CN102925042A - Preparation method of high-weather-resistant low-temperature-curing environment-friendly cation coating - Google Patents
Preparation method of high-weather-resistant low-temperature-curing environment-friendly cation coating Download PDFInfo
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Abstract
The invention discloses a preparation method of a high-weather-resistant low-temperature-curing environment-friendly cation coating. The method comprises the following steps of: preparing a cation coating emulsion; and preparing cation coating color paste. The high-weather-resistant low-temperature-curing environment-friendly cation coating produced with the method can be taken as a cation coating for finishing coat, and has high weather resistance and low curing temperature; and moreover, a coating system is free from lead and tin, has high stability, is corrosion-resistant, can be taken as a base-finishing coat, and has the advantages of optimization of a process, saving in cost and meeting of the requirement of environment protection through low VOC (Volatile Organic Compounds) emission.
Description
Technical field
The present invention relates to a kind of cation paint, be specifically related to a kind of preparation method of high weather-proof low temperature solidifying environment protection type cation paint.
Background technology
Cathode electrophoresis dope uses as automobile industry coating priming paint, can increase substantially its corrosion resistance nature, has improved the particularly market competitiveness of commercial car of domestic automobile industry.Because the development in market, the competition of industry is more and more fierce, in order to satisfy the demand of quality product, environmental protection and cost aspect that automobile and other industries improves constantly, suitability, diversified cathode electrophoresis dope are also with regard to corresponding appearance, wherein the environment protection type cathode electrophoresis coating of high-weatherability, low-temperature curing, unleaded Wuxi and low VOC discharging has become one of direction of the sector development and application, deeply is subjected to the sector personnel's attention.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of high weather-proof low temperature solidifying environment protection type cation paint satisfies the demand of quality product, environmental protection and cost aspect that automobile and other industries improves constantly.
The technical solution used in the present invention is as follows:
A kind of preparation method of high weather-proof low temperature solidifying environment protection type cation paint comprises the preparation of cation paint emulsion and the preparation of cation paint mill base, and concrete steps are as follows:
(1) preparation of cation paint emulsion
With the cationic acrylic acid epoxy resin of 390-395 part, 10-12 part isocyanate crosslinking prepolymer, 35-38 part catalytic curing agent prepolymer, 4-5 part polyethers, in the adding and the resin scuffing of cylinder bore, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1200-1300 rev/min of dispersed with stirring 20-30min, the control temperature is below 50 ℃, again successively with 5-8 part butyl glycol ether, during 12-15 part acetum adds and in the scuffing of cylinder bore, continue dispersed with stirring 80-90min, the control temperature is below 50 ℃, for subsequent use
With 240-250 part deionized water, 4-5 part acetum, 6-8 part emulsifier op-10 solution adds the emulsification scuffing of cylinder bore successively, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1500-1600 rev/min of dispersed with stirring 20-30min, the control temperature is below 40 ℃, with the resin pump add uniformly scattered in and resin, joining day is 90-120min, in and after resin adds, emulsification scuffing of cylinder bore restir disperses 50-60min, add 1-2 part flow agent BYK, restir disperses 20-30min, and the emulsion control indexes is: appearance milky white, solids content 35 ± 2%, particle diameter≤0.2 μ m, pH value 6.7 ± 0.3 after the detection index meets technical requirements, filters and packages;
(2) preparation of cation paint mill base
With the cationic acrylic acid epoxy resin of 220-225 part, 20-25 part carbon black or titanium dioxide, 55-60 part kaolin, 2-4 part polyethers, 80-84 part butyl glycol ether, 0.8-1.0 a part wetting dispersing agent EFKA-5070 adds in the scuffing of cylinder bore successively, with high speed dispersor dispersed with stirring 25-30min, then leave standstill moistening 10-12h, moistening complete after, add again 30-32 part acetum, 5-6 part emulsifying agent, with high speed dispersor dispersed with stirring 25-30min, grind 3-4 time with three-roller, after the detection fineness meets technical requirements, add again the cationic acrylic acid epoxy resin of 50-54 part, 170-180 part deionized water, 20-25 part acetum, 16-18 part butyl glycol ether, 16-18 part Virahol, then, middling speed is disperseed 20-30min, grind 2-3 time with sand mill again, the mill base control indexes is: solids content 50 ± 2%, fineness≤10 μ m, pH value 5.4 ± 0.3, after the detection index meets technical requirements, filter and package.
