CN1710000A - Low-temperature solidified polyester surface paint for procoating metal coiled material and its preparing method - Google Patents
Low-temperature solidified polyester surface paint for procoating metal coiled material and its preparing method Download PDFInfo
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Abstract
The invention relates to polyester resin dope technological field, especially a kind of low temperature solidifying polyester surface lacquer used for pre-smearing of metal convolving material and its producing method. It makes high activeness linear polyester resin modified from glycidyl ester of of versatic acid as membrane forming resin, and amino resin as modification agent, then match with pigment plasm, auxiliary agent and mixed solvent to produce. The finished weight solid shares are 40-80%, and smear 4 cups at 23 Deg. C, its viscosity is 30-200 seconds. It can be solidified to membrane in 30 - 60 seconds at 200 - 216 Deg. C of baseplate temperature. The dope of the invention can reduce the baseplate temperature of solidifying paint membrane (PMT) by 25 Deg. C, and the drying tunnel temperature reduces 50 - 80 Deg. C. It decreases energy waste, reduces the production cost of pre-smearing convolving material.
Description
Technical field
The present invention relates to the Polyester resin lacquer technical field, especially a kind of low-temperature solidified polyester surface paint for procoating metal coiled material and preparation method thereof.
Background technology
The precoating metal coiled material is a continuous coating organic coating and through high temperature rapid curing on the metal original tape of advancing, a kind of organic materials/metallic composite panel of making.Nineteen thirty-five Joe Hunter has built up the thick 0.2mm of article one application in the world in the U.S., the precoating metal winding production line of wide 50mm steel band.After World War II finishes, the precoating metal coiled material obtains very big development as light-duty, cheap material of construction, simultaneously along with economic recovery and progress of science and technology after the war, good material and technical foundation is provided for again the development of precoating metal coiled material, be starting point the 1950's with the U.S., begun precoating metal coiled material fast-developing period, become an emerging industry very soon in American-European developed country.The maximum purposes of precoating metal coiled material is as material of construction, and its consumption accounts for the over half of precoating metal coiled material ultimate production.It cooperates with light-weight steel cage structure, is suitable for building exterior wall wooden handcart, curtain wall, roof boarding, indoor partition wall, rolling screen door, garage door and the mat shelter etc. of industrial premises, public utility, single-family dwelling, station, booth etc.Except that building materials, the inside fitting from the shell of vehicle, liner to boats and ships; From household appliances shell to culinary frying pan and baking tray; To various package packing supplies, it can both provide of all kinds, colourful product for people from art metal furniture.
Late 1920s Kienle reacts with glycerine and phthalic anhydride and has synthesized Synolac the earliest with the unsaturated fatty acids modification.Carothers has started the research and development of vibrin with the research of the synthetic line polymer of hexylene glycol terephthalic acid afterwards.Nineteen forty-one Whenfielt Dikson has made the trevira with practical value.Expiring the beginning of the sixties just occurs coating vibrin and polyester coating, and becomes the main body of pre-coated coil with coating very soon.The coating of using because of the precoating metal coiled material must satisfy its production technique and process the requirement of using two aspects, requirement from production technique, have fast forward, roller coat applies, high temperature, short time baking and the sharply characteristics of cooling of back of coming out of the stove, from requirement to paint film property, finish paint should have good opacifying power and ornamental, and identical product gloss relative error should be not more than 0.5%, aberration Δ E＜1, to have good toughness and hardness simultaneously, to satisfy processing and service requirements.Therefore Polyester resin lacquer is a topmost kind in the at present pre-coating.Have the well balanced of snappiness and hardness through amino resin crosslinked paint film, and other good over-all properties.Coating is mainly formed through the esterification condensation by diprotic acid (comprising aromatic acid, aliphatic dibasic acid and alicyclic diprotic acid) and polyvalent alcohol (mainly being the pure and mild alicyclic dibasic alcohol of binary aliphatic) with vibrin.By selecting the kind of raw material acid and raw alcohol, can synthesize the different vibrin of performance, and then prepare and satisfy the coating that different use propertieies require.The Ministry of Chemical Industry's coatings industry institute and the Shanghai magnificent coating factory of shaking successfully develops and introduces pre-coated coil respectively with amino curing polyester finish paint in the eighties in last century.Along with the development of pre-coated coil industry, a lot of coating producer releases one after another multiple pre-coated coil with amino curing polyester finish paint.
