 32 parts of epoxy chloropropane and 2.5 parts of sodium hydroxide by weight, then 12 parts of hexafluoroisopropanols and 10 parts of Dimethylsilanediols are added, be warming up to 58 DEG C, reaction 4.6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 2 parts of cyclohexyl dimethanols, 10 parts of pyromellitic dianhydrides, 1.5 parts of Mono-n-butyltins, 38 parts of epoxy chloropropane and 40 parts of glycidyl ethers are added in 12 parts of dimethyl formamides and mix; then under the protection of nitrogen, 125 DEG C are warming up to; reaction 3.5h; 20 parts of acetone are added after reaction terminates; then the mixed solvent of 80 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:4; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
High-performance thermosetting polyester type powder paint of the present invention can powder coating preparation technology conveniently, by proportioning by after each raw material mixing through twin screw extruder mixing extrusion, pulverize, sieve after obtain.
In the present invention, with the filmogen that pure polyester resin is main, and with the addition of fluorine-containing vibrin, epoxy resin, nbr carboxyl terminal coordinates with pure polyester resin, improve the water tolerance of powder coating, thermotolerance and the sticking power with base material, wherein, the fluorine-containing vibrin added is by fluorine introducing system, the atomic radius of fluorine is little, the polarizability of C-F key is little, intramolecule compact structure, show low surface tension, the surface energy of adding fluorine-containing vibrin is low, can at surface enrichment, make coating hydrophobic oleophobic, improve the water tolerance of film, resistance to soiling and resistance to acids and bases, epoxy resin joins in system, improves the erosion resistance of film on the one hand, prevents the defect adding the sticking power reduction caused because of fluorine on the other hand, nbr carboxyl terminal adds in system, improves the consistency of each raw material, improves thermotolerance and the oil-proofness of coating simultaneously, further improves the weathering resistance of coating, N, N, N ', N '-four (2-hydroxyethyl) adipamide, four methoxy methyl glycoluril, isocyanuric acid three-glycidyl ester and aminoresin coordinate as solidifying agent, and with the addition of 2-benzylimidazoline and glyoxal ethyline, while not reducing coating heat resistance, reduce solidification value, shorten set time, nano titanium oxide, aluminum oxide, zinc borate, iron mica, polynite, nanometer silver, activity charcoal powder, lanthanum trioxide add in system, be uniformly dispersed in system, the hardness of coating, thermotolerance, pollution resistance and ageing resistance is improved after performance cooperation, coordinate with chitosan, sodium lignosulfonate, starch, further increase the antibacterial resistance to soiling of coating, improve the weathering resistance of coating.
Embodiment
In a particular embodiment, a kind of high-performance thermosetting polyester type powder paint that the present invention proposes, in its raw material, the weight part of pure polyester resin can be 40,42,43,45,46,48,49,49.3,51,52,53,54.6,55 parts; The weight part of fluorine-containing vibrin can be 3,4,4.3,5,5.3,6,6.3,7,7.4,8 parts; The weight part of epoxy resin can be 5,6,7,8,8.6,9,9.3,10,10.3,11,11.3,12,12.6,13,13.4,14,14.6,15 parts; The weight part of nbr carboxyl terminal can be 5,6,7,8,8.5,9,9.3,10,10.2,11,11.3,12,12.6,13,13.4,14,14.6,15 parts; N, N, N ', the weight part of N '-four (2-hydroxyethyl) adipamide can be 1,1.2,1.8,2,2.3,2.7,3,3.4,4,4.6,5 part; The weight part of four methoxy methyl glycoluril can be 2,3,4,5,5.6,6,6.3,7,7.4,8,8.6,9,9.4,10 parts; The weight part of isocyanuric acid three-glycidyl ester can be 1,1.2,1.8,3,3.4,3.8,4,4.5,4.8,5 part; The weight part of aminoresin can be 1,1.2,1.8,2,2.3,2.7,3,3.4,4,4.6,5 part; The weight part of 2-benzylimidazoline can be 1,1.2,1.58,1.6,2,2.3,2.7,3,3.4,3.8,4,4.2,4.8,5 part; The weight part of glyoxal ethyline can be 3,4,5,5.3,6,6.3,7,7.5,8,8.6,9,9.3,10 parts; The weight part of chitosan can be 1,1.2,1.8,2,2.3,2.8,3,3.4,4,4.6,5,5.3,6,6.3,7,7.4,8 part; The weight part of sodium lignosulfonate can be 