CN103555164A - Crylic acid modified alcohol acid automotive coating with good quick-drying property and salt fog resistance and preparation method thereof - Google Patents
Crylic acid modified alcohol acid automotive coating with good quick-drying property and salt fog resistance and preparation method thereof Download PDFInfo
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- CN103555164A CN103555164A CN201310539195.2A CN201310539195A CN103555164A CN 103555164 A CN103555164 A CN 103555164A CN 201310539195 A CN201310539195 A CN 201310539195A CN 103555164 A CN103555164 A CN 103555164A
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Abstract
The invention provides a crylic acid modified alcohol acid automotive coating with good quick-drying property and salt fog resistance. The automotive coating is mixed and prepared from 34-36 of LH-159 resin, 23-25 of 40% HPE resin liquor, 2-3 of carbon black, 0.3-0.5 of dispersing agent, 4-7 of composite phosphate anti-rust pigment, 3-6 of aluminum potassium sulfate, 16-18 of precipitated barium sulphate, 1-3 of anti-settling agent, 0.5-1 of low-molecular-weight epoxy resin, 0.5-1 of stabilizer, 0.2-0.3 of drier, 6-9 of aromatics solvent, and 5-6 of modified padding. The automotive coating has the characteristics of good quick-drying property and salt fog resistance.
Description
Technical field:
The present invention relates to a kind of paint, be specifically related to good acrylic modified alkyd automobile finish of a kind of quick-drying salt fog resistance and preparation method thereof.
Background technology:
Along with the development of Domestic Automotive Industry, also more and more higher to the requirement of goods vehicle vehicle bridge application.On the one hand, automotive axle is disposable application after having combined, and substrate treatment is not in place, thereby the coating of requirement use has the service performance of low prepared surface; On the other hand, some subassemblies (as plastic component) on automotive axle, can not high bake, and after rolling off the production line, is easy to sign and carrying, thereby requires the rate of drying of filming fast; The 3rd, require film adhesive good, salt fog resistance is good.The high chlorination type of vinylformic acid one in the past adopting, the high chlorination type of alkyd one or other is similar, be binary composite membrane-forming base-material.The good acrylic modified alkyd automobile finish of a kind of quick-drying salt fog resistance of the present invention, adopted acrylic acid synthesizing modification long oil alkyd, aliphatic hydrocarbon long-chain in this resin structure and high-performance HCPE (HPE resin), have good compatibility, and plasticization effect is good.Film performance had both possessed snappiness, water tolerance and the easy working characteristic of long oil alkyd, possesses again the characteristic that vinylformic acid is protected light, protected look, anti-efflorescence, also there is the excellent adhesive attraction of HCPE and salt fog resistance etc. simultaneously, this organic assembling can be learnt from other's strong points to offset one's weaknesses in performance.
Goal of the invention:
The invention provides good acrylic modified alkyd automobile finish of a kind of quick-drying salt fog resistance and preparation method thereof, automobile finish of the present invention is filmed and is both possessed snappiness, water tolerance and the easy working characteristic of long oil alkyd, possesses again the characteristic that vinylformic acid is protected light, protected look, anti-efflorescence, also there is the excellent adhesive attraction of HCPE and salt fog resistance etc. simultaneously, this organic assembling can be learnt from other's strong points to offset one's weaknesses in performance.
