CN105273558B - A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint and preparation method thereof - Google Patents
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint and preparation method thereof Download PDFInfo
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- CN105273558B CN105273558B CN201510756183.4A CN201510756183A CN105273558B CN 105273558 B CN105273558 B CN 105273558B CN 201510756183 A CN201510756183 A CN 201510756183A CN 105273558 B CN105273558 B CN 105273558B
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Abstract
The invention discloses a kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, mainly it is made up of high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin, dodecanedioic acid, ultra-violet absorber, light stabilizer, levelling agent and other auxiliary agents, the high epoxide equivalent acrylic resin uses the high epoxide equivalent acrylic resin that superfine titanic oxide is modified, and low epoxide equivalent acrylic resin is low epoxide equivalent GMA type acrylic resins；The present invention reacts by using high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin and dodecanedioic acid, reduces the initial reaction temperature of powdery paints, realizes low-temperature setting；Aid in solidifying by low epoxide equivalent acrylic resin, improve the enough compactness of powder coating, and then improve the decay resistance of coating；The high epoxide equivalent acrylic resin being modified by using superfine titanic oxide obtains splendid ultraviolet radiation absorption and acted on, and improves the weather resistance of coating.
Description
Technical field
It is saturating more particularly, to a kind of low temperature curing type epoxy radicals acrylic acid the present invention relates to a kind of powder coating technology field
Bright powdery paints and preparation method thereof.
Background technology
As technology is constantly progressive, occurs a kind of new spraying coating process in the application of automobile aluminum wheel hub, the technique is
It is made up of for two layers bottom powder and transparent powder, its midsole powder is mainly the pure polyester powdery paints with excellent flow leveling, transparent powder
It is Acrylic transparent powder paint.
At present, the bottom powder of the aluminium wheels of low-temperature setting uses a large amount of on the market, but matched low-temperature solid
The Lacquer finish transparent powder of change does not have Related product.
For the solidification temperature of generally conventional clear top powder coatings at 175-200 DEG C, baking temperature is higher, among practical application
Energy consumption is higher, in addition, automobile aluminum wheel hub requirement has enough toughness to ensure impact resistance, solidification temperature is too high also to allow casting
The toughness for making aluminium wheels declines, and the toughness of aluminium wheels can be increased by reducing powder coating solidification temperature, reduce the production of enterprise
Energy consumption, reach the purpose of energy-conserving and environment-protective.
But solidify relative to 180 DEG C of ordinary temperatures, because the solidification temperature is relatively low, the coating of solidification is because solidify relatively not
It is enough to lose acetic acid salt spray (CASS) performance that preferable weather resistance and anti-copper accelerate completely.
Present invention seek to address that problems with：1st, the solidification temperature of clear top powder coatings is reduced to 150-160 DEG C, reduces enterprise
Industry energy consumption；2nd, increase the weather-proof performance of coating by the acrylic resin modified combination routine antioxidant of ultra-fine transparent titanium dioxide to increase
Add the performance that coating is weather-proof；3rd, ensure lacquer finish coating there is higher consistency under low-temperature setting so that coating have it is good
Acetic acid salt spray (CASS) corrosive nature that good anti-copper accelerates.
Patent that U.S.'s AT Dai Li and S Mo Lite-Li Mu Burgers are delivered " epoxy functional acrylic powder and
By its obtained powder coating ", number of patent application：200810108733.1 although the patent also uses epoxy functional acrylic
Resin, but the specific epoxide equivalent of used acrylic resin is not provided in the patent, and be at relatively high temperatures
Solidify (170-180 DEG C), belong to hot setting, not low-temperature setting (150-160 DEG C), do not introduce weather-proof under low-temperature setting
Property and decay resistance solution, in addition in the patent using acrylate copolymer flow ability modifying agent as levelling agent, the stream
The levelling agent that flat agent uses for conventional nontransparent powder, transparency are poor.
The content of the invention
An object of the present invention is to provide a kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the powder
Coating can be in 150~160 DEG C of solidifications, and ensure that coating has higher consistency, have good weather resistance and resist
The acetic acid salt spray corrosive nature that copper accelerates.
The second object of the present invention provides the preparation method of above-mentioned low temperature curing type epoxy radicals Acrylic transparent powder paint.