Coating is coated on the metal sheet continuously through the high temperature rapid curing film forming, is one of production characteristics of precoating metal coiled material.The energy that high bake consumed occupies sizable ratio in the running cost of producing.Along with the fast development of China's pre-coated coil industry, the energy total amount that it consumed is also considerable in recent years.At present pre-coated coil with the condition of cure of amino curing polyester finish paint all 220～240 ℃ or higher/30～90 second.The pre-coated coil vibrin that a kind of condition of cure is 200～260 ℃/20～90 seconds a reduced solidification value is disclosed as China patent of invention CN1473898A, United States Patent (USP) 4140727 and 4229555 all is to solidify the linear polyester finish paint about pre-coated coil with amino, and condition of cure is 240～260 ℃/40 seconds.Paint film generally needs 224～241 ℃ of following baking-curings of roll bending temperature on the coil production line at present, and oven drying temperature is generally at 350～450 ℃, thereby a large amount of heat energy of needs, is example with 30 meters long electric ovens, and under 60 meters/minute of belt speed, per hour power consumption 1200 is spent.If can reduce the film curing temperature, then be significant saving the energy and reducing production costs.
Summary of the invention
Be to save the energy and reduce the pre-coated coil production cost, the purpose of this invention is to provide a kind of can be at 200～216 ℃ of substrate temperatures, the low-temperature solidified polyester surface paint for procoating metal coiled material of 30～60 seconds film-formings.
The technical solution adopted for the present invention to solve the technical problems is: a kind of low-temperature solidified polyester surface paint for procoating metal coiled material, high reactivity linear polyester resin by the tertiary carbonic acid glycidyl ester modification is that film-forming resin and aminoresin are solidifying agent, being equipped with pigment slurry, auxiliary agent, mixed solvent again makes, finished weight solid part 40%～80%, 23 ℃ are coated with 4 glasss of viscositys is 30～200 seconds, can be 200～216 ℃ of substrate temperatures, 30～60 seconds film-formings.
Further: in the described low-temperature solidified polyester surface paint for procoating metal coiled material finished product each component by weight hundred parts of content be respectively: through the high reactivity linear polyester resin 10%～50% of tertiary carbonic acid glycidyl ester modification, aminoresin 5%～20%, pigment slurry 20%～60%, auxiliary agent 0.1%～5.0%, all the other are mixed solvent.
Further: the high reactivity linear polyester resin of described tertiary carbonic acid glycidyl ester modification, it is the linear polyester resin that in the presence of catalyzer and thermo-stabilizer, makes by a kind of tertiary carbonic acid glycidyl ester, at least a dibasic alcohol and at least a aromatic acid and at least a aliphatic dibasic acid through esterification, its acid number is 0.1～10mgKOH/ gram, hydroxyl value 10～80mgKOH/ gram.
Further: described aminoresin is the urea-formaldehyde resin of methyl or methyl butyl etherificate or the terpolycyantoamino-formaldehyde resin of methyl or methyl butyl etherificate.
Further: described pigment slurry for through the high reactivity linear polyester resin of tertiary carbonic acid glycidyl ester modification and pigment by solid weight than 10: 1～1: 5, add less than the auxiliary agent of resin and total pigment weight 10% and mixed solvent and be dispersed to fineness≤15 micron through grinding, described pigment is mineral dye or pigment dyestuff, as titanium pigment, phthualocyanine pigment, chrome yellow series pigments, inorganic compounding pigment, carbon black pigment.
Further: described mixed solvent is made up of aromatic hydrocarbon solvent, ketones solvent, pure ether solvent, two esters solvents, and weight percentage aromatic hydrocarbon solvent 30%～80%, ketones solvent 0%～40%, pure ether solvent 0%～50%, two esters solvents 5%～40%.