The technical solution used in the present invention is as follows for achieving the above object:
The acrylic modified alkyd automobile finish that salt fog resistance is good, is characterized in that, its component by following weight part is made:
LH-159 resin 34-36,40% high-performance HCPE liquid 23-25, pigment 2-3, dispersion agent 0.3-0.5, composite phosphate rust-stabilising pigment 4-7, potassium aluminum silicate 3-6, process white 16-18, anti-settling agent 1-3, E-51 epoxy resin 0.5-1, stablizer 0.5-1, siccative 0.2-0.3, aromatic solvent 6-9, modified filler 5-6
The preparation method of described LH-159 resin is:
(1) take by weight following component:
Methyl methacrylate 7-9, methacrylic acid 0.2-0.4, benzoyl peroxide 0.1-0.2, C5-9 low-carbon (LC) synthetic fatty acid 10-12, tung oil 13-15, tetramethylolmethane 6-8, MALEIC ANHYDRIDE 4-5, phthalic anhydride 5-7, dimethylbenzene 48-52,
(2) preparation of acrylic ester polymer
A, first the initiator benzoyl peroxide of the methyl methacrylate of formula ratio, methacrylic acid and 80% to be made into compound A standby, and remaining initiator benzoyl peroxide is dissolved in dimethylbenzene, makes benzoyl peroxide xylene solution B standby;
B, in reactor, add dimethylbenzene, be warming up to 120 ℃, start to drip compound A, and at the uniform velocity heat up with the speed of 1 ℃/6 minutes, the highlyest be warming up to 125 ℃, intensification limit, limit drips compound A, and control time for adding is 2.5-3.5h, after dripping off, at 125 ℃, is incubated 1.5h, drip again initiator benzoyl peroxide xylene solution B, in 2h, drip off, be at the uniform velocity warming up to 130 ℃ and maintain more than 2 hours, prepare acrylic ester polymer simultaneously;
(3) acrylic acid modified long oil alkyd
By low-carbon (LC) synthetic fatty acid, tung oil adds reactor, under stirring, add tetramethylolmethane, be warming up to 220-240 ℃, insulation alcoholysis 1-2h, then be cooled to 180-200 ℃, stop stirring, add MALEIC ANHYDRIDE, after its fusing, open and stir, add phthalic anhydride and backflow dimethylbenzene, be warming up to 190-210 ℃, after backflow esterification 2-3h, be cooled to again 125-135 ℃, add acrylic ester polymer, add backflow, prevent that temperature from raising, insulation backflow 2.5-3.5h, transformation efficiency reaches 97% when above, cooling, filter, discharging obtains the LH-159 resin of solids content 50%-52%,
Described modified filler is to be prepared and obtained by following method: a. takes off the raw material of row weight part: kaolin 100-150, calcium carbonate 120-130, zeolite 10-12, nano-sized carbon 1-2, tungstic oxide 1-2, lanthanum trioxide 2-3, peppermint essential oil 2-3, Sodium peroxoborate 1-2, aluminum oxide 2-3, precipitator method barium sulfate 30-34, tea-polyphenol 3-4, triethyl citrate 1-2, titanate coupling agent TMC-TTS4-6, jade powder 1-2;
B, kaolin, calcium carbonate, zeolite are calcined to 4-5h at 450-480 ℃, be cooled to room temperature, after taking-up, add in the sodium hydroxide solution of 3-4% and grind 1-2 hour, then, the hydrochloric acid soln that adds 12-15%, adjusting pH value is 4-5, ageing 10-15 hour, and it is neutral that repeated hydrogenation sodium hydroxide solution regulates lapping liquid pH, filter, dry and obtain filler powder;
C, above-mentioned gained powder is mixed with other remaining component, and even with the high speed dispersion of 8000-10000 rev/min, obtain.
The acrylic modified alkyd automobile finish that described quick-drying salt fog resistance is good, is characterized in that: described pigment is selected from one or more in carbon black, titanium dioxide, chrome yellow, molybdenum red, ferric oxide series, phthalein mountain valley with clumps of trees and bamboo series, toluidine maroon, talcum powder, calcium carbonate, barium sulfate, silicon-dioxide.
The production method of the acrylic modified alkyd automobile finish that described quick-drying salt fog resistance is good, is characterized in that, comprises the following steps:
(1) press formula rate by xylene soluble filtration for high-performance HCPE, the LH-159 resin, dispersion agent, pigment, the filler that add successively again 20-30% formula ratio, with 2000-2600r/min rotating speed high speed dispersion after 1-1.5 hour, then filter with 80 eye mesh screens;
(2) material filtering enters sand mill and is ground to fineness control≤30u discharging, requires outlet material temperature≤60 ℃;
(3) material that mesh-of-grind is qualified adds to adjust to be converted in still, and adds the rest materials in formula, with the middling speed of 100-200r/min, stirs evenly;
(4), after stirring evenly, with aromatic solvent, adjust viscosity to 90-120(S)/be coated with-4, with 200 order vibratory screening apparatuss, filter, pack.
