CN101016434A - Ultraviolet light ultra-low-temperature solidity powder coating - Google Patents

Ultraviolet light ultra-low-temperature solidity powder coating Download PDF

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Publication number
CN101016434A
CN101016434A CN 200710034469 CN200710034469A CN101016434A CN 101016434 A CN101016434 A CN 101016434A CN 200710034469 CN200710034469 CN 200710034469 CN 200710034469 A CN200710034469 A CN 200710034469A CN 101016434 A CN101016434 A CN 101016434A
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CN
China
Prior art keywords
temperature
powder coating
irgacure
epoxy
resin
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CN 200710034469
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Chinese (zh)
Inventor
王海广
赵延良
冯伟云
李新洲
李晶
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湖南至诚涂料有限公司
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Priority to CN 200710034469 priority Critical patent/CN101016434A/en
Publication of CN101016434A publication Critical patent/CN101016434A/en

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Abstract

The invention discloses a second generation ultraviolet light ultra-low temperature solidifying powder coating, which comprises the following steps: allocating modified epoxy resin, modified polyester resin, polysiloxane resin, Irgacure 651/Irgacure 2959 compositing type light trigger, compositing nanometer type CaCO3/ SiO2, hardener, solidifying accelerant, leveling agent, degasifier, glossing agent, white carbon black and filling material; introducing soft molecular chain segment in polyester molecular chain; synthesizing hemi-hedral crystal type and non shaped unsaturated polyester resin as base resin; pre-mixing; grading; warm-melting; squeezing; pelleting; grinding; screening; spraying; setting the temperature of I section at 90-96 deg.c and II section at 80-83 deg.c. This invention can be used to plastic, wood, paper, electronic component, hardware, electric appliance, household electrical appliance, car, furniture, decoration and mechanical means domain.

