JP2002265864A - Powder coating composition and method for producing the same - Google Patents
Powder coating composition and method for producing the sameInfo
- Publication number
- JP2002265864A JP2002265864A JP2001066457A JP2001066457A JP2002265864A JP 2002265864 A JP2002265864 A JP 2002265864A JP 2001066457 A JP2001066457 A JP 2001066457A JP 2001066457 A JP2001066457 A JP 2001066457A JP 2002265864 A JP2002265864 A JP 2002265864A
- Authority
- JP
- Japan
- Prior art keywords
- particles
- powder coating
- coating composition
- curing agent
- curing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Landscapes
- Paints Or Removers (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、低温硬化性の粉体
塗料であっても貯蔵安定性に優れるとともに、密着性、
耐衝撃性、低粘着性等の物性が良好な塗膜が得られる粉
体塗料組成物、及び、上記粉体塗料組成物の製造方法に
関する。The present invention relates to a powder coating material which is curable at a low temperature and has excellent storage stability and adhesion.
The present invention relates to a powder coating composition from which a coating film having good physical properties such as impact resistance and low tackiness can be obtained, and a method for producing the powder coating composition.
【０００２】[0002]
【従来の技術】粉体塗料は、一般的に、塗膜形成性樹脂
及び硬化剤、並びに、所望により硬化触媒、添加剤等を
混合機により均一に混合し、得られた混合物を混練機に
より溶融混練した後、ペレットに成形して、粉砕するこ
とにより得られる。2. Description of the Related Art In general, powder coatings are prepared by uniformly mixing a film-forming resin, a curing agent, and, if desired, a curing catalyst and additives with a mixer, and mixing the resulting mixture with a kneader. After melt-kneading, it is obtained by molding into pellets and pulverizing.
【０００３】近年では、省エネルギーの観点から低温硬
化性の粉体塗料が求められている。エポキシ樹脂、硬化
剤、硬化触媒の配合技術により低温硬化は可能である
が、従来の製造方法によって製造すると、通常１００〜
１２０℃で行われる溶融混練工程の際に硬化剤と塗膜形
成用樹脂との反応が進むため、低温化には限界があっ
た。更に、たとえ製造できたとしても、低温硬化性の粉
体塗料は貯蔵安定性に劣るものであった。また、塗装
後、焼付ける際の焼付け温度が低いため、溶融粘度をあ
まり低くすることができず、素材との濡れが不充分で塗
膜密着性に劣るという問題点もあった。In recent years, low-temperature curable powder coatings have been demanded from the viewpoint of energy saving. Low-temperature curing is possible by the compounding technique of epoxy resin, curing agent and curing catalyst, but when produced by a conventional production method, usually 100 to 100
Since the reaction between the curing agent and the resin for forming a coating film proceeds during the melt-kneading step performed at 120 ° C., there is a limit to the temperature reduction. Furthermore, even if it can be manufactured, the low temperature curable powder coating has poor storage stability. In addition, since the baking temperature at the time of baking after coating is low, the melt viscosity cannot be reduced too much, and there is a problem that the wettability with the material is insufficient and the coating film adhesion is poor.
【０００４】特表２０００−５０４３６９号公報には、
２００μｍより小さいエポキシ樹脂粉末、Ｎ−ヘテロ環
式アミン又は脂肪族、環式脂肪族、芳香族脂肪族若しく
はＮ−ヘテロ環式アミンをベースとする２００μｍより
小さいアミン硬化剤粉末、及び、添加剤を機械的に混合
して得られるエポキシ系粉体塗料を、感熱性基材に塗布
し、熱及び圧力の適用で硬化させる塗膜形成方法が開示
されている。[0004] JP-T-2000-504369 discloses that
Epoxy resin powder smaller than 200 μm, amine hardener powder smaller than 200 μm based on N-heterocyclic amine or aliphatic, cycloaliphatic, araliphatic or N-heterocyclic amine, and additives A coating film forming method is disclosed in which an epoxy-based powder coating obtained by mechanical mixing is applied to a heat-sensitive substrate and cured by applying heat and pressure.
