CN102786858A - Flame resistance epoxy resin powder paint - Google Patents
Flame resistance epoxy resin powder paint Download PDFInfo
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- CN102786858A CN102786858A CN2012101549464A CN201210154946A CN102786858A CN 102786858 A CN102786858 A CN 102786858A CN 2012101549464 A CN2012101549464 A CN 2012101549464A CN 201210154946 A CN201210154946 A CN 201210154946A CN 102786858 A CN102786858 A CN 102786858A
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Abstract
The invention provides an epoxy resin powder paint advantaged by excellent flame resistance and improved mechanical strength even without use of a halogen flame resistance agent. The flame resistance epoxy resin powder paint is a flame resistance epoxy resin powder paint comprising an epoxy resin, a curing agent, a filling material, a laser color former, and a phosphate flame resistance agent, and the thermal expansion coefficient of above glass transition temperature of the epoxy resin powder paint is lower than 10*10-5/DEG C.
Description
Technical field
The present invention relates to epoxy resin powder coating.
Background technology
In the past, used epoxy resin powder coating from the purpose of insulating package electric component, electronic unit.In order to ensure the security of electric component, electronic unit, also require such epoxy resin powder coating in insulating package is filmed, to have high flame retardancy to fire.Therefore in the composition of powder coating, cooperate and give all cpds of flame retardant resistance.
As the method for giving flame retardant resistance; For example; Proposition has also been implemented following the whole bag of tricks: reduce flammable resinous principle; A large amount of cooperate non-flame properties inorganic filling material, particularly a large amount of the cooperation contained crystal water and when burning, discharges crystal water and present the method for inorganic filling materials such as such white lake of flame retardant effect or Marinco H; The silicone resin that the used for epoxy resin incendivity is low or contain resin modified method of cyanurate ring etc.; What the most extensively implement is the method (for example patent documentation 1) that cooperates various halogenated flame retardants.
Patent documentation 1: japanese kokai publication hei 6-57101 communique
Summary of the invention
The present invention accomplishes in view of said circumstances, even a kind of epoxy resin powder coating that does not use halogenated flame retardant also to have excellent flame and improved physical strength is provided.
The physical strength of discovery epoxy resin powder coating such as contriver of the present invention depends on the above thermal expansivity of second-order transition temperature (Tg) of epoxy resin powder coating, thereby has accomplished the present invention.
In order to address the above problem, according to the present invention a kind of fire-retarded epoxy resin powder coating is provided, be the epoxy resin powder coating that contains epoxy resin, solidifying agent, packing material, laser chromogenic reagent and SULPHOSUCCINIC ACID ESTER flame retardant,
The above thermal expansivity of the Tg of above-mentioned epoxy resin powder coating is 10 * 10
-5/ ℃ below.
In an embodiment of the invention, with respect to the quality of above-mentioned epoxy resin powder coating, above-mentioned packing material is more than the 50 quality %.
In an embodiment of the invention, above-mentioned laser chromogenic reagent contains copper compound or zirconium compounds.
In an embodiment of the invention, above-mentioned packing material is a fused silica.
In an embodiment of the invention, above-mentioned solidifying agent contains acid anhydrides.
In an embodiment of the invention, the bending elastic modulus of above-mentioned epoxy resin powder coating is 1.0 * 10
4More than the MPa.
In an embodiment of the invention, the second-order transition temperature of above-mentioned epoxy resin powder coating is below 100 ℃.
In an embodiment of the invention, the packing that above-mentioned epoxy resin powder coating is used for electric component, electronic unit is filmed.
According to the present invention, even a kind of epoxy resin powder coating that does not use halogenated flame retardant also to have excellent flame and improved physical strength is provided.
Embodiment
Below fire-retarded epoxy resin powder coating of the present invention is described.In addition, "～" expression under the situation that does not have to specify above extremely below.