First purpose of the present invention is achieved through the following technical solutions：A kind of low temperature curing type epoxy radicals propylene
Sour transparent powder paint, mainly by high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin, dodecanedioic acid, purple
Ultraviolet absorbers, light stabilizer, levelling agent and other auxiliary agents composition, the high epoxide equivalent acrylic resin epoxide equivalent are
500-700g/eq, described low epoxide equivalent acrylic resin epoxide equivalent is 280~350g/eq.
Further, low temperature curing type epoxy radicals Acrylic transparent powder paint of the present invention is by following parts by weight
Each component is prepared：
The high epoxide equivalent acrylic resin uses the high epoxide equivalent acrylic resin that superfine titanic oxide is modified, and surpasses
Thin titania modified high epoxide equivalent acrylic resin has splendid ultraviolet radiation absorption effect, is greatly improved the resistance to of coating
Hou Xing, the high epoxide equivalent acrylic resin that superfine titanic oxide is modified is that method is prepared by the following procedure to be made：By 100 parts of epipodiums
The acrylic resin of oxygen equivalent adds reactor and is heated to 140-160 DEG C of melting completely, adds 0.1~5 part of modified superfine two
Titanium oxide, 10~20min is stirred, after both are fully coupled, discharging cooling, obtain superfine titanic oxide modified acroleic acid tree
Fat.
The modified superfine titanium dioxide is to pass through silane coupler modified ultrafine rutile phase titanium dioxide, and granularity is
1~1000nm, preferably 50~300nm.
The preparation method of the modified superfine titanium dioxide is as follows：Weigh the titanium dioxide that 1 part of Ultra-fine is 1~1000nm
Titanium, 20 parts of isopropanol is added, using ultrasonic 20-30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.02-
0.06 part of silane coupler, ultrasonic 3-5min, then constant temperature stirs 3~5min at 60-90 DEG C again, is then centrifuged for separating, obtains
To silane coupler modified superfine titanic oxide.
Low epoxide equivalent acrylic resin of the present invention is low epoxide equivalent GMA type acrylic resins, and it is by following
The starting monomer of parts by weight melt polymerization in the presence of initiator forms：
Above-mentioned raw materials monomer summation is 100 with initiator weight ratio:1~5.
The initiator is preferably dibenzoyl peroxide (BPO).
The preparation method of low epoxide equivalent GMA type acrylic resins of the present invention is as follows：It is by summation by weight
100 parts of styrene, methyl methacrylate, n-BMA and GMA starting monomers and 1-5 parts initiator mixing is equal
It is even, add in drop funnel, 300 parts of toluene are added in the three-necked flask equipped with agitator, reflux condenser and dropping funel
Solvent, start to stir, be warming up to 120 DEG C, after temperature is constant, at the uniform velocity instills the starting monomer dissolved with initiator, polymerize after 3h
Reaction terminates, and question response liquid is cooled to room temperature, changes synthesizer into vacuum distillation apparatus, is evaporated under reduced pressure to toluene solvant
Remove completely, you can low epoxide equivalent GMA type acrylic resins, the low epoxide equivalent GMA types acrylic resin ring of gained is made
Oxygen 280~350g/eq of equivalent, glass transition temperature Tg：45~50 DEG C, molecular weight 1000~3000.
Levelling agent of the present invention uses amino modified oligoester levelling agent, and the levelling agent has the high grade of transparency.
The light stabilizer is hindered amine.
Other auxiliary agents are commercial coating conven-tional adjuvants, preferably benzoin (alias styrax).
Second goal of the invention of the present invention is achieved through the following technical solutions：A kind of low temperature curing type epoxy radicals
The preparation method of Acrylic transparent powder paint, comprises the following steps：
(1) high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin, dodecanedioic acid, stream are weighed by proportioning
Flat agent, ultra-violet absorber, light stabilizer and other auxiliary agents, are placed in compounding jar, are sufficiently mixed and crush, and obtain mixing pre-composition
Material；
(2) extruder extrusion temperature is set, mixing premix material is sent into double screw extruder and extruded；
(3) material after extruding is packed after tabletting machine, cooling, crushing, screening.
The time that each component is mixed and crushed in the step (1) is 5~20 minutes, and the preferable time is 5~15 minutes,
The optimal time is 5~10 minutes.
The extruder selects crawler type double screw extruder, and the extrusion temperature includes area's extrusion temperature and 2nd area are squeezed
Go out temperature, area's extrusion temperature is 80~100 DEG C, and two area's extrusion temperatures are 80~120 DEG C.