【０００５】しかしながら、この方法では、エポキシ樹
脂とアミン硬化剤とを予め別々に粉末状に調製した後こ
れらをドライブレンドするために、粉体粒子自体として
は完全に混合されておらず、硬化が不充分であり、得ら
れる塗膜の性能に劣るものであった。However, in this method, since the epoxy resin and the amine curing agent are separately prepared in powder form and then dry-blended, the powder particles themselves are not completely mixed, and the curing is not carried out. It was insufficient, and the performance of the resulting coating film was poor.
【０００６】[0006]
【発明が解決しようとする課題】本発明の目的は、上記
に鑑み、低温硬化性の粉体塗料であっても貯蔵安定性に
優れるとともに、塗膜焼付け後の密着性、耐衝撃性、低
粘着性等の物性が良好な塗膜が得られる粉体塗料組成
物、及び、上記粉体塗料組成物の製造方法を提供するこ
とにある。SUMMARY OF THE INVENTION In view of the above, it is an object of the present invention to provide a low-temperature curable powder coating composition which has excellent storage stability, adhesion after baking of a coating film, low impact resistance, and low viscosity. An object of the present invention is to provide a powder coating composition from which a coating film having good physical properties such as adhesiveness can be obtained, and a method for producing the powder coating composition.
【０００７】[0007]
【課題を解決するための手段】本発明は、エポキシ樹
脂、硬化剤及び硬化触媒からなる第１粒子と、硬化剤及
び硬化触媒からなる第２粒子とからなる粉体塗料組成物
であって、上記第１粒子及び上記第２粒子の平均体積粒
子径が５μｍ以上２５μｍ未満であり、上記粉体塗料組
成物中の硬化剤の合計量の０〜８０重量％が上記第１粒
子に含有され、上記粉体塗料組成物中の硬化触媒の合計
量の０〜７０重量％が上記第１粒子に含有されているこ
とを特徴とする粉体塗料組成物である。The present invention provides a powder coating composition comprising a first particle comprising an epoxy resin, a curing agent and a curing catalyst, and a second particle comprising a curing agent and a curing catalyst, The first particles and the second particles have an average volume particle diameter of 5 μm or more and less than 25 μm, and the first particles contain 0 to 80% by weight of the total amount of the curing agent in the powder coating composition; A powder coating composition, wherein the first particles comprise 0 to 70% by weight of the total amount of the curing catalyst in the powder coating composition.
【０００８】本発明は、また、エポキシ樹脂、硬化剤及
び硬化触媒からなる第１粒子と、硬化剤及び硬化触媒か
らなる第２粒子とからなる粉体塗料組成物であって、上
記第１粒子及び上記第２粒子の平均体積粒子径が２５〜
５０μｍであり、上記粉体塗料組成物中の硬化剤の合計
量の３０〜８０重量％が上記第１粒子に含有され、上記
粉体塗料組成物中の硬化触媒の合計量の０〜７０重量％
が上記第１粒子に含有されていることを特徴とする粉体
塗料組成物である。The present invention also provides a powder coating composition comprising first particles comprising an epoxy resin, a curing agent and a curing catalyst, and second particles comprising a curing agent and a curing catalyst, wherein the first particles comprise And the average volume particle diameter of the second particles is 25 to
50 μm, 30 to 80% by weight of the total amount of the curing agent in the powder coating composition is contained in the first particles, and 0 to 70% by weight of the total amount of the curing catalyst in the powder coating composition %
Is contained in the first particles.