Description

Ultraviolet light ultra-low-temperature solidity powder coating
Technical field
The present invention relates to a kind of powder coating, belong to field of fine chemical.
Background technology
Passed by the course of more than one thousand years of the development that coating is accompanied by human civilization, they beautify, protect and improved our life.Along with the progress of society and the raising of human knowledge's level, people have recognized the high hazardness of solvent based coating gradually, and promptly a large amount of organic volatiles dischargings are to the migration of a large amount of heavy metallic pigments that use in the destruction of ball ecological environment and the coating threat that is constituted that further develops to the mankind.Therefore, greenization is an important directions of coatings industry development from now on.Ultraviolet light polymerization (UV-curing) technology just is subjected to people's very big attention once coming out.The success of this curing process mainly depends on the advance of himself.Having advantages such as curing speed fast (thereby production efficiency height), less contamination, energy-conservation, cured product excellent performance, is a kind of eco-friendly green technology.German Bayer AG successfully develops curable wood coating so far from sixties Mo in last century, and radiation curing technology has obtained fast development over more than 40 year.We can say that UV-curing technology has entered into the every aspect that people produce and live.At present, the application of UV-curing technology aspect coating mainly concentrates on liquid ultraviolet light polymerization system, but a weak point of conventional liquid UV-light coating is, must add the reactive monomer thinner in the coating process for preparation to regulate the viscosity of coating, liquid prepolymer and reactive monomer have stronger pungency to human body, and the reactive monomer thinner also can partly infiltrate base material, and its influence to base material and environment also is difficult to determine.This also is why UV-light coating is so far less than the reason in the food product pack sector application.From back 20 years of eighties of last century so far, the output of powder coating rapidly increases.Since the reform and opening-up, the especially emergence of the household electrical appliances of the nineties in last century and furniture industry makes China's powder coating already obtain rare opportunity to develop.Powder coating heat constantly heats up, and research and development, production technique, coating equipment, construction application have all obtained breakthrough, and its output is only second to the U.S., occupies the second place of the world.According to statistics, national powder coating output calendar year 2001 is 170,000 tons, and 2002 is 200,000 tons, and 2003 is 250,000 tons, and rate of growth reaches 20%-30%, is higher than the rate of growth of world 15%-20%.World authoritative institution estimates that China's powder coating output in 2010 will reach 400,000-450,000 tons, and powder coating shared ratio is with more than half in industrial coating, so the future development of powder coating has a extensive future.The powder coating great advantage is friendly environment (VOC free discharging), good and economic, permanent outdoor weatherability and other performance.But also there is deficiency in powder coating: be the solidification value higher (180-220 ℃) of used heat reactive resin on the one hand, set time long (10-30min), this limits it can only be used for resistant substrates such as metal, and energy consumption is big, time-consuming relatively.On the other hand, the gentle curing initial stage of the melt-flow of thermofixation powder coating has necessarily overlapping, so that grasps badly a little, and the defective on the planeness will appear in coating, as headachy problems such as shrinkage cavity, tangerine peels.
And UV curing powder coating can address these problems, UV curing powder coating is the new coating technology that the powder coating processing technology combines with UV-curing technology, meet 4 " E " (the efficient Excellent performance of the economic Environmental environmental protection of Economic Effective brilliance) principle, have VOC free discharging, save the energy (power consumption only for the thermofixation powder coating 1/5～1/10), curing speed fast (0.1～10S), the production efficiency height, be fit to streamline production, be fit to apply advantages such as heat-sensitive substrate material.It combines the characteristics of traditional powder coating and UV-curing technology.Powder coating is different fully with traditional liquid coating, is complete solvent-free environment-friendly type coating, has that technology is simple, a save energy, non-environmental-pollution, production efficiency advantages of higher, is particularly suitable for the application of metal device.But heat curable powder coating processing temperature height, set time are grown, can not use on heat-sensitive substrate material.Because its fusion levelling carries out synchronously, flow time is short, is prone to phenomenons such as tangerine peel, shrinkage cavity, influences surface quality in addition.If make heat curable powder coating under baking, lower viscosity be arranged, be easy to levelling and finish reaction within a short period of time and form uniform cured paint film, just must reduce the second-order transition temperature of heat curable powder coating resin, improve its adaptability, this can make the stability in