Diameter of particle of the extrudate after pulverizer crushes and sieves in the step (3) is 1~100 μm, preferably 1~
80 μm, more preferably 10~60 μm, diameter of particle refer to the equivalent grain size D of powder50。
The coating process of powdery paints that the present invention prepares gained is：With high-pressure electrostatic spray gun, surface is coated at
On the metal base of reason, thickness is generally 60~150 μm, and 150-160 DEG C of solidification temperature, hardening time is 15~25 minutes, is adopted
Solidified with curing oven.
Metal base of the present invention is the cast member of aluminium and its alloy, such as aluminium wheel or automobile interior furnishings part, and most
It is the base material cleaned by pretreatment well, such as pretreatment was carried out with trbasic zinc phosphate or ferric phosphate.
The present invention has advantages below compared with prior art：
(1) present invention is by using high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin and dodecane two
Acid reaction, the initial reaction temperature of powdery paints is reduced, realize 150~160 DEG C of low-temperature settings.
(2) acrylic acid powder coatings weather resistance when solidifying for 150-160 DEG C is poor, changes by using superfine titanic oxide
Property acrylic resin combine conventional antioxidant and obtain splendid ultraviolet radiation absorption effect, greatly improve the weather resistance of coating, and
Xanthochromia caused by when solving the problems, such as to lift the weatherability more conventional ultra-violet light absorbers of addition.
(3) present invention uses the low epoxide equivalent GMA type resins of 280~350g/eq, relative to the GMA types of high epoxide equivalent
Acrylic resin, add the consistency of coating, improve coating because of the decay resistance of the relatively low loss of solidification temperature, make painting
Layer has acetic acid salt spray (CASS) corrosive nature that good anti-copper accelerates.
Embodiment
Unless otherwise indicated, all technique and all embodiments are all carried out in the gentle pressure of normal temperature.
Scope listed by this paper all includes end value and can be mutually combined.
Herein, term " powdery paints " represents powder paint compositions, and term " powder coating " represents to be applied by powder
The coating that feed composition is formed.
Some instantiations are set forth below, and the present invention will be described, it is necessary to it is pointed out here that be specific examples below
It is served only for that the invention will be further described, does not represent limiting the scope of the invention.Other people make according to the present invention
Some it is nonessential adjustment and modification still fall within protection scope of the present invention.
Different product and different model of each component from the production of various companies in following examples：
The high epoxide equivalent acrylic resin that superfine titanic oxide is modified：Used acrylic resin is SZ002, Guangzhou
YueYi Chemical Co., Ltd.s of city.
Low epoxide equivalent GMA type acrylic resins：Hold up a day resin in Guangzhou
Amino modified oligoester levelling agent：TROY, 570CFL
Ultra-violet absorber：Tinuvin 327, Qi Ba fine chemistry company
Hindered amine：Tinuvin 783, Qi Ba fine chemistry company
Benzoin：Commercially available routine
Ultrafine rutile phase titanium dioxide：1~1000nm of granularity, preferably 50~300nm, it is commercially available
Silane coupler：One or both of KH-550, KH-570.
Embodiment 1
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the low temperature curing type epoxy radicals propylene of the present embodiment
Sour transparent powder paint, its component and weight are：
Wherein,
The high epoxide equivalent acrylic resin epoxide equivalent that the superfine titanic oxide is modified is 500~700g/eq, its by
Superfine titanic oxide silane coupler modified KH-550 is modified gained, preparation method to high epoxide equivalent acrylic resin
It is as follows：
(1) modified superfine titanium dioxide is prepared：1 part of superfine titanic oxide (100~300nm of granularity) is weighed, adds 20 parts
Isopropanol, using ultrasonic 30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.02 part of coupling agent, ultrasound
3min, then constant temperature stirs 3 minutes at 90 DEG C again, is then centrifuged for separating, and obtains the superfine titanic oxide of KH-550 modifications.
(2) the high epoxide equivalent acrylic resin of superfine titanic oxide modification is prepared：By 100 parts high epoxide equivalent acrylic acid
Resin adds reactor and is heated to 150 DEG C of meltings completely, adds the modified superfine titanium dioxide obtained by 2 parts of above-mentioned preparations, stirring
10~20min, treat that silane idol chain agent is fully coupled with resin, discharging cooling, obtain the acrylic acid tree of superfine titanic oxide modification
Fat.