The preparation method of described cationic acrylic acid epoxy resin may further comprise the steps:
(1) preparation of performed polymer
190-200 part TDI adding is furnished with agitator, in the reactor of reflux exchanger and thermometer, start stirring, be warming up to 40-50 ℃, in dropwise adding tank, allocate simultaneously 35-40 part ethylene glycol ethyl ether and 135-140 part diethylene glycol ether into, begin to drip ethylene glycol ethyl ether and diethylene glycol ether mixture, dropping temperature is strict controlled in 50 ± 2 ℃, time for adding is controlled in the 180-210min scope, notice that rate of addition prevents excess Temperature, after dripping, keeping under 48-52 ℃ more than the stirring 30mmin, add again 10-15 part methyl iso-butyl ketone (MIBK), be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 80-90min, after the detection index meets technical requirements, lower the temperature for subsequent use;
(2) preparation of cationic acrylate resin
With 250-255 part solvent propylene glycol monomethyl ether, 18-20 part propyl carbinol adds is furnished with agitator, in the reactor of reflux exchanger and thermometer, start stirring, be warming up to 80-85 ℃, be interrupted and add 420-425 part Resins, epoxy, the dimension temperature is until fully dissolving, add 116-120 part methyl iso-butyl ketone (MIBK), holding temperature also stirs 60-70min, begin to be warming up to 115-118 ℃, evenly drip 10-12 part methacrylic acid, 52-55 part methyl methacrylate, 25-30 part Rocryl 410,38-40 part vinylformic acid hexafluoro butyl ester, 6-8 part vinylbenzene, 2-3 part dibenzoyl peroxide, 0.5-0.6 part Dodecyl Mercaptan and propyl carbinol mixture, time for adding 150-180min, dropwise, after keeping the interior 115-118 ℃ of reaction 100-120min of still, be cooled to 48-52 ℃, stop to stir 15-20min, slowly add 2-3 part diethylamine, 77-80 part diethanolamine, 86-88 part Virahol, stir also and be warming up to again 78-82 ℃, carry out amination reaction 100-120min, detect index and meet technical requirements, be warming up to again 90-95 ℃, after keeping reaction 120-140min, slowly add 290-295 part polyamide resin, after keeping reaction 100-120min, detect index and meet technical requirements, be cooled to 75-80 ℃, slowly add again 385-388 part performed polymer, be warming up to again 78-82 ℃, after keeping reaction 180-200min, detect index and meet technical requirements, add 22-25 part deionized water, holding temperature 78-82 ℃ again, after keeping reaction 120-140min, detect index and meet technical requirements, be cooled to 50-60 ℃ and begin to filter discharging, make cationic acrylic acid epoxy resin, package spare.
The preparation method of described isocyanate crosslinking prepolymer may further comprise the steps:
(1) LY-1 manufacture method
130-132 part IPDI adding is furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocate 72-75 part methyl ethyl ketoxime into, start to stir and heat up at 42-45 ℃, begin to drip methyl ethyl ketoxime, time for adding 180-210min, temperature is controlled at 48-52 ℃ during dropping, dropping temperature should strictly be controlled, and must guard against overtemperature, after dripping, keep and stir 20-30min, after confirming that temperature no longer increases, be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 100-120min, after detecting index and meeting technical requirements, be cooled to 35-40 ℃ for subsequent use;
(2) LY-2 manufacture method
25-27 part TDI adding is furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocates 20-22 part imidazoles into.Start to stir and be warming up to 42-45 ℃, begin to drip imidazoles, dropping temperature is strict controlled in 50 ± 2 ℃, time for adding 120-150min, after dripping imidazoles, keeping under 48-52 ℃ more than the stirring 30min, after confirming that temperature no longer increases, add 2-3 part methyl iso-butyl ketone (MIBK), be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 50-60min, after the detection index meets technical requirements, be cooled to 35-40 ℃, add successively again 200-205 part Polyether 220,25-28 part methyl iso-butyl ketone (MIBK) starts stirring and is warming up to 110-120 ℃ of insulation 110-120min, after the detection index meets technical requirements, 16-18 part TDI is allocated in the dropwise adding tank, when treating that temperature is down to 85-90 ℃, begin to drip tight attention still internal reaction situation during dropping, be warming up to 110-120 ℃ after dripping, insulation 50-60min after the detection index meets technical requirements, lowers the temperature for subsequent use;
(3) the isocyanate crosslinking prepolymer is synthetic
With 405-408 part Resins, epoxy, 266-270 part Virahol adds is furnished with agitator, in the reactor of reflux exchanger and thermometer, start and be heated with stirring to 45-50 ℃, make it to dissolve fully, stop to stir, add 87-90 part diethanolamine, then after being warming up to 78-82 ℃ of insulation 55-60min, after the detection index meets technical requirements, be cooled to 72-75 ℃, under 75 ± 2 ℃, begin slowly to add 293-295 part LY-2, joining day 180-210min, after adding LY-2, then slowly add 202-204 part LY-1, joining day 150-180min, temperature is controlled at 75 ± 2 ℃, be warming up to 78-82 ℃ after adding, insulation 90-100min after the detection index meets technical requirements, is cooled to 40-50 ℃ of filtration discharging for subsequent use.