The theoretical foundation of invention:
(1) determining of acrylic acid modified long oil alkyd (hereinafter referred to as LH-159 resin):
In LH-159 resin, what the present invention adopted is that esterification is prepared acrylic acid modified long oil alkyd.First the acrylic resin of anamorphic zone carboxyl then adds this functional acrylic resins with preparation LH-159 resin in Synolac preparation process; Secondly, general acrylic acid modified alkyd resin and HCPE compatibility are bad, can not be for painting, the present invention selects C5-9 low-carbon (LC) synthetic fatty acid, tung oil as the properties-correcting agent of tetramethylolmethane-phthalic anhydride system, and usage quantity can be enough large, this aliphatic hydrocarbon long-chain, not only system is had to plastification, and fine compatibility and the wettability to color stuffing of system are provided, conjugated double bond in tung oil, in the esterification process in later stage, also there is polymerization to a certain extent with two keys residual in acrylate resin.Make, in this resin segment, to give intermiscibility, pigment wettability, sticking power, hydrophobic nature and photostabilization that this resin is good.
(2) become determining of paint formula:
Acrylic modified alkyd automobile finish, requires that salt fog resistance is good, strong adhesion, and dryness is fast, be easy to construction, the solids ratios 1.8: 1 of determining LH-159 and HPE resin, this ratio has not only guaranteed construction requirement, and has guaranteed film good mechanical property and salt fog resistance.
In automobile finish of the present invention, applied special rust-stabilising pigment-composite phosphate rust-stabilising pigment, it has dual antirust function---and be that chelating protection and physics are antirust, physics is antirust is the general character that general rust-stabilising pigment has, it is by the inertia of rust-stabilising pigment self and impervious next antirust, and this special pigment is except having above-mentioned functions, can also and polymer and steel structure chelated surface, make polymeric membrane finer and close, impervious better, thereby reduction water, oxygen, the seepage force of low-molecular material confrontation paint film, improve erosion resistance and the oil-proofness of paint film, strengthen the sticking power of paint film, water tolerance and oil-proofness.The application of potassium aluminum silicate, shows the unexistent surface effects of conventional fillers and comprehensive physicochemical property.In lacquering of the present invention, added siccative, cross-linking density is further strengthened.
In automobile finish production technique of the present invention, LH-159 resin is the critical material of painting, the synthetic temperature of resin is controlled, the reinforced at the uniform velocity control of property is the key point of resin property quality, and effectively control can make the molecular weight distribution of synthetic resins narrower, thereby obtains desirable paint film; In sand milling operation, high-performance sand grinder grinds 2-3 road, and fineness can reach below 30 μ; Filter progress is that product is carried out to last purification, so that gratifying visual appearance to be provided.
Advantage of the present invention:
1, the present invention adopts acrylic ester polymer modification long oil alkyd, has solved the compatibility with HPE resin, and the plastification of filming; Solved the slow problem of dryness of filming, and the low prepared surface ground contradiction that is difficult for adhering to.
2, acrylic modified alkyd automobile finish of the present invention, salt spray resistance is excellent, through user's life-time service, shows: the resistance to neutral salt spray of paint film reaches 150h and not containing heavy metal, low Hazardous, belongs to environmentally friendly machine.
Embodiment
One, the preparation LH-159 resinogen material of embodiment 1 acrylic acid modified alkyd resin (LH-159 resinogen material)
1.1 materials form
Methyl methacrylate (MMA), methacrylic acid (AA), benzoyl peroxide (B, P, O), C5-9 low-carbon (LC) synthetic fatty acid), tung oil, tetramethylolmethane, MALEIC ANHYDRIDE, phthalic anhydride, dimethylbenzene (XYL) is industrial goods.