storage of heat curable powder coating be restricted.And UV curing powder coating exactly can overcome the above-mentioned defective of heat curable powder coating, so UV curing powder coating has more advantage.For example, the UV curing powder coating melt temperature is 100～140 ℃, and is lower than the melt temperature (177～200 ℃) of heat curable powder coating; Curing speed is in second, and (10～30min) is faster than the speed of heat curable powder coating; And make powder coating can be used for the application of heat-sensitive substrate material (paper, timber, temperature-sensitive alloy material etc.) or alloy thermo-sensitive material composite components such as (plastics, rubber); The powder of UV curing powder coating is to thermally-stabilised, so its processing is easier, can adopts common forcing machine processing, and can not occur crosslinked phenomenon because of processing temperature is high; UV curing powder coating can reach best melt-flow level state before ultraviolet light polymerization, guarantee paint film ideal planeness.Compare with the liquid coating of ultraviolet light polymerization, the raw material of UV curing powder coating is the resin of high molecular weight, has avoided the harm of reactive thinner, and shrinking percentage is low, to base material sticking power height; A UV curing powder coating application can form superior in quality paste paint film (75～125mm), reduced the coating material solidified numerous and diverse technology that repeatedly applies of liquid UV light; The powder that the UV curing powder coating spraying is splashed down is convenient to reclaim and is used, and is coating material solidified more economical than liquid UV light.Therefore, be that the UV curing powder coating of solvent-free environment-protection coating has more technical superiority, economic advantages and ecological dominance than heat curable powder coating and UV curable liquid coating equally.
Summary of the invention
The object of the present invention is to provide the wider and stronger modified version ultraviolet light ultra-low-temperature solidity powder coating of over-all properties of a kind of range of application, and the processing method for preparing a kind of ultraviolet light ultra-low-temperature solidity powder coating.
The technical solution adopted for the present invention to solve the technical problems is that realization the present invention implements when being three kinds of approach, comprises the modification of resin itself; The choose reasonable of light initiation system; The composite Nano CaCO of nucleocapsid structure 3/ SiO 2The application three combine.The purpose of implementing in the time of three kinds of approach is to seek a kind of well balanced system that has between package stability, meltbility, flowability and solidified nature, sets up large-scale experimental data base by experiment, filters out rational prescription; So that obtain the very low temperature ultraviolet light polymerization, good mechanical property, rete is smooth, strong adhesion, stable storing, the modified version ultraviolet light ultra-low-temperature solidity powder coating that range of application is extremely wide.
The invention provides a kind of ultraviolet light ultra-low-temperature solidity powder coating, its component and weight percent thereof are:
(a) modified epoxy 0-55%
(b) modified polyester resin 0-52%
(c) epoxy-silicone resin 0-10%
(d)Irgacure651/Irgacure2959????0.5％
(e) composite Nano type CaCO 3/ SiO 22%
(f) solidifying agent 4-8%
(g) curing catalyst 0.05-0.5%
(h) flow agent 0.1-1.0%
(i) air release agent 0.5-1.0%
(j) optical brightener 0.5-1.0%
(k) filler 30-45%
(l) white carbon black 0.1-0.6%
(m) pigment 0.5-8.0%
Resins, epoxy is conventional bisphenol A-type, oxirane value 0.11-0.13, softening temperature 84-88 ℃; The vibrin acid number is 45-75mgkOH/g, and softening temperature is 85-95 ℃, about 55 ℃ of second-order transition temperature; Epoxy-silicone resin is the low-molecular-weight epoxy resin modified siloxane.
Solidifying agent is to contain terminal hydroxy group and the macromolecular cpd (softening temperature 82-85 ℃, active ingredient equivalent 200-220) of holding amido, and curing catalyst is the imidazolinium compounds with ring amidine structure.
Auxiliary agent is a flow agent, air release agent, and optical brightener, its kind and consumption decide according to required color and colourity; Used filler is titanium dioxide or barium sulfate or barium carbonate or talcum powder, or the mixture of above-mentioned material.
Irgacure651/Irgacure2959 is commercially available light trigger, and structural formula is as follows respectively:
The processing method that the present invention prepares a kind of ultraviolet light ultra-low-temperature solidity powder coating is:
To in adjusting mixing machine, mix 5min after the accurate weighings of starting material such as modified resin, Irgacure651/Irgacure2959, solidifying agent promotor, auxiliary agent, color stuffing, melt extrude by the segmentation temperature that (I district temperature is 90-96 ℃, II district temperature is 80-83 ℃), compressing tablet, pulverize, operations such as screening, powder coating gets product.