The preparation method of described catalytic curing agent prepolymer may further comprise the steps:
With 223-225 part MDI, 38-40 part methyl iso-butyl ketone (MIBK) is allocated in the 500L still, start and be cooled to 45-50 ℃ after stirring is warming up to 60-65 ℃ of affirmation MDI CL again, with 100-105 part isooctyl alcohol, 142-146 part ethylene glycol ethyl ether is allocated in the dropwise adding tank, when treating the still temperature drop to 48-50 ℃, begin to drip, time for adding 90-120min, temperature during dropping is controlled at 50 ± 2 ℃, drips rear dimension temperature and stirs 25-30min, then is warming up to 70-75 ℃, insulation 220-240min, after the detection index meets technical requirements, add 215-218 part methyl iso-butyl ketone (MIBK), 35-40 part catalyzer bismuth salt, Wei Wen stirs 25-30min, is cooled to 45-50 ℃ of filtration discharging for subsequent use.
The high weather-proof low temperature solidifying environment protection type cation paint that the present invention produces can be used as the cation paint that finish paint uses, good weatherability (reaching 600h) not only, solidification value is low (140 ℃, 20min), and unleaded Wuxi in the coating system, good stability, corrosion-resistant, can make paint for priming paint and top lacquer use, Optimization Technology, saving cost, hang down the requirement that the VOC discharging meets environmental protection.
Embodiment
The present invention is further illustrated for following specific embodiment.
Embodiment
A kind of preparation method of high weather-proof low temperature solidifying environment protection type cation paint comprises that the following step poly-:
(1) preparation of cationic acrylate Resins, epoxy
(1) preparation of performed polymer
199 parts of TDI addings are furnished with in the reactor of agitator, reflux exchanger and thermometer, start stirring, be warming up to 45 ℃, in dropwise adding tank, allocate simultaneously 39 parts of ethylene glycol ethyl ethers and 138 parts of diethylene glycol ethers into, begin to drip ethylene glycol ethyl ether and diethylene glycol ether mixture, dropping temperature is strict controlled in 50 ± 2 ℃, and time for adding is controlled in the 180-210min scope, notices that rate of addition prevents excess Temperature.After dripping, keeping under 50 ℃ more than the stirring 30mmin, add again 11 parts of methyl iso-butyl ketone (MIBK), be warming up to again 70 ℃, between 70 ± 2 ℃, be incubated 90min, after the detection index meets technical requirements, lower the temperature for subsequent use;
(2) preparation of cationic acrylate resin
With 252 parts of solvent propylene glycol monomethyl ethers, 20 parts of propyl carbinols add is furnished with agitator, in the reactor of reflux exchanger and thermometer, start stirring, be warming up to 82 ℃, be interrupted and add 423 parts of Resins, epoxy, the dimension temperature is until fully dissolving, add 119 parts of methyl iso-butyl ketone (MIBK), holding temperature also stirs 60min, begin to be warming up to 116 ℃, evenly drip 11 parts of methacrylic acids, 53 parts of methyl methacrylates, 28 parts of Rocryl 410s, 40 parts of vinylformic acid hexafluoro butyl esters, 8 parts of vinylbenzene, 2 parts of dibenzoyl peroxide, 0.5-0.6 part Dodecyl Mercaptan and propyl carbinol mixture, time for adding 160min, dropwise, after keeping the interior 115 ℃ of reaction 120min of still, be cooled to 48 ℃, stop to stir 15min, slowly add 3 parts of diethylamine, 79 parts of diethanolamine, 87 parts of Virahols, stir also and be warming up to again 81 ℃, carry out amination reaction 120min, detect index and meet technical requirements, be warming up to again 92 ℃, keep the reaction 120min after, slowly add 290-295 part polyamide resin, after keeping reaction 100-120min, detect index and meet technical requirements, be cooled to 75 ℃, slowly add again 387 parts of performed polymers, be warming up to again 82 ℃, after keeping reaction 180min, detect index and meet technical requirements, add 24 parts of deionized waters, holding temperature is 80 ℃ again, after keeping reaction 120min, detect index and meet technical requirements, be cooled to 60 ℃ and begin to filter discharging, make cationic acrylic acid epoxy resin, package spare;