The material component weight percent of 1.2LH-159 resin
1.3LH-159 production of resins technique:
(1) preparation of acrylic ester polymer
A, first the initiator benzoyl peroxide of the methyl methacrylate of formula ratio, methacrylic acid and 80% to be made into compound A standby, and remaining initiator benzoyl peroxide is dissolved in dimethylbenzene, makes benzoyl peroxide xylene solution B standby;
B, in reactor, add dimethylbenzene, be warming up to 120 ℃, start to drip compound A, and at the uniform velocity heat up with the speed of 1 ℃/6 minutes, the highlyest be warming up to 125 ℃, intensification limit, limit drips compound A, and control time for adding is 2.5-3.5h, after dripping off, at 125 ℃, is incubated 1.5h, drip again initiator benzoyl peroxide xylene solution B, in 2h, drip off, be at the uniform velocity warming up to 130 ℃ and maintain more than 2 hours, prepare acrylic ester polymer simultaneously; (2) prepare acrylic acid modified alkyd resin
Low-carbon (LC) synthetic fatty acid, tung oil are added to reactor, under stirring, add tetramethylolmethane, be warming up to 240 ℃, insulation alcoholysis 1.5-2h, be cooled to 200 ℃, stop stirring, add MALEIC ANHYDRIDE, after its fusing, open and stir, add phthalic anhydride and backflow dimethylbenzene, be warming up to 200 ℃, backflow esterification, after esterification 3h, be cooled to 130 ℃, add acrylic ester polymer, add backflow, prevent that temperature from raising, general insulation backflow 3h, transformation efficiency reaches 97% when above, and cooling, filtration, discharging obtain the LH-159 resin of solids content 50%-52%.
1.4LH-159 resin detected result
| Project | Index | Assay |
| Color (number, Fe-Co method)≤ | 13 | 13 |
| Solids content % | 51±2 | 51.2 |
| Viscosity (being coated with-4), s | 60-100 | 71 |
| Acid value mgKOH/g≤ | 12 | 9.6 |
The preparation of embodiment 2, lacquering black dumb light acrylic modified alkyd automobile finish
Main raw material(s)
2.1 materials form
LH-159 resin, the high-performance HCPE (HPE resin) of embodiment 1 preparation, middle colour carbon black 3#, composite phosphate rust-stabilising pigment, potassium aluminum silicate, process white, modified filler, various auxiliary agent and aromatic solvent are industrial goods.
2.2 black dumb light acrylic modified alkyd automobile finish each component weight (kg) are:
LH-159 resin 35,40%HPE resin liquid 24, carbon black 3, dispersion agent 0.4, composite phosphate rust-stabilising pigment 45, potassium aluminum silicate 4, process white 17, anti-settling agent 2, low-molecular-weight epoxy resin 0.6, UV light absorber 9440.6, siccative 0.2, aromatic solvent 8, modified filler 5
2.3 black dumb light acrylic modified alkyd automobile finish preparation technologies are:
(1) by xylene soluble for high-performance HCPE (HPE resin) and filter, then add part LH-159 resin and dispersion agent, pigment, filler high speed dispersion (2000-2600r/min) after 1 hour, with 80 eye mesh screens filtrations;
(2) material filtering enters sand mill circular grinding, outlet material temperature≤60 ℃, fineness control≤30u.
(3) material that mesh-of-grind is qualified adds to adjust to be converted in still, and adds remaining material, balance formula, and middling speed (100-200r/min) stirs evenly;
(4), after stirring evenly, with aromatic solvent, adjust viscosity to 90-120(S)/be coated with-4, with 200 order vibratory screening apparatuss, filter, pack.
