CN1461783A - Powdered paint - Google Patents
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- CN1461783A CN1461783A CN 02115292 CN02115292A CN1461783A CN 1461783 A CN1461783 A CN 1461783A CN 02115292 CN02115292 CN 02115292 CN 02115292 A CN02115292 A CN 02115292A CN 1461783 A CN1461783 A CN 1461783A
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Abstract
A thermosetting powder paint is prepared from at least one epoxy-contained resin chosen from epoxyacrylic resin, epoxy resin, etc, at least one carboxy-contained resin chosen from carboxy polyester resin, carboxyacrylic resin, etc, filler and assistant through fusing while mixing, cooling, pulverizing and sieving. Its advantages are high resistance to wipe and controllable lustre.
Description
Technical field:
The present invention relates to the outdoor low brightness paint powder of particularly a kind of thermoset scratch resistance of a kind of powder coating, belong to technical field of coatings.
Background technology:
Powder coating is a kind of green coating of non-volatility organic solvent, and it has resource-saving, solvent-free, low pollution, high-level efficiency, characteristics such as application moulding, and Application Areas is extensive, is developed rapidly in countries in the world.Powder coating market about 30~40% is half light or the kind of low gloss more, outdoor low light powder applied range is mainly used in aspects such as building materials, aluminium section bar, bumper, outdoor household electrical appliances, outdoor pipe, freeway guardrail, outdoor advertising, metrical instrument shell and lamp decoration.There are multiple technologies to be used to reduce the gloss of powder coating systems.These technology comprise add paraffin, silicon-dioxide etc. and so on and system not mutually the filler of mixing reach the delustring purpose, but the amount of the filler that this method need add is big, performances such as the levelling property of coating and physical strength all reduce greatly; Another kind method is that doing of the active powder coating of differential responses mixed (as U.S.3,842,035 introduces), but this method needs a large amount of doing to mix experiment determines its prescription, and owing to be difficult to disperse evenly between two kinds of powder, the gloss of the coating that obtains like this differs greatly, and circulation ratio is bad; The third method is to use mixing cured system, as the different solidifying agent reaction (European Patent Application No. 366 of a kind of resin with two or more, 608 introduce) or two or more resin and a kind of solidifying agent effect (Japanese patent application No. 154,771/88 introduces) and various kinds of resin and multiple solidifying agent effect, the problem of this method is that the proportioning of different curing system is very big to the gloss influence, can different in addition solidifying agent uniform distribution in powder, gloss and planeness to coating all have a significant impact, and under the fabrication process condition of present powder coating, realize that almost be impossible at these 2.Therefore the circulation ratio of this method is very poor, and levelling property is also very undesirable.And adopt the coating gloss of the powder coating that the acrylic resin contain epoxide group and linear low acid value vibrin obtain as base-material (Chinese patent application number 00117364.2 introduce) can drop to below 5% (60 °), has excellent weathering resistance in addition, but it exists scratch resistance poor, and gloss control is shortcoming such as difficulty relatively.After mainly the showing as hard thing and streak the lower surface of gloss of scratch resistance difference, gloss raises, and influences outward appearance.
Summary of the invention: the invention provides that a kind of prescription is simple, technology convenience, gloss may command, scratch resistance outdoor low brightness paint powder and preparation method thereof preferably.The outdoor low brightness paint powder of the present invention comprises with the low acid value carboxyl polyester resin of a kind of linearity as base-material, and a kind of epoxy group(ing) acrylic resin can not add other delustring auxiliary agent in addition as solidifying agent.In this powder coating, the mol ratio of epoxy group(ing) and carboxyl is 0.5: 1~2.0: 1.This powder coating major ingredient comprises:
(a) 5-35% epoxy group(ing) acrylic resin;
(b) 0-5% triglycidyl isocyanurate;
(c) 0-10% bisphenol A type epoxy resin;
(d) 30-65% carboxyl polyester resin;
(e) 0-15% carboxyl acrylic resin;
(f) 29.5-60% filler;
(g) 0.5-1% auxiliary agent.