(2) preparation of isocyanate crosslinking prepolymer
(1) LY-1 manufacture method
131 parts of IPDI addings are furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocate 73 parts of methyl ethyl ketoximes into, start to stir and heat up at 45 ℃, begin to drip methyl ethyl ketoxime, time for adding 200min, temperature is controlled at 50 ℃ during dropping, dropping temperature should strictly be controlled, and must guard against overtemperature, after dripping, keep and stir 30min, after confirming that temperature no longer increases, be warming up to again 70 ℃, between 70 ± 2 ℃, be incubated 120min, after detecting index and meeting technical requirements, be cooled to 40 ℃ for subsequent use;
(2) LY-2 manufacture method
26 parts of TDI addings are furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocate 21 parts of imidazoles into.Start to stir and be warming up to 45 ℃, begin to drip imidazoles, dropping temperature is strict controlled in 50 ± 2 ℃, time for adding 140min, drip imidazoles after, stir more than the 30min keeping under 52 ℃, after confirming that temperature no longer increases, add 3 parts of methyl iso-butyl ketone (MIBK), be warming up to again 70 ℃, between 70 ± 2 ℃, be incubated 60min, after the detection index meets technical requirements, be cooled to 40 ℃, add successively again 200 parts of Polyether 220s, 26 parts of methyl iso-butyl ketone (MIBK) start stirring and are warming up to 120 ℃ of insulation 120min, after the detection index meets technical requirements, 18 parts of TDI are allocated in the dropwise adding tank, when treating that temperature is down to 90 ℃, begin to drip tight attention still internal reaction situation during dropping, be warming up to 110 ℃ after dripping, insulation 60min after the detection index meets technical requirements, lowers the temperature for subsequent use;
(3) the isocyanate crosslinking prepolymer is synthetic
With 407 parts of Resins, epoxy, 268 parts of Virahols add is furnished with agitator, in the reactor of reflux exchanger and thermometer, start and be heated with stirring to 50 ℃, make it to dissolve fully, stop to stir, add 88 parts of diethanolamine, then be warming up to 82 ℃ be incubated 60min after, after the detection index meets technical requirements, be cooled to 75 ℃, under 75 ± 2 ℃, begin slowly to add 294 parts of LY-2, joining day 180min, after adding LY-2, then slowly add 204 parts of LY-1, joining day 160min, temperature is controlled at 75 ± 2 ℃, be warming up to 80 ℃ after adding, insulation 100min after the detection index meets technical requirements, is cooled to 50 ℃ of filtration dischargings for subsequent use;
(3) preparation of catalytic curing agent prepolymer
With 225 parts of MDI, 39 parts of methyl iso-butyl ketone (MIBK) are allocated in the 500L still, start and be cooled to 50 ℃ after stirring is warming up to 65 ℃ of affirmation MDI CLs again, with 100 parts of isooctyl alcohol, 146 parts of ethylene glycol ethyl ethers are allocated in the dropwise adding tank, when treating still temperature drop to 50 ℃, begin to drip, time for adding 100min, temperature during dropping is controlled at 50 ± 2 ℃, drips rear dimension temperature and stirs 30min, then is warming up to 70 ℃, insulation 240min, after the detection index meets technical requirements, add 217 parts of methyl iso-butyl ketone (MIBK), 38 portions of catalyzer bismuth salt, Wei Wen stirs 30min, is cooled to 50 ℃ of filtration dischargings for subsequent use;