The epoxide equivalent of the low epoxide equivalent GMA type acrylic resins is 280~350g/eq, by following parts by weight
Monomer melt polymerization in the presence of initiator B PO forms：
The weight ratio of above-mentioned monomer summation and initiator is 100:2, specific preparation method is as follows：It is by summation by weight
100 parts of styrene, methyl methacrylate, n-BMA and GMA starting monomers and 2 parts of initiator B PO mixing
Uniformly, add in drop funnel, 300 parts of first are added in the three-necked flask equipped with agitator, reflux condenser and dropping funel
Benzene solvent, start to stir, be warming up to 120 DEG C, after temperature is constant, at the uniform velocity instills the starting monomer dissolved with initiator, gather after 3h
Close reaction to terminate, question response liquid is cooled to room temperature, changes synthesizer into vacuum distillation apparatus, is evaporated under reduced pressure molten to toluene
Agent removes completely, you can low epoxide equivalent GMA type acrylic resins, the low epoxide equivalent GMA type acrylic resins of gained is made
Glass transition temperature Tg：45~50 DEG C, molecular weight 1000~3000.
The low temperature curing type epoxy radicals Acrylic transparent powder paint preparation method of the present embodiment is as follows：
(1) the high epoxide equivalent acrylic resin of superfine titanic oxide modification, low epoxide equivalent GMA types third are weighed by proportioning
Olefin(e) acid resin, dodecanedioic acid, amino modified oligoester levelling agent, ultra-violet absorber, hindered amine, benzoin, are placed in batch mixing
Cylinder, it is sufficiently mixed and crushes 5~10min, obtains mixing premix material.
(2) material after being pre-mixed is extruded into JFY-30 type crawler types double screw extruder, sets the area of extrusion temperature one
For 90~100 DEG C, 2nd area are 85~95 DEG C.
(3) it is 30~45 μm that the material after extruding is ground into particle diameter (equivalent grain size D50) through tabletting, cooling, pulverizer
Powder, then sieve, pack, low temperature curing type epoxy radicals Acrylic transparent powder paint is made.
The coating process of powdery paints that the present embodiment prepares gained is：With high-pressure electrostatic spray gun, surface process is coated on
On the automobile aluminum wheel hub ground of processing, application thickness is 60-120 μm, 155 DEG C of solidification temperature, and hardening time is 20 minutes, is used
Curing oven is solidified, and obtains finished automotive aluminium wheels Lacquer finish acrylic clear powder coatings, and coating performance is as follows：
| Detection project | Test stone or method | Assay |
| Outward appearance | / | Flat smooth, excellent transparency |
| CASS is tested | GM4476P, 240h | 2mm is qualified |
| Q-UV-A lamps | GB/T14552,340nm | 1600h light-protection rates 90% |
| Rubble impact test | GM9508P | 8 grades |
Embodiment 2
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the low temperature curing type epoxy radicals propylene of the present embodiment
Sour transparent powder paint, its component and weight are：
Wherein,
The high epoxide equivalent acrylic resin epoxide equivalent that the superfine titanic oxide is modified is 500~700g/eq, its by
Superfine titanic oxide silane coupler modified KH-550 is modified gained, preparation method to high epoxide equivalent acrylic resin
It is as follows：
(1) modified superfine titanium dioxide is prepared：1 part of superfine titanic oxide (100~300nm of granularity) is weighed, adds 20 parts
Isopropanol, using ultrasonic 30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.04 part of coupling agent, ultrasound
3min, then constant temperature stirs 3 minutes at 80 DEG C again, is then centrifuged for separating, and obtains the superfine titanic oxide of KH-550 modifications.
(2) the high epoxide equivalent acrylic resin of superfine titanic oxide modification is prepared：By 100 parts high epoxide equivalent acrylic acid
Resin adds reactor and is heated to 155 DEG C of meltings completely, adds the modified superfine titanium dioxide obtained by 0.5 part of above-mentioned preparation, stirs
20min is mixed, treats that silane idol chain agent is fully coupled with resin, discharging cooling, obtains the acrylic resin of superfine titanic oxide modification.
The epoxide equivalent of the low epoxide equivalent GMA type acrylic resins is 280~350g/eq, by following parts by weight
Monomer melt polymerization in the presence of initiator forms：
The weight ratio of above-mentioned monomer summation and initiator is 100:2, the preparation side of low epoxide equivalent GMA type acrylic resins
Method is such as embodiment 1.