Details are as follows for technical scheme of the present invention: 1. synthesizing epoxy base acrylic resin: adoptable polymerization process has: solution polymerization, letex polymerization, mass polymerization, suspension polymerization etc., and wherein suitable with solution polymerization.Solvent for use comprises: a kind of or mixed solvent in toluene, ethyl acetate, butylacetate, ethylbenzene, dimethylbenzene, acetone, the butanone etc., polymerization temperature is near the boiling temperature of solvent for use.Contain the epoxy group(ing) monomer in the monomer of synthesizing epoxy base acrylic resin and comprise a kind of or mixture in glycidyl methacrylate and the glycidyl acrylate, account for the 5-30% of total monomer weight; Other monomer comprises a kind of or its mixture in (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) propyl acrylate, (methyl) butyl acrylate, (methyl) isobutyl acrylate etc., accounts for the 70-95% of total monomer weight; The alkyl-acrylates monomer can replace with part vinyl aromatic (co) hydrocarbon compound in addition, as: vinylbenzene, vinyl toluene and ethyl styrene etc., its weight accounts for the monomeric 0-25% of alkyl-acrylates.The initiator that polymerization process is used comprises: peroxide and azo-compound class, as: benzoyl peroxide, t-butyl hydrogen peroxide, peroxidation two different phenylpropyl alcohols, Diisopropyl azodicarboxylate etc., its consumption is the 0.5-15% of monomer weight.Simultaneously can add small number of molecules amount conditioning agent, molecular weight regulator comprises lauryl mercaptan, octane-iso base mercaptan, carbon tetrabromide, bromo-trichloromethane etc., and add-on is the 1.5-4% of monomer weight.The reaction solution that polymerization the obtains processing that outgases.Degas method has the tower degassing, the degassing of still formula and twin screw vaporizer method etc.Degassing temperature generally is controlled at 160-200 ℃, and vacuum degree control is in 1.0-1.01 * 10
5Pa.The degassing is emitted resin after handling while hot, and cool to room temperature obtains transparent or faint yellow brittle resin.The epoxy group(ing) acrylic resin that the present invention obtains has following feature: number-average molecular weight is 2,000-10,000; Epoxy equivalent (weight) is 300-1,200; Softening temperature 80-130 ℃; Second-order transition temperature 40-75 ℃ (DSC method).2. synthetic carboxyl polyester resin: carry out polycondensation synthesis of hydroxy vibrin by polycarboxylic acid or acid anhydrides and polyvalent alcohol earlier, and then obtain carboxyl polyester resin with polycarboxylic acid or acid anhydrides addition reaction.The synthetic used monomer of carboxyl polyester resin is that polyfunctional monomer is polycarboxylic acid or acid anhydrides and polyvalent alcohol, polycarboxylic acid or acid anhydrides can be terephthalic acids, m-phthalic acid, Tetra hydro Phthalic anhydride, hexanodioic acid, sebacic acid, Succinic Acid, 1,4-cyclohexane dicarboxylic acid, at least a or its mixture in the trimellitic acid 1,2-anhydride; Polyvalent alcohol can be an ethylene glycol, neopentyl glycol, 1,4 cyclohexane dimethanol, trimethylolethane, at least a or its mixture in the TriMethylolPropane(TMP); Can add little amount of catalyst such as Dibutyltin oxide, normal-butyl tin three monooctyl esters etc. in addition, add-on is the 0.01-0.5% of monomer total amount; Can add small amount of antioxidant, as tributyl phosphate, triphenyl phosphite etc., add-on is the 0.01-0.5% of monomer total amount.When beginning, polyreaction adopts the normal pressure polycondensation, heat up gradually, temperature of reaction can reach 240 ℃, after question response proceeded to a certain degree, reaction system became transparent by muddiness, at this moment carried out the vacuum polycondensation, obtain hydroxy polyester resin, add polycarboxylic acid or acid anhydrides then and carry out addition reaction, carry out the vacuum polycondensation at last again, with the acid number and the viscosity of control resin.Vacuum degree control is in 1.0-1.01 * 10
5Pa obtains carboxyl polyester resin, emits resin while hot, and cool to room temperature obtains water white transparency or faint yellow brittle resin.The carboxyl polyester resin that the present invention obtains has following feature: acid number is 20-60mgKOH/g, and promptly number-average molecular weight is 1,900-8,500, softening temperature is 80-140 ℃, and viscosity is 1,000-8,000mPa.s (200 ℃), second-order transition temperature is 45-75 ℃ (a DSC method).3. synthetic carboxyl acrylic resin: adoptable copolymerization process has: solution polymerization, letex polymerization, mass polymerization, suspension polymerization etc., and wherein suitable with solution polymerization.Solvent for use comprises: a kind of or mixed solvent in toluene, ethyl acetate, butylacetate, ethylbenzene, dimethylbenzene, acetone, the butanone etc., polymerization temperature is near the boiling temperature