Fire-retarded epoxy resin powder coating of the present invention contains epoxy resin, solidifying agent, packing material, laser chromogenic reagent and SULPHOSUCCINIC ACID ESTER flame retardant, and the above thermal expansivity of Tg is 10 * 10
-5/ ℃ below.Here, above-mentioned Tg representes 2161 second-order transition temperatures that measure, that utilize thermo-mechanical analysis (TMA) method according to JIS C.
The epoxy resin that uses among the present invention then can use so long as in molecule, have at least one epoxy group(ing) and be non-halogenated epoxy resin and what be applied to general epoxy resin powder coating at room temperature is solid-state epoxy resin.As such epoxy resin, for example can enumerate bisphenol A-type, Bisphenol F type, bisphenol S type, phenol phenolic varnish type, cresols phenolic varnish type, biphenyl type, naphthalene type, aromatic amine type etc., but be not limited to these.Should explain that these can use separately, also can make up a plurality of uses.
The solidifying agent that uses among the present invention, according to the purpose of application of epoxy powder coating, can be with the multiple alone or in combination use of various solidifying agent.For example; Condenses, Dyhard RU 100 and the verivate thereof of aromatic amines such as diaminodiphenyl-methane or aniline resin, fatty amine and aliphatic dicarboxylic acid, various imidazoles or imidazolinium compounds, hexanodioic acid, sebacic acid, phthalic acid, toxilic acid, trimellitic acid, UVNUL MS-40 dicarboxylicacid, UVNUL MS-40 tetracarboxylic acid, Pyromellitic Acid etc. be can enumerate and dicarboxylicacid or its acid anhydrides gathered; Two hydrazides such as hexanodioic acid, phthalic acid; As the phenolic varnish class with the condenses of aldehyde such as phenol, cresols, xylenol, dihydroxyphenyl propane, carboxylic acid amide, methylolation melamine class, block type isocyanide urea ester class etc.Wherein, the angle of the curing characteristics of the powder coating that obtains from raising, the solidifying agent of preferred anhydrides system.
Can be according to the kind adjustment solidifying agent of epoxy resin that uses and solidifying agent and the ratio of epoxy resin.Preferably generally with respect to epoxy resin, solidifying agent uses in 0.6～1.2 normal scope.If above-mentioned scope then can access good curing characteristics.Should explain,, also can use curing catalysts such as tertiary amines, imidazoles, organo phosphorous compounds as required, wherein,, preferably use organo phosphorous compounds in order further to improve flame retardant resistance for these solidifying agent.
With respect to the total mass of epoxy resin powder coating, the total amount of epoxy resin and solidifying agent is preferably 10～80 quality %, further is preferably 25～60 quality %.Thus, can make the coating of powder coating become good.If use level is less than above-mentioned lower value; The smoothness of then filming sometimes reduces; On the other hand, if more than above-mentioned higher limit, then as the burning till of the curing process after the application time, cause the bad order of so-called sunburner (タ レ) or tip (ト ガ リ) and so on sometimes.
As the packing material that uses among the present invention, can enumerate lime carbonate, calcium sulfate, permanent white, white lake, Marinco H, aluminum oxide, crystallization or fused silica, surface treatment silicon-dioxide, talcum, kaolin, clay, mica, rhombspar, wollastonite, spun glass, granulated glass sphere, zircon, titanium compound, molybdenum compound etc.These can use separately, also can multiple combination use.Preferred molten silicon-dioxide wherein.
With respect to the total mass of epoxy resin powder coating, the use level of packing material is preferably 50 quality %～80 quality %, further is preferably 50 quality %～70 quality %.Thus, can make the coating of powder coating become good.If use level is less than above-mentioned lower value, then when burning till, cause the apparent bad phenomenon of so-called sunburner or tip and so on sometimes, make the physical strength of filming also not enough.On the other hand, if more than above-mentioned higher limit, the smoothness of then filming sometimes reduces.
In addition, do not limit, usually, preferably use 5～30 μ m as median size as the particle diameter of packing material is special.Thus, can give good flowability, improve coating more powder coating, so for the physical strength of filming also for optimum.