1,1.2,1.8,2,2.3,2.6,3,3.4,3.8,4,4.6,5 part; The weight part of starch can be 2,2.3,2.8,3,3.4,3.8,4,4.2,4.75,5 parts; Poly weight part can be 2,2.3,2.8,3,3.4,4,4.2,4.8,5 parts; The weight part of polyvinyl butyral acetal can be 3,4,5,5.3,6,6.3,7,7.5,8,8.6,9,9.3,10 parts; The weight part of nano titanium oxide can be 5,6,7,7.5,8,8.6,9,9.3,10,10.6,11,11.3,12,12.6,13,13.4,14,14.6,15 parts; The weight part of aluminum oxide can be 2,3,4,4.6,5,5.3,6,6.3,7,7.4,8,8.6,9,9.4,10 parts; The weight part of zinc borate can be 1,1.2,1.8,2,2.3,3,3.4,4,4.6,5 part; The weight part of iron mica can be 2,3,4,4.5,5,5.6,6,6.3,7,7.8,8,8.6,9,9.4,10 parts; The weight part of polynite can be 1,1.2,1.6,2,2.3,3,3.4,4,4.6,5 part; The weight part of nanometer silver can be 2,3,4,4.5,5,5.6,6,6.3,7,7.4,8,8.6,9,9.4,10 parts; The weight part of activity charcoal powder can be 1,1.2,1.8,2,2.3,2.6,3,3.4,4,4.6,5 part; The weight part of lanthanum trioxide can be 2,2.3,2.8,3,3.4,4,4.6,6 parts; The weight part of auxiliary agent can be 1,1.2,1.8,2,2.6,3,3.4,4,4.6,5 part.
Below, by specific embodiment, technical scheme of the present invention is described in detail.
Embodiment 1
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: terminal carboxyl polyester resin 50 parts, 7.6 parts, fluorine-containing vibrin, epoxy resin 9 parts, nbr carboxyl terminal 11 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 4 parts, four methoxy methyl glycoluril 7 parts, isocyanuric acid three-glycidyl ester 3 parts, 3.6 parts, aminoresin, 2-benzylimidazoline 4 parts, glyoxal ethyline 7 parts, chitosan 6.5 parts, sodium lignosulfonate 3.8 parts, starch 4 parts, polyethylene 3.5 parts, polyvinyl butyral acetal 8.2 parts, nano titanium oxide 10 parts, 7 parts, aluminum oxide, zinc borate 3.8 parts, iron mica 6.5 parts, polynite 2.6 parts, nanometer silver 7 parts, activity charcoal powder 3.2 parts, lanthanum trioxide 5.3 parts, auxiliary agent 3 parts,
Wherein, the acid number of described terminal carboxyl polyester resin is 480mgKOH/g, and molecular weight is 4300, and second-order transition temperature is 61 DEG C; Described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 1:3:3;
Described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 32 parts of epoxy chloropropane and 2.5 parts of sodium hydroxide by weight, then 12 parts of hexafluoroisopropanols and 10 parts of Dimethylsilanediols are added, be warming up to 58 DEG C, reaction 4.6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 2 parts of cyclohexyl dimethanols, 10 parts of pyromellitic dianhydrides, 1.5 parts of Mono-n-butyltins, 38 parts of epoxy chloropropane and 40 parts of glycidyl ethers are added in 12 parts of dimethyl formamides and mix; then under the protection of nitrogen, 125 DEG C are warming up to; reaction 3.5h; 20 parts of acetone are added after reaction terminates; then the mixed solvent of 80 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:4; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Embodiment 2
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: hydroxyl telechelic polyester resin 52 parts, 7 parts, fluorine-containing vibrin, epoxy resin 10 parts, nbr carboxyl terminal 10 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 5 parts, four methoxy methyl glycoluril 6 parts, isocyanuric acid three-glycidyl ester 4 parts, 3 parts, aminoresin, 2-benzylimidazoline 4.5 parts, glyoxal ethyline 6 parts, chitosan 7 parts, sodium lignosulfonate 3 parts, starch 4.5 parts, polyethylene 3 parts, polyvinyl butyral acetal 9 parts, nano titanium oxide 8 parts, 8 parts, aluminum oxide, zinc borate 3 parts, iron mica 7 parts, polynite 2 parts, nanometer silver 9 parts, activity charcoal powder 2 parts, lanthanum trioxide 6 parts, auxiliary agent 2 parts,
Wherein, the molecular weight of described hydroxyl telechelic polyester resin is 5000, and second-order transition temperature is 62 DEG C; Described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 3:8:1;