【０００９】上記硬化剤は、アミン化合物、フェノール
化合物及び酸化合物からなる群より選択される少なくと
も１つであることが好ましく、上記エポキシ樹脂のエポ
キシ当量に対する粉体塗料組成物中の全硬化剤の活性水
素当量の比は、０．７〜１．３であることが好ましい。
上記エポキシ樹脂は、エポキシ当量が６００〜２２００
であって、通常、粉体塗料に使用されているビスフェノ
ールＡ型エポキシ樹脂又はビスフェノールＦ型エポキシ
樹脂であることが好ましい。Preferably, the curing agent is at least one selected from the group consisting of an amine compound, a phenol compound and an acid compound, and the total curing agent in the powder coating composition relative to the epoxy equivalent of the epoxy resin is used. The ratio of the active hydrogen equivalent is preferably 0.7 to 1.3.
The epoxy resin has an epoxy equivalent of 600 to 2200.
It is preferable to use a bisphenol A type epoxy resin or a bisphenol F type epoxy resin usually used for powder coatings.
【００１０】本発明は、更に、上記粉体塗料組成物の製
造方法であって、エポキシ樹脂、硬化剤及び硬化触媒か
らなる成分を混練し粉砕することにより第１粒子を得る
工程；硬化剤及び硬化触媒からなる成分を混練し粉砕す
ることにより第２粒子を得る工程；上記第１粒子及び上
記第２粒子を均一に混合する工程；からなることを特徴
とする粉体塗料組成物の製造方法である。以下、本発明
についてさらに詳細に説明する。[0010] The present invention further relates to a method for producing the powder coating composition, wherein a component comprising an epoxy resin, a curing agent and a curing catalyst is kneaded and pulverized to obtain first particles; Kneading and pulverizing a component comprising a curing catalyst to obtain second particles; and uniformly mixing the first particles and the second particles; and a method for producing a powder coating composition. It is. Hereinafter, the present invention will be described in more detail.
【００１１】本発明の粉体塗料組成物は、第１粒子と第
２粒子とからなるものである。本発明の粉体塗料組成物
は、エポキシ樹脂と特定の割合の硬化剤及び硬化触媒と
を混練し粉砕することにより第１粒子を調製し、これと
は別に残りの割合の硬化剤及び硬化触媒を混練し粉砕す
ることにより第２粒子を調製した後、これらの第１粒子
と第２粒子とを均一に混合することにより得られるもの
である。[0011] The powder coating composition of the present invention comprises first particles and second particles. The powder coating composition of the present invention is prepared by kneading and pulverizing an epoxy resin and a specific ratio of a curing agent and a curing catalyst to prepare first particles, and separately from the first particles, the remaining ratio of the curing agent and the curing catalyst Is prepared by kneading and pulverizing to prepare second particles, and then uniformly mixing the first particles and the second particles.
【００１２】上記第１粒子は、エポキシ樹脂、硬化剤及
び硬化触媒からなるものである。上記第１粒子は、平均
体積粒子径が５〜５０μｍである。５μｍ未満である
と、スピットが発生し易く、かつ、搬送性に問題が生
じ、５０μｍを超えると、各原料成分の混合が不充分と
なり、得られる塗膜の物性や外観に劣る。好ましくは、
１０〜３５μｍであり、より好ましくは、１５〜２５μ
ｍである。上記平均体積粒子径は、日機装株式会社のマ
イクロトラックＨＲＡ Ｘ−１００のレーザー光散乱に
よる粒径測定装置による粒径測定装置により測定するこ
とができる。The first particles are composed of an epoxy resin, a curing agent and a curing catalyst. The first particles have an average volume particle diameter of 5 to 50 μm. If it is less than 5 μm, spits are liable to be generated, and there is a problem in transportability. If it exceeds 50 μm, mixing of each raw material component is insufficient, and the physical properties and appearance of the obtained coating film are poor. Preferably,
10 to 35 μm, more preferably 15 to 25 μm
m. The average volume particle diameter can be measured by a particle size measuring device of Nikkiso Co., Ltd. Microtrac HRA X-100 using a particle size measuring device by laser light scattering.