Further: described auxiliary agent is high molecular polyurethane-modified acrylic acid class pigment dispersing agent, aerosil class anti-settling agent, polyacrylic ester defoamer, fluorine modified polyacrylate class flow agent, tosic acid class curing catalysts.
Further: described tertiary carbonic acid glycidyl ester is C
8-C
14Glycidyl ester; Described aliphatic dihydroxy alcohol is ethylene glycol, glycol ether, propylene glycol, methyl propanediol, neopentyl glycol, 2,2-methyl butyl neopentyl glycol; Described alicyclic dibasic alcohol is the cyclohexyl dimethanol; Described aromatic acid is Tetra hydro Phthalic anhydride, dimethyl terephthalate (DMT), phthalic acid, m-phthalic acid; Described aliphatic dibasic acid is hexanodioic acid, nonane diacid, sebacic acid; Described alicyclic diprotic acid is the cyclohexyl dioctyl phthalate.
More enter～go on foot ground: described aromatic hydrocarbon solvent is dimethylbenzene, S-100, S-150; Described ketones solvent is pimelinketone, mibk or diacetone alcohol; Described pure ether solvent is propylene glycol monomethyl ether, propylene glycol butyl ether or ethylene glycol ethyl ether amyl acetate; Described two esters solvents are diethyl oxalate, Ethanedioic acid, dipropyl ester, ethylene sebacate or its combination, dimethyl succinate, Methyl glutarate, dimethyl adipate or its combination.
The preparation method of above-mentioned low-temperature solidified polyester surface paint for procoating metal coiled material has following processing step:
A. the high reactivity linear polyester resin of tertiary carbonic acid glycidyl ester modification is synthetic,
Tertiary carbonic acid glycidyl ester with weight percentage 10-30%, the m-phthalic acid of 20-50%, the hexanodioic acid of 5-15%, the methyl propanediol of 25-40%, the organotin catalysts of 0.03-0.05%, triphenyl phosphite stablizer and the refluxing xylene solvent of 0.05-0.08% are put in the reaction kettle of the esterification, filling material in the vertical tube jacket condensator of this device, thermometer is equipped with at the top, under protection of inert gas, slowly be warmed up to 210 ℃～220 ℃, under this temperature, continue reaction then, controlling the vertical tube condenser overhead simultaneously steams the thing temperature and is no more than 101 ℃, steam the thing temperature until the top and reduce to 80 ℃, and reactant becomes limpid and acid number is reduced to 0.1～10mgKOH/ gram, cooling, add the latting drown mixed solvent, filter discharging;
B. pigment slurry preparation,
The high reactivity linear polyester resin of the tertiary carbonic acid glycidyl ester modification of weight percentage 20-60%, the pigment of 30-65%, the dispersing auxiliary of 0.5-2%, the mixed solvent of 5-10% are dropped into premix in the premix cylinder, again premix slurry is dispersed to fineness≤15 micron through grinding plant, filters discharging;
C. low-temperature curing polyester finish coat preparation,
Hundred parts of content are respectively by weight: 10%～50% the high reactivity linear polyester resin through the tertiary carbonic acid glycidyl ester modification, 5%～20% aminoresin, 20%～60% pigment slurry, 0.1%～5.0% auxiliary agent, mixed solvent surplus thorough mixing in paint mixing tank is even, discharging, packing.
The invention has the beneficial effects as follows, low-temperature solidified polyester surface paint for procoating metal coiled material of the present invention, satisfy under the prerequisite of the every technical indicator of coil in assurance, can make the substrate temperature (PMT) of film curing reduce about 25 ℃, 50～80 ℃ of the corresponding reductions of drying tunnel temperature.Reduce energy consumption, reduced the production cost of pre-coated coil, had good economic benefits and social benefit.
Embodiment
A kind of low-temperature solidified polyester surface paint for procoating metal coiled material, by high reactivity linear polyester resin 10%～50% and aminoresin 5%～20% through the tertiary carbonic acid glycidyl ester modification is solidifying agent, being equipped with pigment slurry 20%～60%, auxiliary agent 0.1%～5.0%, mixed solvent surplus again makes, finished weight solid part 40%～80%, 23 ℃ are coated with 4 glasss of viscositys is 30～200 seconds, can be 200～216 ℃ of substrate temperatures, 30～60 seconds film-formings.