of solvent for use.Contain carboxylic monomer in the monomer of synthetic carboxyl acrylic resin and comprise a kind of or mixture in methacrylic acid and the vinylformic acid, account for the 5-30% of total monomer weight; Other monomer comprises a kind of or its mixture in (methyl) methyl acrylate, (methyl) ethyl propenoate, (methyl) propyl acrylate, (methyl) butyl acrylate, (methyl) isobutyl acrylate etc., accounts for the 70-95% of total monomer weight; The alkyl-acrylates monomer can replace with part vinyl aromatic (co) hydrocarbon compound in addition, as: vinylbenzene, vinyl toluene and ethyl styrene etc., its weight accounts for the monomeric 0-25% of alkyl-acrylates.The initiator that polymerization process is used comprises: peroxide and azo-compound class, as: benzoyl peroxide, t-butyl hydrogen peroxide, peroxidation two different phenylpropyl alcohols, Diisopropyl azodicarboxylate etc., its consumption is the 0.5-15% of monomer weight.Simultaneously can add small number of molecules amount conditioning agent, molecular weight regulator comprises lauryl mercaptan, octane-iso base mercaptan, carbon tetrabromide, bromo-trichloromethane etc., and add-on is the 1.5-4% of monomer weight.The reaction solution that polymerization the obtains processing that outgases.Degassing temperature generally is controlled at 160-200 ℃, and vacuum degree control is in 1.0-1.01 * 10
5Pa.The degassing is emitted resin after handling while hot, and cool to room temperature obtains transparent or faint yellow brittle resin.The carboxyl acrylic resin that the present invention obtains has following feature: number-average molecular weight is 2,000-10,000; Acid number is 30-2,00; Softening temperature 80-130 ℃; Second-order transition temperature 40-75 ℃ (DSC method).4. the preparation of powder coating: the above-mentioned resin that makes is mixed with a certain proportion of filler, pigment, flow agent, catalyzer etc., again through single, double screw extrusion press melting mixing, cool off, pulverize, sieve, obtain the outdoor low brightness paint powder of scratch resistance of the present invention.The consumption of terminal carboxyl polyester resin is 35-65% (weight) in the powder coating of the present invention; The carboxy acrylic consumption is 0-15% (weight); The acrylic resin consumption of epoxy group(ing) is 5-35% (weight); Triglycidyl isocyanurate (TGIC) consumption is 0-20% (weight); The bisphenol A type epoxy resin consumption is 0-10% (weight); TGIC and Resins, epoxy are the commercially available prod; The filler that also has 30-60% in addition is as titanium dioxide, barium sulfate, light calcium carbonate, talcum powder etc.; The auxiliary agent that can add 0.5-1% in addition is as flow agent, promotor etc.The pigment that uses in this powder coating is commercially available pigment, and its kind and consumption are decided according to required color and colourity.The flow agent that uses in this powder coating is commercially available acrylic polymer, and as Resiflow PV5 of WORLEE company etc., its consumption is 0.5-0.7%.The powder coating of gained of the present invention, its median size are 10-75 μ m, and it is sprayed on the metallic surface of handling through degreasing and rust removal, toast 10-25 minute down at 160-210 ℃ then, and top coat smooth, smooth, the color and luster homogeneous just can obtain filming.Spraying method commonly used has: friction spraying, electrostatic spraying, fluidized-bed spraying etc. are wherein more suitable with electrostatic spraying.Powder coating of the present invention, spraying, the coating mirror surface luster after solidifying are adjustablely 30% below (to press GB9754-88 mensuration, 60 °), resistance to impact shock 〉=50Kg.cm (pressing GB1732-93 measures), pencil hardness H above (pressing GB6739-86 measures), sticking power (cross-hatching is measured by GB9286-88) is 1 grade, and weathering resistance is that GB1865-80 mensuration is pressed in ultraviolet artificial accelerated aging test (QUV).
The outdoor low brightness paint powder of scratch resistance of the present invention, it is low to have a cost, and process for preparing resins is simple, and scratch resistance is better, the gloss may command, gloss can arrive<5%, and characteristics such as have excellent weather resistance.
Embodiment:
The invention will be further elaborated by following examples.
[embodiment 1]
Synthesizing of epoxy group(ing) acrylic resin, filling a prescription is:
Glycidyl methacrylate (GMA) 90g
Methyl methacrylate (MMA) 210g
Benzoyl peroxide (BPO) 15g
Butylacetate (solvent) 300g
Above monomer and initiator are mixed, have in the four-hole round-bottomed flask of reflux condensate device, add the 300g butylacetate at 1000ml, feed nitrogen, air in the displacement bottle starts stirring, is warming up near 130 ℃, butylacetate begins to reflux, keep temperature-resistant, drip mix monomer, about 3 hours, drip off, continue reaction 2 hours, obtain homogeneous transparent heavy-gravity polymers soln.