【００１３】上記第２粒子は、硬化剤及び硬化触媒から
なるものである。上記第２粒子は、上述の第１粒子と同
様に平均体積粒子径が５〜５０μｍである。５μｍ未満
であると、スピットが発生し易く、かつ、搬送性に問題
が生じ、５０μｍを超えると、混合が不充分となり、得
られる塗膜の物性や外観に劣る。好ましくは、１０〜３
５μｍであり、より好ましくは、１５〜２５μｍであ
る。上記第２粒子の平均体積粒子径は、上記範囲内であ
れば上記第１粒子と同じである必要はないが、通常、上
記第１粒子の平均体積粒子径と同程度か又はそれよりも
小さい方が塗膜の性能上有利である。The second particles comprise a curing agent and a curing catalyst. The second particles have an average volume particle diameter of 5 to 50 μm, like the first particles. If it is less than 5 μm, spits are likely to occur, and a problem arises in transportability. If it exceeds 50 μm, mixing becomes insufficient, and the physical properties and appearance of the resulting coating film are poor. Preferably, 10-3
It is 5 μm, more preferably 15 to 25 μm. The average volume particle diameter of the second particles does not need to be the same as that of the first particles as long as the average particle diameter is within the above range, but is usually equal to or smaller than the average volume particle diameter of the first particles. It is more advantageous for the performance of the coating film.
【００１４】本発明の粉体塗料組成物に含まれるエポキ
シ樹脂としては特に限定されず、粉体塗料に通常使用さ
れるものを使用することができ、例えば、ビスフェノー
ルＡ型エポキシ樹脂、ビスフェノールＦ型エポキシ樹
脂、ノボラック型エポキシ樹脂、脂環式エポキシ樹脂、
線状脂肪族エポキシ樹脂等を挙げることができる。これ
らのうち、ビスフェノールＡ型エポキシ樹脂、ビスフェ
ノールＦ型エポキシ樹脂が好ましい。The epoxy resin contained in the powder coating composition of the present invention is not particularly limited, and those usually used in powder coatings can be used. For example, bisphenol A type epoxy resin, bisphenol F type Epoxy resin, novolak type epoxy resin, alicyclic epoxy resin,
Linear aliphatic epoxy resins and the like can be mentioned. Of these, bisphenol A epoxy resin and bisphenol F epoxy resin are preferred.
【００１５】上記粉体塗料組成物中のエポキシ樹脂は、
エポキシ当量が６００〜２２００であることが好まし
い。６００未満であると、塗料の貯蔵中にブロッキング
を生じる場合があり、２２００を超えると、エポキシ樹
脂の融点が高くなり、低温硬化粉体塗料には適さない。
より好ましくは、６７０〜１０００であり、更に好まし
くは、６７０〜８４０である。The epoxy resin in the above powder coating composition comprises:
It is preferable that the epoxy equivalent is 600 to 2200. If it is less than 600, blocking may occur during storage of the coating material, and if it exceeds 2200, the melting point of the epoxy resin becomes high, and it is not suitable for a low-temperature curing powder coating material.
More preferably, it is 670-1000, and still more preferably, it is 670-840.
【００１６】上記粉体塗料組成物中のエポキシ樹脂は、
軟化点が１３０℃以下であることが好ましい。１３０℃
を超えると、低温での焼付け時の粘度が充分に低下せ
ず、塗膜の物性及び塗膜の外観が低下する場合がある。
より好ましくは、９０〜１０５℃である。The epoxy resin in the above powder coating composition comprises:
It is preferable that the softening point is 130 ° C. or less. 130 ° C
If it exceeds 300, the viscosity at the time of baking at a low temperature does not sufficiently decrease, and the physical properties of the coating film and the appearance of the coating film may decrease.
More preferably, it is 90 to 105 ° C.