Described high reactivity lienar for vibrin through the tertiary carbonic acid glycidyl ester modification, it is the linear polyester resin that in the presence of catalyzer and thermo-stabilizer, makes by a kind of tertiary carbonic acid glycidyl ester, at least a dibasic alcohol and at least a aromatic acid and at least a aliphatic dibasic acid through esterification, its acid number is 0.1～10mgKOH/ gram, hydroxyl value 10～80mgKOH/ gram.
Described aminoresin is the urea-formaldehyde resin of methyl or methyl butyl etherificate or the terpolycyantoamino-formaldehyde resin of methyl or methyl butyl etherificate.
Described pigment slurry be the tertiary carbonic acid glycidyl ester modification high reactivity lienar for vibrin and pigment by solid weight than 10: 1～1: 5, add less than the auxiliary agent of resin and total pigment weight 10% and mixed solvent and be dispersed to fineness≤15 micron through grinding, described pigment is mineral dye or pigment dyestuff, as titanium pigment, phthualocyanine pigment, chrome yellow series pigments, inorganic compounding pigment, carbon black pigment.
Described mixed solvent is made up of aromatic hydrocarbon solvent, ketones solvent, pure ether solvent, two esters solvents, and weight percentage aromatic hydrocarbon solvent 30%～80%, ketones solvent 0%～40%, pure ether solvent 0%～50%, two esters solvents 5%～40%.
Described auxiliary agent is high molecular polyurethane-modified acrylic acid class pigment dispersing agent, aerosil class anti-settling agent, polyacrylic ester defoamer, fluorine modified polyacrylate class flow agent, tosic acid class curing catalysts.
Described tertiary carbonic acid glycidyl ester is C
8-C
14Glycidyl ester; Described aliphatic dihydroxy alcohol is ethylene glycol, glycol ether, propylene glycol, methyl propanediol, neopentyl glycol, 2,2-methyl butyl neopentyl glycol; Described alicyclic dibasic alcohol is the cyclohexyl dimethanol; Described aromatic acid is Tetra hydro Phthalic anhydride, dimethyl terephthalate (DMT), phthalic acid, m-phthalic acid; Described aliphatic dibasic acid is hexanodioic acid, nonane diacid, sebacic acid; Described alicyclic diprotic acid is the cyclohexyl dioctyl phthalate.
Described aromatic hydrocarbon solvent is dimethylbenzene, S-100, S-150; Described ketones solvent is pimelinketone, mibk or diacetone alcohol; Described pure ether solvent is propylene glycol monomethyl ether, propylene glycol butyl ether or ethylene glycol ethyl ether amyl acetate; Described two esters solvents are diethyl oxalate, Ethanedioic acid, dipropyl ester, ethylene sebacate or its combination, dimethyl succinate, Methyl glutarate, dimethyl adipate or its combination.
A kind of preparation method of low-temperature solidified polyester surface paint for procoating metal coiled material has following processing step:
A. the high reactivity linear polyester resin of tertiary carbonic acid glycidyl ester modification is synthetic,
With 97.7 weight part tertiary carbonic acid glycidyl esters, 252.0 weight part m-phthalic acid, 73.9 weight part hexanodioic acid, 154.3 weight part methyl propanediol, 0.3 weight part organotin esterifying catalyst, 0.5 weight part triphenyl phosphite thermo-stabilizer and 25.0 weight part refluxing xylene solvents are put into thermometer are housed, agitator, the vertical tube condenser of thermometer band filler and chuck is equipped with at the top, in the reactor of condensation reflux unit, under protection of inert gas, slowly be warmed up to 210 ℃～220 ℃, under this temperature, continue reaction then, controlling the vertical tube condenser overhead simultaneously steams the thing temperature and is no more than 101 ℃, steam the thing temperature until the top and reduce to 80 ℃, and reactant becomes limpid and acid number is reduced to processing requirement, be cooled to 110 ℃, add 336.6 weight part latting drown mixed solvents, filter discharging, obtain the weight solids content and be 60% polyester resin solution;
B. pigment slurry preparation,
The high reactivity linear polyester resin of the above-mentioned tertiary carbonic acid glycidyl ester modification of 100.0 weight parts, the titanium white powder pigment of 120.0 weight parts, the dispersing auxiliary of 3.0 weight parts, the mixed solvent of 20.0 weight parts are dropped into premix in the premix cylinder, again premix slurry is dispersed to fineness≤15 micron through grinding plant, filter discharging, pigment slurry solid part is 75%;
C. low-temperature curing polyester finish coat preparation,
With the above-mentioned mill base of 100 weight parts, the high reactivity linear polyester resin through the tertiary carbonic acid glycidyl ester modification of 25.0 weight parts, the aminoresin of 10.2 weight parts, 1.6 the tosic acid class catalyzer of weight part, 1.0 the flow agent of weight part, the defoamer of 0.2 weight part, the mixed solvent of 4.8 weight parts joins in the paint mixing tank respectively, thorough mixing is even, filter, packing makes low-temperature solidified polyester surface paint for procoating metal coiled material, its solid part is 70%, 23 ℃, and to be coated with 4 glasss of viscositys be 95 seconds.