This polymers soln is joined in the 1000ml there-necked flask, start stirring, heat up, remove solvent treatment, the butylacetate boiling distillates, along with steaming of butylacetate, temperature progressively raises, and begins to vacuumize when temperature is raised to 150, sloughs the solvent acetic acid butyl ester under vacuum, reach 200 ℃ up to temperature, vacuum tightness reaches 10mmHg.While hot resin is poured out, be cooled to room temperature, obtain transparent brittle resin, its epoxy equivalent (weight) is 527, and softening temperature is 108 ℃, and second-order transition temperature is 60.4 ℃.
[embodiment 2]
Synthesizing of carboxyl polyester resin, filling a prescription is:
Terephthalic acid 304.7g
Hexanodioic acid 5g
Neopentyl glycol 217.3g
M-phthalic acid (acidolysis) 45g
Catalyzer 0.25g
Neopentyl glycol and catalyzer are joined in the 1000ml there-necked flask that has stirring, logical nitrogen pipe and reflux,, and start stirring, be heated to neopentyl glycol then and all melt with the air in the nitrogen replacement bottle; Add terephthalic acid and hexanodioic acid, heat up, esterification, dehydration reaches 240 ℃ up to top temperature; When the reactant clarification, beginning vacuumizes for the first time, and acid number bleeds off vacuum after dropping to below the 10mgKOH/g, adds acidolysis m-phthalic acid 45g; When the reflux head temperature descends, and acid number drops to 40mgKOH/g, vacuumizes for the second time, and acid number is reduced to about 26mgKOH/g, while hot discharging; Cooling obtains the water white transparency brittle resin, and measuring resinous acid value is 2 for 26.3mgKOH/g viscosity, 100mPa.s (200 ℃), and softening temperature is 110 ℃, second-order transition temperature is 63.3 ℃.
[embodiment 3]
Synthesizing of carboxyl acrylic resin, filling a prescription is:
Methacrylic acid (MA) 49.5g
Methyl methacrylate (MMA) 59.4g
Butyl acrylate (BuA) 109g
Vinylbenzene (St) 115.5g
Benzoyl peroxide (BPO) 25g
Toluene (solvent) 270g
Above monomer and initiator are mixed, have in the four-hole round-bottomed flask of reflux condensate device, add 270g toluene at 1000ml, feed nitrogen, air in the displacement bottle starts stirring, is warming up near 130 ℃, toluene begins to reflux, keep temperature-resistant, drip mix monomer, about 3 hours, drip off, continue reaction 2 hours, obtain homogeneous transparent heavy-gravity polymers soln.
This polymers soln is joined in the 1000ml there-necked flask, start stirring, heat up, remove solvent treatment, the toluene boiling distillates, along with steaming of toluene, temperature progressively raises, and begins to vacuumize when temperature is raised to 150 ℃, sloughs solvent toluene under vacuum, reach 200 ℃ up to temperature, vacuum tightness reaches 10mmHg.While hot resin is poured out, be cooled to room temperature, obtain transparent brittle resin, its acid number is 102mgKOH/g, and softening temperature is 108 ℃, and second-order transition temperature is 61 ℃.
[embodiment 4]
The preparation of powder coating, filling a prescription is:
Raw material consumption weight percent
Epoxy group(ing) acrylic resin 28g 11.7% in the example 1
Carboxyl polyester resin 120g 50.3% in the example 2
Carboxyl acrylic resin 7 2.9% in the example 3
TGIC?????????????????????????2??????????????0.8%
Resins, epoxy (E-12) 5 2.1%
Titanium dioxide 75g 31.4%
Flow agent PV5 1.5g 0.6%
St-yrax 0.5g 0.2%
Above material is pulverized mixing in the high-speed stirring pulverizer, extrude in twin screw extruder then, extrusion temperature is 110 ℃, and extrudate is cooled off, pulverizes, crosses 200 mesh sieves, obtains weather resistant low brightness paint powder.Mode with electrostatic spraying is coated on the model of oil removing, processing of rust removing, and voltage is 63KV.The model that spraying is good solidified 15 minutes down at 200 ℃, obtained scratch resistance low light coating preferably, listed in down by all other performances of model that national standard method is measured.