Described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 25 parts of epoxy chloropropane and 3 parts of sodium hydroxide by weight, then 5 parts of hexafluoroisopropanols and 15 parts of Dimethylsilanediols are added, be warming up to 55 DEG C, reaction 6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 1 part of cyclohexyl dimethanol, 15 parts of pyromellitic dianhydrides, 1 part of Mono-n-butyltin, 45 parts of epoxy chloropropane and 25 parts of glycidyl ethers are added in 15 parts of dimethyl formamides and mix; then under the protection of nitrogen, 105 DEG C are warming up to; reaction 4h; 10 parts of acetone are added after reaction terminates; then the mixed solvent of 100 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:3; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Embodiment 3
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: terminal carboxyl polyester resin 25 parts, hydroxyl telechelic polyester resin 23 parts, 8 parts, fluorine-containing vibrin, epoxy resin 8 parts, nbr carboxyl terminal 12 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 3 parts, four methoxy methyl glycoluril 8 parts, isocyanuric acid three-glycidyl ester 2.5 parts, 4.5 parts, aminoresin, 2-benzylimidazoline 3 parts, glyoxal ethyline 9 parts, chitosan 5 parts, sodium lignosulfonate 4 parts, starch 3 parts, polyethylene 4 parts, polyvinyl butyral acetal 7 parts, nano titanium oxide 12 parts, 6 parts, aluminum oxide, zinc borate 4 parts, iron mica 6 parts, polynite 3 parts, nanometer silver 6 parts, activity charcoal powder 3.8 parts, lanthanum trioxide 4 parts, auxiliary agent 3.5 parts,
Wherein, the acid number of described terminal carboxyl polyester resin is 520mgKOH/g, and molecular weight is 3800, and second-order transition temperature is 62 DEG C; The molecular weight of described hydroxyl telechelic polyester resin is 4500, and second-order transition temperature is 63 DEG C; Described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 1:8:3;
Described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 35 parts of epoxy chloropropane and 2 parts of sodium hydroxide by weight, then 15 parts of hexafluoroisopropanols and 5 parts of Dimethylsilanediols are added, be warming up to 60 DEG C, reaction 4h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 3 parts of cyclohexyl dimethanols, 8 parts of pyromellitic dianhydrides, 2 parts of Mono-n-butyltins, 30 parts of epoxy chloropropane and 50 parts of glycidyl ethers are added in 8 parts of dimethyl formamides and mix; then under the protection of nitrogen, 130 DEG C are warming up to; reaction 2h; 25 parts of acetone are added after reaction terminates; then the mixed solvent of 50 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:5; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Embodiment 4
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: pure polyester resin 40 parts, 8 parts, fluorine-containing vibrin, epoxy resin 5 parts, nbr carboxyl terminal 15 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 1 part, four methoxy methyl glycoluril 10 parts, isocyanuric acid three-glycidyl ester 1 part, 5 parts, aminoresin, 2-benzylimidazoline 1 part, glyoxal ethyline 10 parts, chitosan 1 part, sodium lignosulfonate 5 parts, starch 2 parts, polyethylene 5 parts, polyvinyl butyral acetal 3 parts, nano titanium oxide 15 parts, 2 parts, aluminum oxide, zinc borate 5 parts, iron mica 2 parts, polynite 5 parts, nanometer silver 2 parts, activity charcoal powder 5 parts, lanthanum trioxide 2 parts, auxiliary agent 5 parts,
Wherein, described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 2:5:3;
Described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 28 parts of epoxy chloropropane and 2.3 parts of sodium hydroxide by weight, then 8 parts of hexafluoroisopropanols and 13 parts of Dimethylsilanediols are added, be warming up to 56 DEG C, reaction 5.5h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 1.5 parts of cyclohexyl dimethanols, 12 parts of pyromellitic dianhydrides, 1.6 parts of Mono-n-butyltins, 42 parts of epoxy chloropropane and 42 parts of glycidyl ethers are added in 13 parts of dimethyl formamides and mix; then under the protection of nitrogen, 122 DEG C are warming up to; reaction 3.3h; 17 parts of acetone are added after reaction terminates; then the mixed solvent of 78 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:3.8; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Embodiment 5