The low temperature curing type epoxy radicals Acrylic transparent powder paint preparation method of the present embodiment is as follows：
(1) the high epoxide equivalent acrylic resin of superfine titanic oxide modification, low epoxide equivalent GMA types third are weighed by proportioning
Olefin(e) acid resin, dodecanedioic acid, amino modified oligoester levelling agent, ultra-violet absorber, hindered amine, benzoin, are placed in batch mixing
Cylinder, it is sufficiently mixed and crushes 10min, obtains mixing premix material.
(2) material after being pre-mixed is extruded into JFY-30 type crawler types double screw extruder, sets the area of extrusion temperature one
For 90~100 DEG C, 2nd area are 85~95 DEG C.
(3) it is 25~45 μm that the material after extruding is ground into particle diameter (equivalent grain size D50) through tabletting, cooling, pulverizer
Powder, then sieve, pack, low temperature curing type epoxy radicals Acrylic transparent powder paint is made.
The present embodiment prepares the coating process of the powdery paints of gained with embodiment 1, obtains finished automotive aluminium wheels Lacquer finish
Acrylic clear powder coatings, coating performance are as follows：155 DEG C/20min solidifies
| Detection project | Test stone or method | Assay |
| Outward appearance | / | Flat smooth, excellent transparency |
| CASS is tested | GM4476P, 240h | 3mm is qualified |
| Q-UV-A lamps | GB/T14552,340nm | 1400h light-protection rates 90% |
| Rubble impact test | GM9508P | 8 grades |
Embodiment 3
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the low temperature curing type epoxy radicals propylene of the present embodiment
Sour transparent powder paint, its component and weight are：
Wherein,
The high epoxide equivalent acrylic resin epoxide equivalent that the superfine titanic oxide is modified is 500~700g/eq, its by
Superfine titanic oxide silane coupler modified KH-570 is modified gained, preparation method to high epoxide equivalent acrylic resin
It is as follows：
(1) modified superfine titanium dioxide is prepared：1 part of superfine titanic oxide (100~600nm of granularity) is weighed, adds 20 parts
Isopropanol, using ultrasonic 30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.04 part of coupling agent, ultrasound
3min, then constant temperature stirs 4 minutes at 80 DEG C again, is then centrifuged for separating, and obtains the superfine titanic oxide of KH-570 modifications.
(2) the high epoxide equivalent acrylic resin of superfine titanic oxide modification is prepared：By 100 parts high epoxide equivalent acrylic acid
Resin adds reactor and is heated to 155 DEG C of meltings completely, adds the modified superfine titanium dioxide obtained by 1 part of above-mentioned preparation, stirring
20min, treat that silane idol chain agent is fully coupled with resin, discharging cooling, obtain the acrylic resin of superfine titanic oxide modification.
The epoxide equivalent of the low epoxide equivalent GMA type acrylic resins is 280~350g/eq, by following parts by weight
Monomer melt polymerization in the presence of initiator forms：
The weight ratio of above-mentioned monomer summation and initiator is 100:2, the preparation side of low epoxide equivalent GMA type acrylic resins
Method is such as embodiment 1.
The low temperature curing type epoxy radicals Acrylic transparent powder paint preparation method of the present embodiment is as follows：
(1) the high epoxide equivalent acrylic resin of superfine titanic oxide modification, low epoxide equivalent GMA types third are weighed by proportioning
Olefin(e) acid resin, dodecanedioic acid, amino modified oligoester levelling agent, ultra-violet absorber, hindered amine, benzoin, are placed in batch mixing
Cylinder, it is sufficiently mixed and crushes 10min, obtains mixing premix material.
(2) material after being pre-mixed is extruded into JFY-30 type crawler types double screw extruder, sets the area of extrusion temperature one
For 90~100 DEG C, 2nd area are 85~95 DEG C.
(3) it is 25~40 μm that the material after extruding is ground into particle diameter (equivalent grain size D50) through tabletting, cooling, pulverizer
Powder, then sieve, pack, low temperature curing type epoxy radicals Acrylic transparent powder paint is made.