As the laser chromogenic reagent that uses among the present invention, use metal salt compound.As metal salt compound, can enumerate nickel compounds such as lactic acid nickel, nickelous hypophosphite, nickel formate, copper compounds such as verditer, cupric oxalate, zirconium compoundss such as zirconium silicate, lead compound etc.These can a plurality of alone or in combination uses.Wherein, preferably use the metal salt compound except that lead compound, more preferably use copper compound or zirconium compounds.Thus, can give sufficient color emissivity, and can realize alleviating carrying capacity of environment with more a spot of interpolation.
The use level of laser chromogenic reagent is preferably 0.5～20 quality % with respect to the total mass of powder coating, more preferably 0.5～10 quality %.If use level is less than above-mentioned lower value, then color emissivity is not enough sometimes, on the other hand, if more than above-mentioned higher limit, then causes the reduction significantly of wet fastness.
In order to give sufficient flame retardant resistance, the preferred phosphorus content of the SULPHOSUCCINIC ACID ESTER flame retardant that uses among the present invention is high and at room temperature be solid-state SULPHOSUCCINIC ACID ESTER flame retardant, for example can enumerate triphenyl or aromatic condensation type SULPHOSUCCINIC ACID ESTER etc.
With respect to the quality of the epoxy resin that uses, the containing ratio that the SULPHOSUCCINIC ACID ESTER flame retardant preferably fits in phosphorus composition is 1～3 quality %, more preferably fits in 2～2.5 quality %.If the phosphorus containing ratio less than above-mentioned lower value, then can't obtain sufficient flame retardant resistance sometimes,, also find to improve effect that flame retardant resistance gives sometimes more than it even if greater than above-mentioned higher limit.In addition, through cooperating the SULPHOSUCCINIC ACID ESTER flame retardant, can improve the physical strengths such as heat-resisting cyclicity of the powder coating that obtains with the mode that becomes the phosphorus composition in the above-mentioned scope.
The above thermal expansivity of Tg that contains the fire-retarded epoxy resin powder coating of the present invention of mentioned component is 10 * 10
-5/ ℃ below.Fire-retarded epoxy resin powder coating of the present invention is because the above thermal expansivity of Tg is 10 * 10
-5/ ℃ below, can improve physical strengths such as heat-resisting cyclicity.This reason is still indeterminate, but thinks the reason that diminishes owing to the difference with the thermal expansivity of electronic unit.
In addition, the lower value of the thermal expansivity that the Tg of fire-retarded epoxy resin powder coating of the present invention is above is not special to be limited, and is generally 8.5 * 10
-5/ ℃ more than, be preferably 5 * 10
-5/ ℃ more than.
Here, the above thermal expansivity of above-mentioned Tg is a value of utilizing thermo-mechanical analysis (TMA) method to measure according to JIS C 2161, the MV of the thermal expansivity in the zone of expression Tg～160 ℃.
In addition, the above-mentioned Tg of epoxy resin powder coating of the present invention be preferably below 100 ℃, more preferably below 95 ℃.Through Tg is below the above-mentioned higher limit, thereby the stress that improves epoxy resin powder coating relaxes ability, and its result can improve the heat-resisting cyclicity of epoxy resin powder coating.In addition, the lower value of the Tg of epoxy resin powder coating of the present invention is not special to be limited, and is generally more than 60 ℃.
In addition, the bending elastic modulus of measuring according to JIS K 6911 of epoxy resin powder coating of the present invention is preferably 1.0 * 10
4More than the MPa.Through bending elastic modulus is more than the above-mentioned lower value, thereby can further improve physical strengths such as heat-resisting cyclicity.In addition, the higher limit of the bending elastic modulus of epoxy resin powder coating of the present invention is not special to be limited, and is generally 1.3 * 10
4Below the MPa.
Powder coating of the present invention except that the composition that cooperates above explanation, can cooperate additives such as pigment, flow agent, coupling agent, skimmer as required.In addition, also can use silicone resin, melamine resin etc. to have the resin of cyanurate ring skeleton, perhaps the flame retardant resistance auxiliary agent of non-halogen such as zinc borate, expansile graphite in order to improve flame retardant resistance.