A kind of high-performance thermosetting polyester type powder paint that the present invention proposes, its raw material comprises following component by weight: terminal carboxyl polyester resin 32 parts, hydroxyl telechelic polyester resin 23 parts, 3 parts, fluorine-containing vibrin, epoxy resin 15 parts, nbr carboxyl terminal 5 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 5 parts, four methoxy methyl glycoluril 2 parts, isocyanuric acid three-glycidyl ester 5 parts, 1 part, aminoresin, 2-benzylimidazoline 5 parts, glyoxal ethyline 3 parts, chitosan 8 parts, sodium lignosulfonate 1 part, starch 5 parts, polyethylene 2 parts, polyvinyl butyral acetal 10 parts, nano titanium oxide 5 parts, 10 parts, aluminum oxide, zinc borate 1 part, iron mica 10 parts, polynite 1 part, nanometer silver 10 parts, activity charcoal powder 1 part, lanthanum trioxide 6 parts, auxiliary agent 1 part,
Wherein, the acid number of described terminal carboxyl polyester resin is 550mgKOH/g, and molecular weight is 3000, and second-order transition temperature is 65 DEG C; The molecular weight of described hydroxyl telechelic polyester resin is 4000, and second-order transition temperature is 65 DEG C; Described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 3:6:1;
Described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 33 parts of epoxy chloropropane and 2.6 parts of sodium hydroxide by weight, then 12 parts of hexafluoroisopropanols and 9 parts of Dimethylsilanediols are added, be warming up to 58 DEG C, reaction 4.6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 2.4 parts of cyclohexyl dimethanols, 9 parts of pyromellitic dianhydrides, 1.3 parts of Mono-n-butyltins, 38 parts of epoxy chloropropane and 29 parts of glycidyl ethers are added in 9 parts of dimethyl formamides and mix; then under the protection of nitrogen, 109 DEG C are warming up to; reaction 3.8h; 12 parts of acetone are added after reaction terminates; then the mixed solvent of 66 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:4.5; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
Its outward appearance of high-performance thermosetting polyester type powder paint described in embodiment 1-5 is loose without caking, uniform color, and density is 1.5-1.6g/cm
3; Horizontal melt fluidity is 26-30mm; Fineness of powder 180 screen residue < 0.5%; Room temperature 3 years stable storings, 10-15min solidification at 195-205 DEG C.
Carry out Performance Detection by after high-performance thermosetting polyester type powder paint solidification described in embodiment 1-5 to film, result is as shown in the table:
| Test item | Performance perameter |
| Outward appearance | Smoothly |
| Gloss (60 ° of gauge outfits) | 15-80％ |
| Shock-resistance (weighted-drop) | By 50kg.cm (4.9Nm) |
| Drawing test | ＞5mm |
| Penetration hardness | By 4kg (39N) |
| Pliability test (tap web axle) | Pass through 3mm |
| Cross Hatch sticking power | 100% attachment |
| Surface hardness | 2-3H |
| Salt-fog test | Pass through 1000h |
| Wet fastness | Pass through 1000h |
| Water immersion test | Pass through 240h |
| Uvioresistant is tested | Splendid |
| The washing composition of resistance to boiling is tested | 24h is unchanged |
| Be exposed to the sun test in outdoor | 12 months good, without powder phenomenon-tion |
| Acid resistance (5%HCl) | Pass through 300h |
| Alkali resistance (5%NaOH) | Pass through 300h |
| Petrol-resistance (120 #Gasoline) | Pass through 300h |
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (10)
1. a high-performance thermosetting polyester type powder paint, it is characterized in that, its raw material comprises following component by weight: pure polyester resin 40-55 part, fluorine-containing vibrin 3-8 part, epoxy resin 5-15 part, nbr carboxyl terminal 5-15 part, N, N, N ', N '-four (2-hydroxyethyl) adipamide 1-5 part, four methoxy methyl glycoluril 2-10 parts, isocyanuric acid three-glycidyl ester 1-5 part, aminoresin 1-5 part, 2-benzylimidazoline 1-5 part, glyoxal ethyline 3-10 part, chitosan 1-8 part, sodium lignosulfonate 1-5 part, starch 2-5 part, polyethylene 2-5 part, polyvinyl butyral acetal 3-10 part, nano titanium oxide 5-15 part, aluminum oxide 2-10 part, zinc borate 1-5 part, iron mica 2-10 part, polynite 1-5 part, nanometer silver 2-10 part, activity charcoal powder 1-5 part, lanthanum trioxide 2-6 part, auxiliary agent 1-5 part.