The present embodiment prepares the coating process of the powdery paints of gained with embodiment 1, obtains finished automotive aluminium wheels Lacquer finish
Acrylic clear powder coatings, coating performance are as follows：155 DEG C/20min solidifies
| Detection project | Test stone or method | Assay |
| Outward appearance | / | Flat smooth, excellent transparency |
| CASS is tested | GM4476P, 240h | 3mm is qualified |
| Q-UV-A lamps | GB/T14552,340nm | 1500h light-protection rates 90% |
| Rubble impact test | GM9508P | 9 grades |
Embodiment 4
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the low temperature curing type epoxy radicals propylene of the present embodiment
Sour transparent powder paint, its component and weight are：
Wherein,
The high epoxide equivalent acrylic resin epoxide equivalent that the superfine titanic oxide is modified is 500~700g/eq, its by
Superfine titanic oxide silane coupler modified KH-570 is modified gained, preparation method to high epoxide equivalent acrylic resin
It is as follows：
(1) modified superfine titanium dioxide is prepared：1 part of superfine titanic oxide (100~600nm of granularity) is weighed, adds 20 parts
Isopropanol, using ultrasonic 30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.04 part of coupling agent, ultrasound
3min, then constant temperature stirs 4 minutes at 80 DEG C again, is then centrifuged for separating, and obtains the superfine titanic oxide of KH-570 modifications.
(2) the high epoxide equivalent acrylic resin of superfine titanic oxide modification is prepared：By 100 parts high epoxide equivalent acrylic acid
Resin adds reactor and is heated to 160 DEG C of meltings completely, adds the modified superfine titanium dioxide obtained by 0.1 part of above-mentioned preparation, stirs
20min is mixed, treats that silane idol chain agent is fully coupled with resin, discharging cooling, obtains the acrylic resin of superfine titanic oxide modification.
The epoxide equivalent of the low epoxide equivalent GMA type acrylic resins is 280~350g/eq, by following parts by weight
Monomer melt polymerization in the presence of initiator forms：
The weight ratio of above-mentioned monomer summation and initiator is 100:2, the preparation side of low epoxide equivalent GMA type acrylic resins
Method is such as embodiment 1.
The low temperature curing type epoxy radicals Acrylic transparent powder paint preparation method of the present embodiment is as follows：
(1) the high epoxide equivalent acrylic resin of superfine titanic oxide modification, low epoxide equivalent GMA types third are weighed by proportioning
Olefin(e) acid resin, dodecanedioic acid, amino modified oligoester levelling agent, ultra-violet absorber, hindered amine, benzoin, are placed in batch mixing
Cylinder, it is sufficiently mixed and crushes 10min, obtains mixing premix material.
(2) material after being pre-mixed is extruded into JFY-30 type crawler types double screw extruder, sets the area of extrusion temperature one
For 90~100 DEG C, 2nd area are 85~95 DEG C.
(3) it is 25~45 μm that the material after extruding is ground into particle diameter (equivalent grain size D50) through tabletting, cooling, pulverizer
Powder, then sieve, pack, low temperature curing type epoxy radicals Acrylic transparent powder paint is made.
The present embodiment prepares the coating process of the powdery paints of gained with embodiment 1, obtains finished automotive aluminium wheels Lacquer finish
Acrylic clear powder coatings, coating performance are as follows：155 DEG C/20min solidifies
| Detection project | Test stone or method | Assay |
| Outward appearance | / | Flat smooth, excellent transparency |
| CASS is tested | GM4476P, 240h | 3mm is qualified |
| Q-UV-A lamps | GB/T14552,340nm | 1000h light-protection rates 90% |
| Rubble impact test | GM9508P | 7 grades |
Embodiment 5
A kind of low temperature curing type epoxy radicals Acrylic transparent powder paint, the low temperature curing type epoxy radicals propylene of the present embodiment
Sour transparent powder paint, its component and weight are：
Wherein,
The high epoxide equivalent acrylic resin epoxide equivalent that the superfine titanic oxide is modified is 500~700g/eq, its by
Superfine titanic oxide silane coupler modified KH-570 is modified gained, preparation method to high epoxide equivalent acrylic resin
It is as follows：
(1) modified superfine titanium dioxide is prepared：1 part of superfine titanic oxide (100~600nm of granularity) is weighed, adds 20 parts
Isopropanol, using ultrasonic 30min under Ultrasound Instrument normal temperature, obtain unit for uniform suspension, add 0.06 part of coupling agent, ultrasound
3min, then constant temperature stirs 4 minutes at 80 DEG C again, is then centrifuged for separating, and obtains the superfine titanic oxide of KH-570 modifications.