The modified version ultraviolet light ultra-low-temperature solidity powder coating of the present invention's preparation, its mean particle size is 30-40 μ m, less than 100 μ m particle ratios greater than 100%, it is sprayed on the thick degreasing and rust removal cold-rolled steel sheet of 0.8mm, thickness 50-80 μ m, 80-100 ℃ of IR lamp baking 2-4 minute, stop 1-2 minute smooth, smooth, the uniform top coat of color and luster that just can obtain filming at 100-120 ℃ of ultra-violet lamp more then.Spraying method commonly used has: electrostatic spraying, friction spraying, the spraying of sulfuration bed etc., and better suited spraying method is electrostatic spraying, and spray voltage is controlled between the 60-80kv, and spray distance is at 15-30 centimetre.The glossiness of the coating minute surface of powder coating of the present invention after spraying, curing can be made into various photochromic and colorful colors: Gao Guang (＞85%), half light (85-50%), low light (50-20%), unglazed (＜20%), its photochromic color can be allocated (experimental technique is pressed GB/T9754-88 and measured, 60 °) arbitrarily; Bending≤2mm (pressing GB/T6742-86 measures); Resistance to impact shock (kgcm) is greater than 50 (pressing GB/T1732-93 measures); Pencil hardness 2H above (pressing GB/T6739-96 measures); Sticking power (cross-hatching is measured by GB/T9286-1996) is 1 grade; Drawing test is more than or equal to 8mm (pressing GB/T9753-88 measures); Salt-fog test is greater than 500hr qualified (pressing GB/T1771-91 measures); Warm test＞1000h is qualified (pressing GB/T1740-79 measures).
The invention has the beneficial effects as follows, can be under 100-120 ℃ of ultraviolet light conditions fast setting (time is in second), the coating after the curing is more taller than the routine techniques index of powder coating, has avoided solidifying film layer poor adhesive force and the not good enough defective of surperficial levelling under the common cold condition, has scientific formulation, solidification value is low, and set time is short, good mechanical property, rete is smooth, strong adhesion, the advantage of stable storing, and greatly reduce energy consumption.It is of wide application, over-all properties is very strong, can be widely used in fields such as five metals, electrical equipment, household electrical appliances, automobile, furniture, decoration, mechanical means, be specially adapted to the application of field of coating such as plastics, timber, paper and various thermo-sensitivity accessories that can not hot setting.
Embodiment:
Embodiment 1:
The raw material of the embodiment of the invention 1 powder coating is formed and weight percent sees Table one;
Table one:
Sequence number Title material Parts by weight/% Consumption/kg
????1 Modified epoxy ????27 ????27
????2 Modified polyester resin ????19.5 ????19.5
????3 Epoxy-silicone resin ????8 ????8
????4 Solidifying agent ????6 ????6
????5 Curing catalyst ????0.2 ????0.2
????6 ????Irgacure651/Irgacure ????2959 ????0.5 ????0.5
????7 Composite Nano type CaCO3/ SiO2 ????2 ????2
????8 Flow agent ????0.4 ????0.4
????9 Air release agent ????1 ????1
????10 Optical brightener ????1 ????1
????11 Titanium dioxide ????32 ????32
????12 White carbon black ????0.4 ????0.4
????13 Pigment ????2.0 ????2.0
Preparation method: with above modified epoxy, modified polyester resin, epoxy-silicone resin, Irgacure651/Irgacure2959, composite Nano type CaCO 3/ SiO 2, solidifying agent curing catalyst, flow agent, air release agent, optical brightener, white carbon black, filler, pigment melt extrude by batching → pre-mixing → segmentation temperature that (I district temperature is 90-96 ℃, II district temperature is 80-83 ℃) → compressing tablet → pulverizing → screening, the type that is improved ultraviolet light ultra-low-temperature solidity powder coating.
Resins, epoxy is conventional bisphenol A-type, oxirane value 0.11-0.13, softening temperature 84-88 ℃; The vibrin acid number is 45-75mgkOH/g, and softening temperature is 85-95 ℃, about 55 ℃ of second-order transition temperature; Epoxy-silicone resin is the low-molecular-weight epoxy resin modified siloxane.
Solidifying agent is to contain terminal hydroxy group and the macromolecular cpd (softening temperature 82-85 ℃, active ingredient equivalent 200-220) of holding amido, and curing catalyst is the imidazolinium compounds with ring amidine structure.Auxiliary agent is flow agent, air release agent, optical brightener.Filler is titanium dioxide, barium sulfate, barium carbonate, talcous mixture.
Modified version ultraviolet light ultra-low-temperature solidity powder coating of the present invention is sprayed on the cold model of degreasing and rust removal in the mode of electrostatic spraying, spray voltage is controlled between the 60-80kv, thickness 50-80 μ m, spray distance is at 15-30 centimetre, earlier 80-100 ℃ of IR lamp baking 2-4 minute, stopped 1-2 minute at 100-120 ℃ of ultra-violet lamp again, press national standard method and measure the every performance of model.Result such as table two;
Table two:
Embodiment 2-4:
The raw material composition of embodiment of the invention 2-4 powder coating and weight percent thereof are shown in following table three, and preparation method and performance test methods are identical with embodiment 1,80-100 ℃ of IR lamp baking 2-4 minute, stop 1-2 minute at 100-120 ℃ of ultra-violet lamp more earlier.
Resins, epoxy is conventional bisphenol A-type, oxirane value 0.11-0.13, softening temperature 84-88 ℃; The vibrin acid number is 45-75mgkOH/g, and softening temperature is 85-95 ℃, about 55 ℃ of second-order transition temperature; Epoxy-silicone resin is the low-molecular-weight epoxy resin modified siloxane.Solidifying agent is to contain terminal hydroxy group and the macromolecular cpd (softening temperature 80-83 ℃, active ingredient equivalent 200-220) of holding amido, and curing catalyst is the imidazolinium compounds with ring amidine structure.Filler is titanium dioxide or barium sulfate or barium carbonate or talcum powder.
Table three:

Claims (3)

1, a kind of ultraviolet light ultra-low-temperature solidity powder coating, its component and weight percent thereof are:
(a) modified epoxy 0-55%
(b) modified polyester resin 0-52%
(c) epoxy-silicone resin 0-10%
(d)Irgacure?651/Irgacure?2959?0.5％
(e) composite Nano type CaCO 3/ SiO 22%
(f) solidifying agent 4-8%
(g) curing catalyst 0.05-0.5%
(h) flow agent 0.1-1.0%
(i) air release agent 0.5-1.0%
(j) optical brightener 0.5-1.0%
(k) filler 30-45%
(1) white carbon black 0.1-0.6%
(m) pigment 0.5-8.0%;
Resin binder is for having introduced flexible molecule segmental hemihedral crystal type and unformed two kinds of unsaturated polyester resins, softening temperature 80-83 ℃, active ingredient equivalent 200-220; Light initiation system is Irgacure 651/Irgacure 2959 compound systems; The nano material that adds is SiO 2The composite Nano type CaCO of parcel 3/ SiO 2
Resins, epoxy is conventional bisphenol A-type, oxirane value 0.11-0.13, softening temperature 84-88 ℃; The vibrin acid number is 45-75mgkOH/g, and softening temperature is 85-95 ℃, about 55 ℃ of second-order transition temperature; Epoxy-silicone resin is the low-molecular-weight epoxy resin modified polyorganosiloxane.
2, ultraviolet light ultra-low-temperature solidity powder coating as claimed in claim 1 is characterized in that: with modified epoxy, modified polyester resin, Irgacure 651/Irgacure 2959 compound light triggers, composite Nano type CaCO 3/ SiO 2, epoxy-silicone resin, solidifying agent, curing catalyst, flow agent, air release agent, optical brightener, white carbon black, pigment, filler, by batching → pre-mixing → segmentation temperature melt extrude → processing method of compressing tablet → pulverizing → screening makes, the I district temperature that the segmentation temperature melt extrudes is 90-96 ℃, and II district temperature is 80-83 ℃.
3, a kind of ultraviolet light ultra-low-temperature solidity powder coating as claimed in claim 1 is characterized in that: described filler is titanium dioxide or barium sulfate or barium carbonate or talcum powder, or titanium dioxide, barium sulfate, barium carbonate, talcous mixture.
CN 200710034469 2007-02-13 2007-02-13 Ultraviolet light ultra-low-temperature solidity powder coating CN101016434A (en)

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Cited By (21)

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CN101805556A (en) * 2010-04-12 2010-08-18 安徽华辉塑业科技有限公司 Thermosetting powder coating with high tenacity
CN102311697A (en) * 2010-07-05 2012-01-11 湖南松井化学技术有限公司 Ultraviolet light or electron beam radiation curing powder coating
CN102690584A (en) * 2012-06-12 2012-09-26 天长市巨龙车船涂料有限公司 Epoxy resin powder paint and application thereof
CN103122199A (en) * 2013-02-27 2013-05-29 山东朗法博粉末涂装科技有限公司 Ultra-low-temperature curing dual-component powder coating and preparation method thereof
CN103131308A (en) * 2012-12-28 2013-06-05 广州擎天材料科技有限公司 High-low acid value bi-component end carboxyl polyester resin composition for super-weather-proof dry-blending extinction powder coatings and application of the same
CN103483993A (en) * 2013-09-03 2014-01-01 蚌埠市鸿安精密机械有限公司 Low-temperature curing powder paint
CN103497628A (en) * 2013-09-03 2014-01-08 蚌埠德美过滤技术有限公司 Improved ultraviolet-light ultralow-temperature-curable powdery paint
CN103497653A (en) * 2013-09-04 2014-01-08 安徽拓普森电池有限责任公司 Powdery paint for ceiling
CN103525269A (en) * 2013-09-24 2014-01-22 安徽锐视光电技术有限公司 Low-temperature curing heavy anticorrosive powder paint
CN103666216A (en) * 2013-11-29 2014-03-26 江苏帕齐尼铜业有限公司 Unsaturated polyester powder coating for copper
CN103965735A (en) * 2014-05-06 2014-08-06 张家港江南粉末涂料有限公司 Fast curing automobile balance part powder coating and production method thereof
CN104449200A (en) * 2013-09-25 2015-03-25 苏州裕丰装饰门窗有限公司 Heat-insulation heat-preservation powdered paint, preparation method and coating method of heat-insulation heat-preservation powdered paint, coating formed by using coating method and application of coating
CN104861835A (en) * 2015-05-19 2015-08-26 成都纳硕科技有限公司 Matrix resin of low-temperature cured powder coating
CN104893516A (en) * 2015-05-19 2015-09-09 成都纳硕科技有限公司 Preparation method of rapid light-cured powder coating
CN104910767A (en) * 2015-05-19 2015-09-16 成都纳硕科技有限公司 Fast light-curing powder paint
CN104910769A (en) * 2015-05-19 2015-09-16 成都纳硕科技有限公司 Powder coating containing talcum powder filler
CN106634478A (en) * 2016-11-22 2017-05-10 天长市金陵电子有限责任公司 Special high-weatherability coating for electrostatic spraying
CN106752767A (en) * 2016-12-12 2017-05-31 衡阳山泰化工有限公司 A kind of low temperature cured powder coating
CN106752759A (en) * 2016-11-22 2017-05-31 天长市金陵电子有限责任公司 A kind of electrostatic spraying special low temperature cured powder paint and preparation method thereof
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CN108300136A (en) * 2016-08-31 2018-07-20 东莞市金虹电子科技有限公司 A kind of preparation method and product of graphene heat radiation coating