(4) preparation of positively charged ion finished product coating
(1) preparation of cation paint emulsion
With 392 parts of cationic acrylic acid epoxy resins, 12 parts of isocyanate crosslinking prepolymers, 36 parts of catalytic curing agent prepolymers, 4 parts of polyethers, in the adding and the resin scuffing of cylinder bore, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1300 rev/mins of dispersed with stirring 30min, the control temperature is below 50 ℃, in successively 7 parts of butyl glycol ethers, 13 parts of acetums being added and in the scuffing of cylinder bore again, continue dispersed with stirring 90min, the control temperature is below 50 ℃, and is for subsequent use
With 240 parts of deionized waters, 4 parts of acetums, 7 parts of emulsifier op-10 solution add the emulsification scuffing of cylinder bore successively, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1500 rev/mins of dispersed with stirring 20min, the control temperature is below 40 ℃, with the resin pump add uniformly scattered in and resin, joining day is 110min, in and after resin adds, emulsification scuffing of cylinder bore restir disperses 60min, add 1.5 parts of flow agent BYK, restir disperses 30min, and the emulsion control indexes is: appearance milky white, solids content 35 ± 2%, particle diameter≤0.2 μ m, pH value 6.7 ± 0.3 after the detection index meets technical requirements, filters and packages;
(2) preparation of cation paint mill base
With 221 parts of cationic acrylic acid epoxy resins, 25 parts of carbon blacks or titanium dioxide, 58 parts of kaolin, 3 parts of polyethers, 82 parts of butyl glycol ethers, 0.8-1.0 a part wetting dispersing agent EFKA-5070 adds in the scuffing of cylinder bore successively, with high speed dispersor dispersed with stirring 30min, then leave standstill moistening 12h, moistening complete after, add again 32 parts of acetums, 5 parts of emulsifying agents, with high speed dispersor dispersed with stirring 30min, grind 3 times with three-roller, after the detection fineness meets technical requirements, add again 52 parts of cationic acrylic acid epoxy resins, 180 parts of deionized waters, 22 parts of acetums, 17 parts of butyl glycol ethers, 17 parts of Virahols, then, middling speed is disperseed 30min, grind 3 times with sand mill again, the mill base control indexes is: solids content 50 ± 2%, fineness≤10 μ m, pH value 5.4 ± 0.3, after the detection index meets technical requirements, filter and package.
The above-mentioned emulsion that makes is directly stirred, directly carry out cathode electro-coating.
Ability cathode electrophoresis technique is adopted in test, and the coated article iron plate is hung on negative electrode, and anode is stainless steel substrates; Before galvanic deposit, need to carry out pre-treatment through oil removing-washing-neutralization-washing-Biao accent-serial operations such as washing-phosphatization.
Electrodeposition condition is: electrophoretic voltage is 90V, and electrophoresis temperature is 25 ℃, electrophoresis time 3min.
After galvanic deposit is finished, taking-up is removed the floating lacquer in surface with the iron plate of filming with deionized water, film afterwards at 150 ℃ of lower baking-curing 30min, make the appearance of film clear, colorless, smooth smooth, thickness 26.5 μ m, hardness of paint film 4H, adhesion 1 grade, resistance to salt water (concentration is 3% NaCl solution)〉480h.