2. high-performance thermosetting polyester type powder paint according to claim 1, it is characterized in that, in its raw material, the weight ratio of pure polyester resin, fluorine-containing vibrin, epoxy resin, nbr carboxyl terminal is 45-53:5-8:6-12:7-13.
3. high-performance thermosetting polyester type powder paint according to claim 1 or 2, it is characterized in that, its raw material comprises following component by weight: pure polyester resin 48-52 part, fluorine-containing vibrin 7-8 part, epoxy resin 8-10 part, nbr carboxyl terminal 10-12 part, N, N, N ', N '-four (2-hydroxyethyl) adipamide 3-5 part, four methoxy methyl glycoluril 6-8 parts, isocyanuric acid three-glycidyl ester 2.5-4 part, aminoresin 3-4.5 part, 2-benzylimidazoline 3-4.5 part, glyoxal ethyline 6-9 part, chitosan 5-7 part, sodium lignosulfonate 3-4 part, starch 3-4.5 part, polyethylene 3-4 part, polyvinyl butyral acetal 7-9 part, nano titanium oxide 8-12 part, aluminum oxide 6-8 part, zinc borate 3-4 part, iron mica 6-7 part, polynite 2-3 part, nanometer silver 6-9 part, activity charcoal powder 2-3.8 part, lanthanum trioxide 4-6 part, auxiliary agent 2-3.5 part.
4. high-performance thermosetting polyester type powder paint according to any one of claim 1-3, it is characterized in that, its raw material comprises following component by weight: pure polyester resin 50 parts, 7.6 parts, fluorine-containing vibrin, epoxy resin 9 parts, nbr carboxyl terminal 11 parts, N, N, N ', N '-four (2-hydroxyethyl) adipamide 4 parts, four methoxy methyl glycoluril 7 parts, isocyanuric acid three-glycidyl ester 3 parts, 3.6 parts, aminoresin, 2-benzylimidazoline 4 parts, glyoxal ethyline 7 parts, chitosan 6.5 parts, sodium lignosulfonate 3.8 parts, starch 4 parts, polyethylene 3.5 parts, polyvinyl butyral acetal 8.2 parts, nano titanium oxide 10 parts, 7 parts, aluminum oxide, zinc borate 3.8 parts, iron mica 6.5 parts, polynite 2.6 parts, nanometer silver 7 parts, activity charcoal powder 3.2 parts, lanthanum trioxide 5.3 parts, auxiliary agent 3 parts.
5. high-performance thermosetting polyester type powder paint according to any one of claim 1-4, is characterized in that, described pure polyester resin is the combination of a kind of in terminal carboxyl polyester resin and hydroxyl telechelic polyester resin or two kinds.
6. high-performance thermosetting polyester type powder paint according to claim 5, it is characterized in that, the acid number of described terminal carboxyl polyester resin is 400-550mgKOH/g, and molecular weight is 3000-5000, and second-order transition temperature is 60-65 DEG C; The molecular weight of described hydroxyl telechelic polyester resin is 4000-5500, and second-order transition temperature is 60-65 DEG C.