Gloss (60 °) 3
Shock resistance 〉=50cm
The sticking power one-level
Pencil hardness H
Accelerated deterioration (QUV) 〉=240 hour [embodiment 5-7] formulation for coating material is as shown in table 1, and all the other are identical with example 4
Table 1
Example | ?5 | ?6 | ?7 |
Epoxy group(ing) acrylic resin/g in the example 1 | ?25 | ?22 | ?19 |
Carboxy(l)polyester/g in the example 2 | ?120 | ?120 | ?120 |
Carboxyl acrylic resin/g in the example 3 | ?3 | ?5 | ?7 |
TGIC/g | ?2.5 | ?3 | ?3.5 |
Resins, epoxy (E-12)/g | ?5 | ?5 | ?5 |
Titanium dioxide/g | ?75 | ?75 | ?75 |
Flow agent/g | ?1.5 | ?1.5 | ?1.5 |
St-yrax/g | ?0.5 | ?0.5 | ?0.5 |
Glossiness | ?12 | ?19 | ?27 |
Shock strength | ?≥50cm | ?≥50cm | ?≥50cm |
Hardness | ?H | ?H | ?H |
Sticking power | One-level | One-level | One-level |
Accelerated deterioration (QUV) | 〉=240 hours | 〉=240 hours | 〉=240 hours |
Claims (8)
1. powder coating is characterized in that its major ingredient comprises:
(a) 5-35% epoxy group(ing) acrylic resin;
(b) 0-5% triglycidyl isocyanurate;
(c) 0-10% bisphenol A type epoxy resin;
(d) 30-65% carboxyl polyester resin;
(e) 0-15% carboxyl acrylic resin;
(f) 29.5-60% filler;
(g) 0.5-1% auxiliary agent.
2. powder coating according to claim 1, the epoxy equivalent (weight) that it is characterized in that used epoxy group(ing) acrylic resin is 300-1,200, number-average molecular weight is 2,000-10,000, softening temperature is 80-130 ℃, second-order transition temperature is 40-75 ℃.
3. powder coating according to claim 1 is characterized in that used carboxyl polyester resin acid number at 20-60mgKOH/g, and promptly number-average molecular weight is 1,900-8, and 500, softening temperature is 80-140 ℃, second-order transition temperature is 45-75 ℃.
4. powder coating according to claim 1 is characterized in that used carboxyl acrylic resin acid number at 30-200mgKOH/g, and softening temperature is 80-130 ℃, and second-order transition temperature is 40-75 ℃.
5. powder coating according to claim 1, the monomer that it is characterized in that containing in the epoxy group(ing) acrylic resin synthetic monomer epoxide group is (methyl) glycidyl acrylate; Other monomer is (methyl) alkyl acrylate and vinyl monomer.
6. powder coating according to claim 1, it is characterized in that the synthetic used monomer of carboxyl polyester resin is a polyfunctional monomer, polycarboxylic acid or acid anhydrides are terephthalic acids, m-phthalic acid, Tetra hydro Phthalic anhydride, hexanodioic acid, sebacic acid, Succinic Acid, 1, the 4-cyclohexane dicarboxylic acid, at least a or its mixture in the trimellitic acid 1,2-anhydride; Polyvalent alcohol is an ethylene glycol, neopentyl glycol, 1,4 cyclohexane dimethanol, trimethylolethane, at least a or its mixture in the TriMethylolPropane(TMP).
7. powder coating according to claim 1, the monomer that it is characterized in that containing in the carboxyl acrylic resin synthetic monomer carboxylic group is (methyl) vinylformic acid; Other monomer is (methyl) alkyl acrylate and vinyl monomer.
8. powder coating according to claim 1 is characterized in that epoxy group(ing) acrylic resin and carboxyl acrylic resin synthetic method are solution polymerization or letex polymerization or mass polymerization or suspension polymerization.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN 02115292 CN1202184C (en) | 2002-05-29 | 2002-05-29 | Powdered paint |
Applications Claiming Priority (1)
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CN 02115292 CN1202184C (en) | 2002-05-29 | 2002-05-29 | Powdered paint |
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CN1461783A true CN1461783A (en) | 2003-12-17 |
CN1202184C CN1202184C (en) | 2005-05-18 |
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CN102477247A (en) * | 2010-11-24 | 2012-05-30 | 海洋王照明科技股份有限公司 | Polyester resin bottom powder as well as lamp coated by same and coating method thereof |
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2002
- 2002-05-29 CN CN 02115292 patent/CN1202184C/en not_active Expired - Fee Related
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CN102618161B (en) * | 2012-04-16 | 2015-06-17 | 广东华江粉末科技有限公司 | Deeply matt polyurethane powder coating for outdoor use and production process for deeply matt polyurethane powder coating |
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