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CN101805556A (en) * 2010-04-12 2010-08-18 安徽华辉塑业科技有限公司 Thermosetting powder coating with high tenacity
CN102311697A (en) * 2010-07-05 2012-01-11 湖南松井化学技术有限公司 Ultraviolet light or electron beam radiation curing powder coating
CN102690584A (en) * 2012-06-12 2012-09-26 天长市巨龙车船涂料有限公司 Epoxy resin powder paint and application thereof
CN103131308A (en) * 2012-12-28 2013-06-05 广州擎天材料科技有限公司 High-low acid value bi-component end carboxyl polyester resin composition for super-weather-proof dry-blending extinction powder coatings and application of the same
CN103131308B (en) * 2012-12-28 2016-01-20 广州擎天材料科技有限公司 A kind of be superly weather-proofly dry mixed extinction powder coating just acid number bicomponent terminal carboxyl polyester resin composition and application thereof
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CN103497628A (en) * 2013-09-03 2014-01-08 蚌埠德美过滤技术有限公司 Improved ultraviolet-light ultralow-temperature-curable powdery paint
CN103483993B (en) * 2013-09-03 2016-02-10 蚌埠市鸿安精密机械有限公司 A kind of low-temperature curable powder coating
CN103497653A (en) * 2013-09-04 2014-01-08 安徽拓普森电池有限责任公司 Powdery paint for ceiling
CN103497653B (en) * 2013-09-04 2016-03-16 安徽拓普森电池有限责任公司 A kind of top ceiling powder coating
CN103525269A (en) * 2013-09-24 2014-01-22 安徽锐视光电技术有限公司 Low-temperature curing heavy anticorrosive powder paint
CN104449200A (en) * 2013-09-25 2015-03-25 苏州裕丰装饰门窗有限公司 Heat-insulation heat-preservation powdered paint, preparation method and coating method of heat-insulation heat-preservation powdered paint, coating formed by using coating method and application of coating
CN103666216A (en) * 2013-11-29 2014-03-26 江苏帕齐尼铜业有限公司 Unsaturated polyester powder coating for copper
CN103965735A (en) * 2014-05-06 2014-08-06 张家港江南粉末涂料有限公司 Fast curing automobile balance part powder coating and production method thereof
CN104893516A (en) * 2015-05-19 2015-09-09 成都纳硕科技有限公司 Preparation method of rapid light-cured powder coating
CN104910767A (en) * 2015-05-19 2015-09-16 成都纳硕科技有限公司 Fast light-curing powder paint
CN104910769A (en) * 2015-05-19 2015-09-16 成都纳硕科技有限公司 Powder coating containing talcum powder filler
CN104861835A (en) * 2015-05-19 2015-08-26 成都纳硕科技有限公司 Matrix resin of low-temperature cured powder coating
CN107304326A (en) * 2016-04-25 2017-10-31 江门市东健粉末涂装科技有限公司 Powdery paints and preparation method thereof and the application in wood surface spraying
CN108300136A (en) * 2016-08-31 2018-07-20 东莞市金虹电子科技有限公司 A kind of preparation method and product of graphene heat radiation coating
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CN106752759A (en) * 2016-11-22 2017-05-31 天长市金陵电子有限责任公司 A kind of electrostatic spraying special low temperature cured powder paint and preparation method thereof
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