D. low-temperature curing polyester finish coat service check
Scribbling on the galvanized sheet of epoxy primer, with the low-temperature curing polyester finish coat among No. 60 coiling scraper coating embodiment, 260 ℃ of oven temperatures, storing time 30 seconds, 204 ℃ of substrate temperatures (PMT).The gained coating dry film is thick to be 25 microns, and the visual inspection flat appearance is smooth.Pressing national standard method detects.T is curved: 2T; Impact: 100cm, pencil hardness 2H, cupping: 6.5mm; Anti-MEK wiping: 〉=100 times.
The result shows that this low-temperature curing polyester finish coat can solidify under lower substrate temperature, performance satisfies the requirement of precoating metal coiled material with polyester finish coat fully.
Claims (10)
1, a kind of low-temperature solidified polyester surface paint for procoating metal coiled material, it is characterized in that: the high reactivity linear polyester resin by the tertiary carbonic acid glycidyl ester modification is a film-forming resin, aminoresin is solidifying agent, being equipped with pigment slurry, auxiliary agent, mixed solvent again makes, finished weight solid part 40%～80%, 23 ℃ are coated with 4 glasss of viscositys is 30～200 seconds, can be 200～216 ℃ of substrate temperatures, and 30～60 seconds film-formings.
2, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1, it is characterized in that: in the finished product each component by weight hundred parts of content be respectively: through the high reactivity linear polyester resin 10%～50% of tertiary carbonic acid glycidyl ester modification, aminoresin 5%～20%, pigment slurry 20%～60%, auxiliary agent 0.1%～5.0%, all the other are mixed solvent.
3, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1, it is characterized in that: described high reactivity lienar for vibrin through the tertiary carbonic acid glycidyl ester modification, it is the linear polyester resin that in the presence of catalyzer and thermo-stabilizer, makes by a kind of tertiary carbonic acid glycidyl ester, at least a dibasic alcohol and at least a aromatic acid and at least a aliphatic dibasic acid through esterification, its acid number is 0.1～10mgKOH/ gram, hydroxyl value 10～80mgKOH/ gram.
4, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1 is characterized in that: described aminoresin is the urea-formaldehyde resin of methyl or methyl butyl etherificate or the melamine-formaldehyde resin of methyl or methyl butyl etherificate.
5, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1, it is characterized in that: described pigment slurry for through the high reactivity lienar for vibrin of tertiary carbonic acid glycidyl ester modification and pigment by solid weight than 10: 1～1: 5, add less than the auxiliary agent of resin and total pigment weight 10% and mixed solvent and be dispersed to fineness≤15 micron through grinding, described pigment is mineral dye or pigment dyestuff, as titanium pigment, phthualocyanine pigment, chrome yellow series pigments, inorganic compounding pigment, carbon black pigment.
6, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1, it is characterized in that: described mixed solvent is made up of aromatic hydrocarbon solvent, ketones solvent, pure ether solvent, two esters solvents, and weight percentage aromatic hydrocarbon solvent 30%～80%, ketones solvent 0%～40%, pure ether solvent 0%～50%, two esters solvent 5%-40%.
7, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 1 is characterized in that: described auxiliary agent is high molecular polyurethane-modified acrylic acid class pigment dispersing agent, aerosil class anti-settling agent, polyacrylic ester defoamer, fluorine modified polyacrylate class flow agent, tosic acid class curing catalysts.
8, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 3 is characterized in that: described tertiary carbonic acid glycidyl ester is C
8-C
14Glycidyl ester; Described aliphatic dihydroxy alcohol is ethylene glycol, glycol ether, propylene glycol, 2-methyl propanediol, neopentyl glycol, 2,2-methyl butyl neopentyl glycol; Described alicyclic dibasic alcohol is the cyclohexyl dimethanol; Described aromatic acid is Tetra hydro Phthalic anhydride, dimethyl terephthalate (DMT), phthalic acid, m-phthalic acid; Described aliphatic dibasic acid is hexanodioic acid, nonane diacid, sebacic acid; Described alicyclic diprotic acid is the cyclohexyl dioctyl phthalate.
9, low-temperature solidified polyester surface paint for procoating metal coiled material according to claim 6 is characterized in that: described aromatic hydrocarbon solvent is dimethylbenzene, S-100, S-150; Described ketones solvent is pimelinketone, mibk or diacetone alcohol; Described pure ether solvent is propylene glycol monomethyl ether, propylene glycol butyl ether or ethylene glycol ethyl ether amyl acetate; Described two esters solvents are diethyl oxalate, Ethanedioic acid, dipropyl ester, ethylene sebacate or its combination, dimethyl succinate, Methyl glutarate, dimethyl adipate or its combination.
10, a kind of preparation method of low-temperature solidified polyester surface paint for procoating metal coiled material is characterized in that having following processing step:
A. the high reactivity linear polyester resin of tertiary carbonic acid glycidyl ester modification is synthetic,
Tertiary carbonic acid glycidyl ester with weight percentage 10-30%, the m-phthalic acid of 20-50%, the hexanodioic acid of 5-15%, the methyl propanediol of 25-40%, the organotin catalysts of 0.03-0.05%, triphenyl phosphite stablizer and the refluxing xylene solvent of 0.05-0.08% are put in the reaction kettle of the esterification, filling material in the vertical tube jacket condensator of this device, thermometer is equipped with at the top, under protection of inert gas, slowly be warmed up to 210 ℃～220 ℃, under this temperature, continue reaction then, controlling the vertical tube condenser overhead simultaneously steams the thing temperature and is no more than 101 ℃, steam the thing temperature until the top and reduce to 80 ℃, and reactant becomes limpid and acid number is reduced to 0.1～10mgKOH/ gram, cooling, add the latting drown mixed solvent, filter discharging;
B. pigment slurry preparation,
The high reactivity linear polyester resin of the tertiary carbonic acid glycidyl ester modification of weight percentage 20-60%, the pigment of 30-65%, the dispersing auxiliary of 0.5-2%, the mixed solvent of 5-10% are dropped into premix in the premix cylinder, again premix slurry is dispersed to fineness≤15 micron through grinding plant, filters discharging;
C. low-temperature curing polyester finish coat preparation,
Hundred parts of content are respectively by weight: 10%～50% the high reactivity linear polyester resin through the tertiary carbonic acid glycidyl ester modification, 5%～20% aminoresin, 20%～60% pigment slurry, 0.1%～5.0% auxiliary agent, mixed solvent surplus thorough mixing in paint mixing tank is even, discharging, packing.
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| CNB2005100408562A CN1330719C (en) | 2005-07-01 | 2005-07-01 | Low-temperature solidified polyester surface paint for procoating metal coiled material and its preparing method |
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| JPH02142869A (en) * | 1988-11-22 | 1990-05-31 | Toray Ind Inc | Coating composition for coated steel sheet |
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| CN101735712A (en) * | 2008-11-21 | 2010-06-16 | 上海振华造漆厂 | Coating for anti-camouflage virid coils and preparation method and application thereof |
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