Wherein, modified filler is to be prepared and obtained by following method:
A, take off the raw material of row weight part: kaolin 120, calcium carbonate 125, zeolite 11, nano-sized carbon 1.5, tungstic oxide 1.5, lanthanum trioxide 2.5, peppermint essential oil 2.5, Sodium peroxoborate 1.5, aluminum oxide 2.5, precipitator method barium sulfate 33, tea-polyphenol 3.5, triethyl citrate 1.5, titanate coupling agent TMC-TTS5, jade powder 1.5;
B, kaolin, calcium carbonate, zeolite are calcined to 4-5h at 450-480 ℃, be cooled to room temperature, after taking-up, add in the sodium hydroxide solution of 3-4% and grind 1-2 hour, then, the hydrochloric acid soln that adds 12-15%, adjusting pH value is 4-5, ageing 10-15 hour, and it is neutral that repeated hydrogenation sodium hydroxide solution regulates lapping liquid pH, filter, dry and obtain filler powder;
C, above-mentioned gained powder is mixed with other remaining component, and even with the high speed dispersion of 8000-10000 rev/min, obtain.
2.4 black dumb light acrylic modified alkyd automobile finish detected results
Claims (3)
1. the good acrylic modified alkyd automobile finish of quick-drying salt fog resistance, is characterized in that, its component by following weight part is made:
LH-159 resin 34-36,40% high-performance HCPE liquid 23-25, pigment 2-3, dispersion agent 0.3-0.5, composite phosphate rust-stabilising pigment 4-7, potassium aluminum silicate 3-6, process white 16-18, anti-settling agent 1-3, E-51 epoxy resin 0.5-1, stablizer 0.5-1, siccative 0.2-0.3, aromatic solvent 6-9, modified filler 5-6
The preparation method of described LH-159 resin is:
(1) take by weight following component:
Methyl methacrylate 7-9, methacrylic acid 0.2-0.4, benzoyl peroxide 0.1-0.2, C5-9 low-carbon (LC) synthetic fatty acid 10-12, tung oil 13-15, tetramethylolmethane 6-8, MALEIC ANHYDRIDE 4-5, phthalic anhydride 5-7, dimethylbenzene 48-52,
(2) preparation of acrylic ester polymer
A, first the initiator benzoyl peroxide of the methyl methacrylate of formula ratio, methacrylic acid and 80% to be made into compound A standby, and remaining initiator benzoyl peroxide is dissolved in dimethylbenzene, makes benzoyl peroxide xylene solution B standby;
B, in reactor, add dimethylbenzene, be warming up to 120 ℃, start to drip compound A, and at the uniform velocity heat up with the speed of 1 ℃/6 minutes, the highlyest be warming up to 125 ℃, intensification limit, limit drips compound A, and control time for adding is 2.5-3.5h, after dripping off, at 125 ℃, is incubated 1.5h, drip again initiator benzoyl peroxide xylene solution B, in 2h, drip off, be at the uniform velocity warming up to 130 ℃ and maintain more than 2 hours, prepare acrylic ester polymer simultaneously;
(3) acrylic acid modified long oil alkyd
By low-carbon (LC) synthetic fatty acid, tung oil adds reactor, under stirring, add tetramethylolmethane, be warming up to 220-240 ℃, insulation alcoholysis 1-2h, then be cooled to 180-200 ℃, stop stirring, add MALEIC ANHYDRIDE, after its fusing, open and stir, add phthalic anhydride and backflow dimethylbenzene, be warming up to 190-210 ℃, after backflow esterification 2-3h, be cooled to again 125-135 ℃, add acrylic ester polymer, add backflow, prevent that temperature from raising, insulation backflow 2.5-3.5h, transformation efficiency reaches 97% when above, cooling, filter, discharging obtains the LH-159 resin of solids content 50%-52%,
Described modified filler is to be prepared and obtained by following method: a. takes off the raw material of row weight part: kaolin 100-150, calcium carbonate 120-130, zeolite 10-12, nano-sized carbon 1-2, tungstic oxide 1-2, lanthanum trioxide 2-3, peppermint essential oil 2-3, Sodium peroxoborate 1-2, aluminum oxide 2-3, precipitator method barium sulfate 30-34, tea-polyphenol 3-4, triethyl citrate 1-2, titanate coupling agent TMC-TTS 4-6, jade powder 1-2;
B, kaolin, calcium carbonate, zeolite are calcined to 4-5h at 450-480 ℃, be cooled to room temperature, after taking-up, add in the sodium hydroxide solution of 3-4% and grind 1-2 hour, then, the hydrochloric acid soln that adds 12-15%, adjusting pH value is 4-5, ageing 10-15 hour, and it is neutral that repeated hydrogenation sodium hydroxide solution regulates lapping liquid pH, filter, dry and obtain filler powder;
C, above-mentioned gained powder is mixed with other remaining component, and even with the high speed dispersion of 8000-10000 rev/min, obtain.