(2) the high epoxide equivalent acrylic resin of superfine titanic oxide modification is prepared：By 100 parts high epoxide equivalent acrylic acid
Resin adds reactor and is heated to 155 DEG C of meltings completely, adds the modified superfine titanium dioxide obtained by 5 parts of above-mentioned preparations, stirring
20min, treat that silane idol chain agent is fully coupled with resin, discharging cooling, obtain the acrylic resin of superfine titanic oxide modification.
The epoxide equivalent of the low epoxide equivalent GMA type acrylic resins is 280~350g/eq, by following parts by weight
Monomer melt polymerization in the presence of initiator forms：
The weight ratio of above-mentioned monomer summation and initiator is 100:2, the preparation side of low epoxide equivalent GMA type acrylic resins
Method is such as embodiment 1.
The low temperature curing type epoxy radicals Acrylic transparent powder paint preparation method of the present embodiment is as follows：
(1) the high epoxide equivalent acrylic resin of superfine titanic oxide modification, low epoxide equivalent GMA types third are weighed by proportioning
Olefin(e) acid resin, dodecanedioic acid, amino modified oligoester levelling agent, ultra-violet absorber, hindered amine, benzoin, are placed in batch mixing
Cylinder, it is sufficiently mixed and crushes 10min, obtains mixing premix material.
(2) material after being pre-mixed is extruded into JFY-30 type crawler types double screw extruder, sets the area of extrusion temperature one
For 90~100 DEG C, 2nd area are 85~95 DEG C.
(3) it is 25~45 μm that the material after extruding is ground into particle diameter (equivalent grain size D50) through tabletting, cooling, pulverizer
Powder, then sieve, pack, low temperature curing type epoxy radicals Acrylic transparent powder paint is made.
The present embodiment prepares the coating process of the powdery paints of gained with embodiment 1, obtains finished automotive aluminium wheels Lacquer finish
Acrylic clear powder coatings, coating performance are as follows：155 DEG C/20min solidifies
| Detection project | Test stone or method | Assay |
| Outward appearance | / | Flat smooth, poor transparency |
| CASS is tested | GM4476P, 240h | 3mm is qualified |
| Q-UV-A lamps | GB/T14552,340nm | 1800h light-protection rates 90% |
| Rubble impact test | GM9508P | 7 grades |
Above-described embodiment 1 to 5 can be seen that：
(1) embodiment 1 to embodiment 5 is respectively provided with the acetic acid salt spray corrosivity that good impact resistance and anti-copper accelerate
Energy；
(2) powder coating of embodiment 1 to embodiment 5 exposes more than 1000h light-protection rates to the open air up to 90% under Q-UV-A lamps,
Preferable weatherability is respectively provided with, and modification contained in the high epoxide equivalent acrylic resin being modified with superfine titanic oxide surpasses
The lifting of the content of thin titanium dioxide, weatherability may be implemented under Q-UV-A lamps expose to the open air 1800h light-protection rates up to 90% (embodiment 5,
Modified superfine titanium dioxide for high epoxide equivalent acrylic resin dosage 5%), excellent in weather, but now relative transparency
Difference, therefore, the high epoxide equivalent acrylic resin of superfine titanic oxide modification can be drawn due to containing modified superfine titanium dioxide
The advantages of with durability of coating is improved, but the modified superfine content of titanium dioxide contained by it should not be excessive, not so can influence to apply
Layer transparency, therefore, modified superfine amount of titanium is preferably the 0.3%~2% of high epoxide equivalent acrylic resin dosage
(lifting of 0.1% weatherability is little, and 5% influences coating transparency).
Table：Embodiment 1 to the durability of coating of embodiment 5 contrasts
Described above, only presently preferred embodiments of the present invention is not intended to limit the invention, every skill according to the present invention
Any trickle amendment, equivalent substitution and the improvement that art is substantially made to above example, should be included in technical solution of the present invention
Protection domain in.