Fire-retarded epoxy resin powder coating of the present invention can obtain through suitable selection above-mentioned each composition and the suitable use level of adjusting each composition.
Make not special qualification of method of powder coating among the present invention, can use general method.As an example, can utilize the mixing tank thorough mixing evenly the material composition that fits in the regulation ratio of components after, carry out melting mixing with extrusion machine, twin shaft mixing roll etc., then utilize kibbler to be ground into suitable granularity and classification and obtain.
Though can performing well in the packing of electric component such as ceramic condenser for example, electronic unit, not special qualification the, epoxy resin powder coating of the present invention film.
Embodiment
Below, through embodiment the present invention is described particularly, but the present invention is not limited to following embodiment.
The material composition of the use level shown in the table 1 (mass parts) is utilized mixer mixing, behind the melting mixing, utilize kibbler to pulverize, making mean particle size is the epoxy resin powder coating of 40～60 μ m.The powder coating that obtains is estimated for following project.The result is shown in following table.
1. epoxy resin
Bisphenol A type epoxy resin: Mitsubishi Chemical Ind's system, " EPIKOTE 1003 " (epoxy equivalent (weight) 720)
Brominated epoxy resin: chemical company of Nippon Steel system, " EPO TOHTO YDB-400 " (epoxy equivalent (weight) 400)
2. solidifying agent
BTDA: UVNUL MS-40 tetracarboxylic anhydride
TMA: trimellitic acid 1,2-anhydride
3. curing catalyst
TPP: triphenylphosphine
4. packing material
Fused silica: imperial gloomy corporate system, " RD-8 " (median size 15 μ m)
5. pigment
White pigments (titanium oxide): the former industry corporate system of stone, " TTO-55 "
Blue pigment (cyanines are blue): sumitomo chemical company system, " CYANINE BLUE-GH "
6. additive
Silane coupling agent: GE Toshiba Silicones system, " A-187 "
Flow agent: Surface Specialties corporate system, MODAFLOW POWDER
7. fire retardant
SULPHOSUCCINIC ACID ESTER: big eight chemical company's systems, " PX-200 " (phosphorus containing ratio 8.9 quality %)
ANTIMONY TRIOXIDE SB 203 99.8 PCT
8. laser chromogenic reagent
Nickelous hypophosphite
Copper compound
Zirconium compounds
9. ion capturing agent
Hydrotalcite: consonance chemical industrial company system, " DHT-4A "
(TP)
1. gelation time:, measure with 165 ℃ heat dishes according to JIS C 2161.
2. flame retardant test: test board thickness is made as 0.8mm, measures according to the UL94 method.
3. second-order transition temperature (Tg):, measure with the TMA method according to JIS C 2161.
4. thermal expansivity (below the Tg ,/℃): according to JIS C 2161, measure, and calculate the MV of the thermal expansivity in the zone of 30 ℃～Tg with the TMA method.
5. thermal expansivity (more than the Tg ,/℃): according to JIS C 2161, measure, and calculate the MV of the thermal expansivity in the zone of Tg～160 ℃ with the TMA method.
6. flexural strength (MPa):, measure with flexural strength according to JIS K 6911.
7. heat-resisting cyclicity
is used to carry out the electronic unit of powder body coating more than the thickness 0.75mm, confirms fissured having or not.
8. heat-resisting cyclicity
is used to carry out the electronic unit of powder body coating more than the thickness 0.75mm, confirms fissured having or not.
9. bending elastic modulus (MPa): measure bending elastic modulus according to JIS K 6911.
Table 1
The above thermal expansivity of the Tg of the epoxy resin powder coating of embodiment is 10 * 10
-5/ ℃ below.Such epoxy resin powder coating exists
Thermal cycling test in, possess the heat-resisting cyclicity more than 2500;
Thermal cycling test in possess the heat-resisting cyclicity more than 1500, and possess the above flexural strength and 1.0 * 10 of 110MPa
4The bending elastic modulus that MPa is above.