Claims (4)
1. the preparation method of a high weather-proof low temperature solidifying environment protection type cation paint is characterized in that, comprises the preparation of cation paint emulsion and the preparation of cation paint mill base, and concrete steps are as follows:
(1) preparation of cation paint emulsion
With the cationic acrylic acid epoxy resin of 390-395 part, 10-12 part isocyanate crosslinking prepolymer, 35-38 part catalytic curing agent prepolymer, 4-5 part polyethers, in the adding and the resin scuffing of cylinder bore, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1200-1300 rev/min of dispersed with stirring 20-30min, the control temperature is below 50 ℃, again successively with 5-8 part butyl glycol ether, during 12-15 part acetum adds and in the scuffing of cylinder bore, continue dispersed with stirring 80-90min, the control temperature is below 50 ℃, for subsequent use
With 240-250 part deionized water, 4-5 part acetum, 6-8 part emulsifier op-10 solution adds the emulsification scuffing of cylinder bore successively, connect the refrigerated water cooling circulation system, then use high speed dispersor with 1500-1600 rev/min of dispersed with stirring 20-30min, the control temperature is below 40 ℃, with the resin pump add uniformly scattered in and resin, joining day is 90-120min, in and after resin adds, emulsification scuffing of cylinder bore restir disperses 50-60min, add 1-2 part flow agent BYK, restir disperses 20-30min, and the emulsion control indexes is: appearance milky white, solids content 35 ± 2%, particle diameter≤0.2 μ m, pH value 6.7 ± 0.3 after the detection index meets technical requirements, filters and packages;
(2) preparation of cation paint mill base
With the cationic acrylic acid epoxy resin of 220-225 part, 20-25 part carbon black or titanium dioxide, 55-60 part kaolin, 2-4 part polyethers, 80-84 part butyl glycol ether, 0.8-1.0 a part wetting dispersing agent EFKA-5070 adds in the scuffing of cylinder bore successively, with high speed dispersor dispersed with stirring 25-30min, then leave standstill moistening 10-12h, moistening complete after, add again 30-32 part acetum, 5-6 part emulsifying agent, with high speed dispersor dispersed with stirring 25-30min, grind 3-4 time with three-roller, after the detection fineness meets technical requirements, add again the cationic acrylic acid epoxy resin of 50-54 part, 170-180 part deionized water, 20-25 part acetum, 16-18 part butyl glycol ether, 16-18 part Virahol, then, middling speed is disperseed 20-30min, grind 2-3 time with sand mill again, the mill base control indexes is: solids content 50 ± 2%, fineness≤10 μ m, pH value 5.4 ± 0.3, after the detection index meets technical requirements, filter and package.
2. the preparation method of the weather-proof low temperature solidifying environment protection type cation paint of height according to claim 1 is characterized in that, the preparation method of described cationic acrylic acid epoxy resin may further comprise the steps:
(1) preparation of performed polymer
190-200 part TDI adding is furnished with agitator, in the reactor of reflux exchanger and thermometer, start stirring, be warming up to 40-50 ℃, in dropwise adding tank, allocate simultaneously 35-40 part ethylene glycol ethyl ether and 135-140 part diethylene glycol ether into, begin to drip ethylene glycol ethyl ether and diethylene glycol ether mixture, dropping temperature is strict controlled in 50 ± 2 ℃, time for adding is controlled in the 180-210min scope, notice that rate of addition prevents excess Temperature, after dripping, keeping under 48-52 ℃ more than the stirring 30mmin, add again 10-15 part methyl iso-butyl ketone (MIBK), be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 80-90min, after the detection index meets technical requirements, lower the temperature for subsequent use;
The preparation of cationic acrylate resin
With 250-255 part solvent propylene glycol monomethyl ether, 18-20 part propyl carbinol adds is furnished with agitator, in the reactor of reflux exchanger and thermometer, start stirring, be warming up to 80-85 ℃, be interrupted and add 420-425 part Resins, epoxy, the dimension temperature is until fully dissolving, add 116-120 part methyl iso-butyl ketone (MIBK), holding temperature also stirs 60-70min, begin to be warming up to 115-118 ℃, evenly drip 10-12 part methacrylic acid, 52-55 part methyl methacrylate, 25-30 part Rocryl 410,38-40 part vinylformic acid hexafluoro butyl ester, 6-8 part vinylbenzene, 2-3 part dibenzoyl peroxide, 0.5-0.6 part Dodecyl Mercaptan and propyl carbinol mixture, time for adding 150-180min, dropwise, after keeping the interior 115-118 ℃ of reaction 100-120min of still, be cooled to 48-52 ℃, stop to stir 15-20min, slowly add 2-3 part diethylamine, 77-80 part diethanolamine, 86-88 part Virahol, stir also and be warming up to again 78-82 ℃, carry out amination reaction 100-120min, detect index and meet technical requirements, be warming up to again 90-95 ℃, after keeping reaction 120-140min, slowly add 290-295 part polyamide resin, after keeping reaction 100-120min, detect index and meet technical requirements, be cooled to 75-80 ℃, slowly add again 385-388 part performed polymer, be warming up to again 78-82 ℃, after keeping reaction 180-200min, detect index and meet technical requirements, add 22-25 part deionized water, holding temperature 78-82 ℃ again, after keeping reaction 120-140min, detect index and meet technical requirements, be cooled to 50-60 ℃ and begin to filter discharging, make cationic acrylic acid epoxy resin, package spare.