Claims (3)
1. a kind of solidification temperature is 150-160 DEG C of low temperature curing type epoxy radicals Acrylic transparent powder paint, by following weight
The each component of part is prepared：
Characterized in that, the high epoxide equivalent acrylic resin epoxide equivalent is 500-700g/eq, described low epoxide equivalent
Acrylic resin epoxide equivalent is 280~350g/eq；
The levelling agent uses amino modified oligoester levelling agent；
The light stabilizer is hindered amine；
Other auxiliary agents are benzoin；
The high epoxide equivalent acrylic resin that the high epoxide equivalent acrylic resin is modified using superfine titanic oxide, ultra-fine two
The high epoxide equivalent acrylic resin that titanium oxide is modified be by high epoxide equivalent acrylic resin and modified superfine titanium dioxide by
100:0.5~2 weight is than being made；
The modified superfine titanium dioxide be pass through silane coupler modified ultrafine rutile phase titanium dioxide, granularity be 50~
300nm；
Described low epoxide equivalent acrylic resin is low epoxide equivalent GMA type acrylic resins, its by following parts by weight original
Material list body melt polymerization in the presence of initiator dibenzoyl peroxide forms：
Above-mentioned raw materials monomer summation is 100 with initiator weight ratio:1~5.
2. a kind of preparation method of low temperature curing type epoxy radicals Acrylic transparent powder paint as claimed in claim 1, it is special
Sign is, comprises the following steps：
(1) by proportioning weigh high epoxide equivalent acrylic resin, low epoxide equivalent acrylic resin, dodecanedioic acid, levelling agent,
Ultra-violet absorber, light stabilizer and other auxiliary agents, are placed in compounding jar, are sufficiently mixed and crush, and obtain mixing premix material；
(2) extruder extrusion temperature is set, mixing premix material is sent into double screw extruder and extruded；
(3) material after extruding is packed after tabletting machine, cooling, crushing, screening.
3. the preparation method of low temperature curing type epoxy radicals Acrylic transparent powder paint according to claim 2, its feature
It is, the extrusion temperature includes area's extrusion temperature and two area's extrusion temperatures, and area's extrusion temperature is 80~100 DEG C, 2nd area
Extrusion temperature is 80~120 DEG C.
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| CN107151468B (en) * | 2016-03-04 | 2020-05-15 | 中国石油化工股份有限公司 | Acrylic resin powder composition, coating and application |
| CN106366809B (en) * | 2016-08-30 | 2018-08-28 | 安徽美佳新材料股份有限公司 | A kind of high-impact automobile clear top powder coatings |
| CN106543862A (en) * | 2016-10-18 | 2017-03-29 | 铜陵市肆得科技有限责任公司 | A kind of damping vibration attenuation expediting setting type composite epoxy antirust powdery paints for automobile chassis and preparation method thereof |
| CN106519912A (en) * | 2016-10-18 | 2017-03-22 | 铜陵市肆得科技有限责任公司 | Hybrid ultra-high-molecular-weight polyethylene toughening-modified composite epoxy anti-rust powder coating for automotive chassis and preparation method thereof |
| CN107868584B (en) * | 2017-11-14 | 2020-09-08 | 擎天材料科技有限公司 | Matte transparent powder coating for automobile aluminum hub finish and preparation method thereof |
| CN110003763B (en) * | 2019-03-01 | 2021-07-23 | 广东华润涂料有限公司 | Two-component water-based epoxy resin paint |
| CN115746640B (en) * | 2022-11-11 | 2024-03-26 | 擎天材料科技有限公司 | Anti-indentation acrylic transparent powder coating |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6407181B1 (en) * | 2000-08-21 | 2002-06-18 | Rohm And Haas Company | Low temperature curing powder coating for producing reduced gloss, weatherable coatings |
| CN1708561A (en) * | 2002-11-07 | 2005-12-14 | 舒飞士特种化工有限公司 | Powder coating compositions |
| CN105017871A (en) * | 2015-07-13 | 2015-11-04 | 华南理工大学 | Ultraviolet-proof exterior wall coating and preparation method therefor |
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2015
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6407181B1 (en) * | 2000-08-21 | 2002-06-18 | Rohm And Haas Company | Low temperature curing powder coating for producing reduced gloss, weatherable coatings |
| CN1708561A (en) * | 2002-11-07 | 2005-12-14 | 舒飞士特种化工有限公司 | Powder coating compositions |
| CN105017871A (en) * | 2015-07-13 | 2015-11-04 | 华南理工大学 | Ultraviolet-proof exterior wall coating and preparation method therefor |
Non-Patent Citations (1)
| Title |
|---|
| 耐候低光粉末涂料用丙烯酸树脂的合成研究;顾宇昕等;《现代涂料与涂装》;20030531(第5期);第17页右栏第2-3段，第18页右栏第4段 * |
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