On the other hand; The powder coating that contains the comparative example of brominated epoxy resin; In the thermal cycling test of
, heat-resisting cyclicity is below 500; In the thermal cycling test of
, heat-resisting cyclicity is below 500.In addition, the flexural strength of the split coating of comparative example is for less than 1.0 * 10 less than 110MPa and bending elastic modulus
4MPa.
Claims (8)
1. a fire-retarded epoxy resin powder coating is characterized in that,
Be the epoxy resin powder coating that contains epoxy resin, solidifying agent, packing material, laser chromogenic reagent and SULPHOSUCCINIC ACID ESTER flame retardant,
The above thermal expansivity of the second-order transition temperature of said epoxy resin powder coating is 10 * 10
-5/ ℃ below.
2. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, with respect to the quality of said epoxy resin powder coating, said packing material is more than the 50 quality %.
3. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, said laser chromogenic reagent contains copper compound or zirconium compounds.
4. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, said packing material is a fused silica.
5. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, said solidifying agent contains acid anhydrides.
6. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, the bending elastic modulus of said epoxy resin powder coating is 1.0 * 10
4More than the MPa.
7. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, the second-order transition temperature of said epoxy resin powder coating is below 100 ℃.
8. fire-retarded epoxy resin powder coating as claimed in claim 1, wherein, the packing that said epoxy resin powder coating is used for electric component, electronic unit is filmed.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2011111065 | 2011-05-18 | ||
| JP2011-111065 | 2011-05-18 |
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| CN102786858A true CN102786858A (en) | 2012-11-21 |
| CN102786858B CN102786858B (en) | 2017-09-01 |
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| CN (1) | CN102786858B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103965737A (en) * | 2014-05-09 | 2014-08-06 | 福建万安实业有限公司 | Flame retardant powder coating |
| CN107629378A (en) * | 2017-11-05 | 2018-01-26 | 包红珠 | A kind of oil plant of gas square diffuser |
| CN109642110A (en) * | 2016-08-26 | 2019-04-16 | 大金工业株式会社 | Powder coating, laminate and pipe |
| CN114230202A (en) * | 2022-01-20 | 2022-03-25 | 漳州市瑞隆达工贸有限公司 | Preparation process of hollow glass |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP6349836B2 (en) * | 2014-03-25 | 2018-07-04 | 住友ベークライト株式会社 | Epoxy resin powder coating for varistor and varistor |
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Patent Citations (4)
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| JP2004292765A (en) * | 2003-03-28 | 2004-10-21 | Sumitomo Bakelite Co Ltd | Flame resistant epoxy resin powder coating material for laser printing |
| CN1730548A (en) * | 2004-08-06 | 2006-02-08 | 株式会社日本触媒 | Resin composition, method of its composition, and cured formulation |
| CN101343412A (en) * | 2007-07-12 | 2009-01-14 | 三菱瓦斯化学株式会社 | Prepreg and laminate |
| CN101148457A (en) * | 2007-11-02 | 2008-03-26 | 湖南大学 | Phosphorus-containing tri-functional group liquid alicyclic epoxy compound and preparation method thereof |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103965737A (en) * | 2014-05-09 | 2014-08-06 | 福建万安实业有限公司 | Flame retardant powder coating |
| CN109642110A (en) * | 2016-08-26 | 2019-04-16 | 大金工业株式会社 | Powder coating, laminate and pipe |
| CN109642110B (en) * | 2016-08-26 | 2021-11-02 | 大金工业株式会社 | Powder coating material, laminate, and pipe |
| CN107629378A (en) * | 2017-11-05 | 2018-01-26 | 包红珠 | A kind of oil plant of gas square diffuser |
| CN114230202A (en) * | 2022-01-20 | 2022-03-25 | 漳州市瑞隆达工贸有限公司 | Preparation process of hollow glass |
Also Published As
| Publication number | Publication date |
|---|---|
| JP2012255139A (en) | 2012-12-27 |
| CN102786858B (en) | 2017-09-01 |
| JP5949116B2 (en) | 2016-07-06 |
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