3. the preparation method of the weather-proof low temperature solidifying environment protection type cation paint of height according to claim 1 is characterized in that, the preparation method of described isocyanate crosslinking prepolymer may further comprise the steps:
(1) LY-1 manufacture method
130-132 part IPDI adding is furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocate 72-75 part methyl ethyl ketoxime into, start to stir and heat up at 42-45 ℃, begin to drip methyl ethyl ketoxime, time for adding 180-210min, temperature is controlled at 48-52 ℃ during dropping, dropping temperature should strictly be controlled, and must guard against overtemperature, after dripping, keep and stir 20-30min, after confirming that temperature no longer increases, be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 100-120min, after detecting index and meeting technical requirements, be cooled to 35-40 ℃ for subsequent use;
(2) LY-2 manufacture method
25-27 part TDI adding is furnished with in the reactor of agitator, reflux exchanger and thermometer, in dropwise adding tank, allocates 20-22 part imidazoles into;
Start to stir and be warming up to 42-45 ℃, begin to drip imidazoles, dropping temperature is strict controlled in 50 ± 2 ℃, time for adding 120-150min, after dripping imidazoles, keeping under 48-52 ℃ more than the stirring 30min, after confirming that temperature no longer increases, add 2-3 part methyl iso-butyl ketone (MIBK), be warming up to again 60-70 ℃, between 70 ± 2 ℃, be incubated 50-60min, after the detection index meets technical requirements, be cooled to 35-40 ℃, add successively again 200-205 part Polyether 220,25-28 part methyl iso-butyl ketone (MIBK) starts stirring and is warming up to 110-120 ℃ of insulation 110-120min, after the detection index meets technical requirements, 16-18 part TDI is allocated in the dropwise adding tank, when treating that temperature is down to 85-90 ℃, begin to drip tight attention still internal reaction situation during dropping, be warming up to 110-120 ℃ after dripping, insulation 50-60min after the detection index meets technical requirements, lowers the temperature for subsequent use;
(3) the isocyanate crosslinking prepolymer is synthetic
With 405-408 part Resins, epoxy, 266-270 part Virahol adds is furnished with agitator, in the reactor of reflux exchanger and thermometer, start and be heated with stirring to 45-50 ℃, make it to dissolve fully, stop to stir, add 87-90 part diethanolamine, then after being warming up to 78-82 ℃ of insulation 55-60min, after the detection index meets technical requirements, be cooled to 72-75 ℃, under 75 ± 2 ℃, begin slowly to add 293-295 part LY-2, joining day 180-210min, after adding LY-2, then slowly add 202-204 part LY-1, joining day 150-180min, temperature is controlled at 75 ± 2 ℃, be warming up to 78-82 ℃ after adding, insulation 90-100min after the detection index meets technical requirements, is cooled to 40-50 ℃ of filtration discharging for subsequent use.