7. high-performance thermosetting polyester type powder paint according to any one of claim 1-6, it is characterized in that, described epoxy resin is that hydrogenated bisphenol A epoxy resin, tetraphenolethane epoxy resin, bisphenol-s epoxy resin are by weight the combination for 1-3:3-8:1-3.
8. high-performance thermosetting polyester type powder paint according to any one of claim 1-7, it is characterized in that, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by epoxy chloropropane and sodium hydroxide, then hexafluoroisopropanol and Dimethylsilanediol is added, be warming up to 55-60 DEG C, reaction 4-6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; Cyclohexyl dimethanol, pyromellitic dianhydride, Mono-n-butyltin, epoxy chloropropane and glycidyl ether are added in dimethyl formamide and mixes; then under the protection of nitrogen, 105-130 DEG C is warming up to; reaction 2-4h; acetone is added after reaction terminates; then the mixed solvent of second alcohol and water is added; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
9. high-performance thermosetting polyester type powder paint according to any one of claim 1-8, it is characterized in that, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 25-35 part epoxy chloropropane and 2-3 part sodium hydroxide by weight, then 5-15 part hexafluoroisopropanol and 5-15 part Dimethylsilanediol is added, be warming up to 55-60 DEG C, reaction 4-6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates, by weight by 1-3 part cyclohexyl dimethanol, 8-15 part pyromellitic dianhydride, 1-2 part Mono-n-butyltin, 30-45 part epoxy chloropropane and 25-50 part glycidyl ether add in 8-15 part dimethyl formamide and mix, then under the protection of nitrogen, 105-130 DEG C is warming up to, reaction 2-4h, 10-25 part acetone is added after reaction terminates, then the mixed solvent of 50-100 part second alcohol and water is added, in the mixed solvent of wherein second alcohol and water, the ratio of the volume of second alcohol and water is 1:3-5, leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
10. high-performance thermosetting polyester type powder paint according to any one of claim 1-9, it is characterized in that, described fluorine-containing vibrin is prepared according to following technique: add in reaction unit by 32 parts of epoxy chloropropane and 2.5 parts of sodium hydroxide by weight, then 12 parts of hexafluoroisopropanols and 10 parts of Dimethylsilanediols are added, be warming up to 58 DEG C, reaction 4.6h, obtains glycidyl ether through filtration, underpressure distillation after reaction terminates; By weight 2 parts of cyclohexyl dimethanols, 10 parts of pyromellitic dianhydrides, 1.5 parts of Mono-n-butyltins, 38 parts of epoxy chloropropane and 40 parts of glycidyl ethers are added in 12 parts of dimethyl formamides and mix; then under the protection of nitrogen, 125 DEG C are warming up to; reaction 3.5h; 20 parts of acetone are added after reaction terminates; then the mixed solvent of 80 parts of second alcohol and waters is added; in the mixed solvent of wherein second alcohol and water; the ratio of the volume of second alcohol and water is 1:4; leave standstill after stirring, after filtration, washing, drying obtains described fluorine-containing vibrin.
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| CN106750222A (en) * | 2016-11-30 | 2017-05-31 | 安徽神剑新材料股份有限公司 | A kind of extra-weather-proof fluorine-containing polyester resin of end carboxyl used for powder coating and preparation method thereof |
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| CN106750222A (en) * | 2016-11-30 | 2017-05-31 | 安徽神剑新材料股份有限公司 | A kind of extra-weather-proof fluorine-containing polyester resin of end carboxyl used for powder coating and preparation method thereof |
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| CN111138970A (en) * | 2019-12-23 | 2020-05-12 | 江阴市玲珑高分子材料有限公司 | Thermosetting powder coating |
| CN112574634A (en) * | 2020-11-19 | 2021-03-30 | 宁波爱甬新材料科技有限公司 | Fast-curing powder coating and preparation method thereof |
| CN112574634B (en) * | 2020-11-19 | 2022-08-09 | 宁波爱甬新材料科技有限公司 | Fast-curing powder coating and preparation method thereof |
| CN117165168A (en) * | 2023-08-16 | 2023-12-05 | 云南领克新型材料有限公司 | Nanometer self-cleaning powder coating and preparation method thereof |
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