2. the good acrylic modified alkyd automobile finish of quick-drying salt fog resistance according to claim 1, is characterized in that: described pigment is selected from one or more in carbon black, titanium dioxide, chrome yellow, molybdenum red, ferric oxide series, phthalein mountain valley with clumps of trees and bamboo series, toluidine maroon, talcum powder, calcium carbonate, barium sulfate, silicon-dioxide.
3. the production method of the good acrylic modified alkyd automobile finish of quick-drying salt fog resistance according to claim 1, is characterized in that, comprises the following steps:
(1) press formula rate by xylene soluble filtration for high-performance HCPE, the LH-159 resin, dispersion agent, pigment, the filler that add successively again 20-30% formula ratio, with 2000-2600r/min rotating speed high speed dispersion after 1-1.5 hour, then filter with 80 eye mesh screens;
(2) material filtering enters sand mill and is ground to fineness control≤30u discharging, requires outlet material temperature≤60 ℃;
(3) material that mesh-of-grind is qualified adds to adjust to be converted in still, and adds the rest materials in formula, with the middling speed of 100-200 r/min, stirs evenly;
(4), after stirring evenly, with aromatic solvent, adjust viscosity to 90-120(S)/be coated with-4, with 200 order vibratory screening apparatuss, filter, pack.
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| CN104629061A (en) * | 2015-01-30 | 2015-05-20 | 广东省宜华木业股份有限公司 | Preparation method for water-based acrylic-modified alkyd resin |
| CN105838248A (en) * | 2016-04-25 | 2016-08-10 | 南京高崎电机有限公司 | Novel automobile paint |
| CN106752607A (en) * | 2016-11-23 | 2017-05-31 | 安徽菱湖漆股份有限公司 | A kind of poly modified acrylic acid leaf springs of car paint and preparation method thereof |
| CN107641440A (en) * | 2017-11-09 | 2018-01-30 | 鹤山市千年化工实业有限公司 | Anti-corrosion automobile coating |
| CN108129964A (en) * | 2017-12-13 | 2018-06-08 | 成都拜迪新材料有限公司 | The preparation method of halogenated polyethylene modified water-based alkyd resin and coating |
| CN113897099A (en) * | 2021-11-17 | 2022-01-07 | 瑞易德新材料股份有限公司 | Chlorinated polypropylene coating and preparation method thereof |
| CN114634751A (en) * | 2020-12-16 | 2022-06-17 | 河南青山环保科技有限公司 | Water-based acid and alkali resistant finish paint and production process thereof |
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| CN107641440A (en) * | 2017-11-09 | 2018-01-30 | 鹤山市千年化工实业有限公司 | Anti-corrosion automobile coating |
| CN108129964A (en) * | 2017-12-13 | 2018-06-08 | 成都拜迪新材料有限公司 | The preparation method of halogenated polyethylene modified water-based alkyd resin and coating |
| CN114634751A (en) * | 2020-12-16 | 2022-06-17 | 河南青山环保科技有限公司 | Water-based acid and alkali resistant finish paint and production process thereof |
| CN113897099A (en) * | 2021-11-17 | 2022-01-07 | 瑞易德新材料股份有限公司 | Chlorinated polypropylene coating and preparation method thereof |
| CN113897099B (en) * | 2021-11-17 | 2022-07-26 | 瑞易德新材料股份有限公司 | Chlorinated polypropylene coating and preparation method thereof |
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