4. the preparation method of the weather-proof low temperature solidifying environment protection type cation paint of height according to claim 1 is characterized in that, the preparation method of described catalytic curing agent prepolymer may further comprise the steps:
With 223-225 part MDI, 38-40 part methyl iso-butyl ketone (MIBK) is allocated in the 500L still, start and be cooled to 45-50 ℃ after stirring is warming up to 60-65 ℃ of affirmation MDI CL again, with 100-105 part isooctyl alcohol, 142-146 part ethylene glycol ethyl ether is allocated in the dropwise adding tank, when treating the still temperature drop to 48-50 ℃, begin to drip, time for adding 90-120min, temperature during dropping is controlled at 50 ± 2 ℃, drips rear dimension temperature and stirs 25-30min, then is warming up to 70-75 ℃, insulation 220-240min, after the detection index meets technical requirements, add 215-218 part methyl iso-butyl ketone (MIBK), 35-40 part catalyzer bismuth salt, Wei Wen stirs 25-30min, is cooled to 45-50 ℃ of filtration discharging for subsequent use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012103971554A CN102925042A (en) | 2012-10-18 | 2012-10-18 | Preparation method of high-weather-resistant low-temperature-curing environment-friendly cation coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2012103971554A CN102925042A (en) | 2012-10-18 | 2012-10-18 | Preparation method of high-weather-resistant low-temperature-curing environment-friendly cation coating |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289498B (en) * | 2013-06-24 | 2015-11-04 | 浩力森涂料（上海）有限公司 | A kind of Multipurpose high weather resistant acrylic acid electrophoretic paint and preparation method thereof |
| CN105885510A (en) * | 2016-05-23 | 2016-08-24 | 潍坊合力水性涂料制造有限公司 | Cross-linking agent for electrophoretic paint and production technology of cross-linking agent |
| CN106009871A (en) * | 2016-05-23 | 2016-10-12 | 潍坊合力水性涂料制造有限公司 | Cross-linking agent for cathode electrophoretic paint and production process thereof |
| CN106480779A (en) * | 2016-12-12 | 2017-03-08 | 郑州艾莫弗信息技术有限公司 | A kind of paper surface color fixing agent and preparation method thereof |
| CN106758516A (en) * | 2016-12-12 | 2017-05-31 | 刘海平 | The preparation method and obtained color fixing agent of a kind of paper color fixing agent |
| CN106752816A (en) * | 2016-12-02 | 2017-05-31 | 浩力森化学科技（江苏）有限公司 | With high durable, salt fog performance electrophoretic coating high and preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548488A (en) * | 2003-05-08 | 2004-11-24 | 中央涂料工业股份有限公司 | Composition for electrode deposition painting and method of preparing corresponding aquatic resin |
| CN101100567A (en) * | 2007-07-27 | 2008-01-09 | 湖南工程学院 | Method for preparing bottom surface unification cathode electrophoresis dope |
-
2012
- 2012-10-18 CN CN2012103971554A patent/CN102925042A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1548488A (en) * | 2003-05-08 | 2004-11-24 | 中央涂料工业股份有限公司 | Composition for electrode deposition painting and method of preparing corresponding aquatic resin |
| CN101100567A (en) * | 2007-07-27 | 2008-01-09 | 湖南工程学院 | Method for preparing bottom surface unification cathode electrophoresis dope |
Non-Patent Citations (2)
| Title |
|---|
| 刘玉: "丙烯酸环氧树脂高耐候环保型阴极电泳涂料的研究", 《现代涂料与涂装》 * |
| 王湘晖等: "阴极电泳涂料用阳离子丙烯酸树脂的", 《中国涂料》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103289498B (en) * | 2013-06-24 | 2015-11-04 | 浩力森涂料（上海）有限公司 | A kind of Multipurpose high weather resistant acrylic acid electrophoretic paint and preparation method thereof |
| CN105885510A (en) * | 2016-05-23 | 2016-08-24 | 潍坊合力水性涂料制造有限公司 | Cross-linking agent for electrophoretic paint and production technology of cross-linking agent |
| CN106009871A (en) * | 2016-05-23 | 2016-10-12 | 潍坊合力水性涂料制造有限公司 | Cross-linking agent for cathode electrophoretic paint and production process thereof |
| CN106752816A (en) * | 2016-12-02 | 2017-05-31 | 浩力森化学科技（江苏）有限公司 | With high durable, salt fog performance electrophoretic coating high and preparation method |
| CN106480779A (en) * | 2016-12-12 | 2017-03-08 | 郑州艾莫弗信息技术有限公司 | A kind of paper surface color fixing agent and preparation method thereof |
| CN106758516A (en) * | 2016-12-12 | 2017-05-31 | 刘海平 | The preparation method and obtained color fixing agent of a kind of paper color fixing agent |
| CN106758516B (en) * | 2016-12-12 | 2018-03-23 | 江西德盛精细化学品有限公司 | A kind of preparation method of paper color fixing agent and obtained color fixing agent |
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