【００１７】本発明の粉体塗料組成物に含まれる硬化剤
としては、エポキシ樹脂に通常使用されるものであれば
特に限定されず、例えば、アミン化合物、フェノール化
合物、無水フタル酸を含む酸化合物等を挙げることがで
き、これらは１種又は２種以上を使用することができ
る。これらのうち、アミン化合物、フェノール化合物、
酸化合物が好ましい。The curing agent contained in the powder coating composition of the present invention is not particularly limited as long as it is one usually used for an epoxy resin. For example, an acid compound containing an amine compound, a phenol compound and phthalic anhydride And these can be used alone or in combination of two or more. Among these, amine compounds, phenol compounds,
Acid compounds are preferred.
【００１８】上記粉体塗料組成物中の硬化剤は、上記エ
ポキシ樹脂のエポキシ当量に対する粉体塗料組成物中の
全硬化剤の活性水素当量の比が０．７〜１．３となるよ
うに含有されることが好ましい。０．７未満であると、
未反応のエポキシ樹脂が塗膜中に存在し、物性等の性能
が劣り、低温硬化性の粉体塗料組成物として不都合が生
じる場合があり、１．３を超えると、未反応の硬化剤が
塗膜に存在し、耐水性等の塗膜物性が低下する。The curing agent in the powder coating composition is adjusted so that the ratio of the active hydrogen equivalent of all the curing agents in the powder coating composition to the epoxy equivalent of the epoxy resin is 0.7 to 1.3. It is preferable to be contained. If it is less than 0.7,
Unreacted epoxy resin is present in the coating film, and its properties such as physical properties are inferior. Inconvenience may occur as a low-temperature curable powder coating composition. It is present in the coating film, and the physical properties of the coating film such as water resistance are reduced.
【００１９】上記第１粒子及び上記第２粒子の後述する
平均体積粒子径が５μｍ以上２５μｍ未満である場合、
上記粉体塗料組成物中の硬化剤は、その合計量の０〜８
０重量％が上記第１粒子に含有される。８０重量％を超
えると、上記第１粒子の製造過程において硬化が進み、
上記粉体塗料組成物中において混合に均一性を欠くの
で、得られる塗膜の物性に劣る。好ましくは、２５〜７
５重量％であり、より好ましくは、５０〜７５重量％で
ある。When the below-mentioned average volume particle diameter of the first particles and the second particles is 5 μm or more and less than 25 μm,
The curing agent in the powder coating composition is used in an amount of 0 to 8 based on the total amount thereof.
0% by weight is contained in the first particles. If it exceeds 80% by weight, curing proceeds in the process of producing the first particles,
Since the powder coating composition lacks uniformity in mixing, the resulting coating film has poor physical properties. Preferably, 25 to 7
The content is 5% by weight, more preferably 50 to 75% by weight.
【００２０】上記第１粒子及び上記第２粒子の平均体積
粒子径が２５〜５０μｍである場合、上記粉体塗料組成
物中の硬化剤は、その合計量の３０〜８０重量％が上記
第１粒子に含有される。３０重量％未満であると、上記
粉体塗料組成物中において各原料成分が均一に混ざりに
くいので、得られる塗膜の物性が劣り、８０重量％を超
えると、上記第１粒子の製造過程において硬化が進み、
上記粉体塗料組成物中において混合に均一性を欠くの
で、得られる塗膜の物性が劣る。好ましくは４０〜７５
重量％であり、より好ましくは５０〜７５重量％であ
る。上記粉体塗料組成物中の硬化剤のうち、上記第１粒
子中の含有量を除く量は、第２粒子に含有される。When the first particles and the second particles have an average volume particle diameter of 25 to 50 μm, the curing agent in the powder coating composition accounts for 30 to 80% by weight of the total amount of the first particles. Contained in particles. When the amount is less than 30% by weight, the respective raw material components are difficult to mix uniformly in the powder coating composition, so that the physical properties of the obtained coating film are inferior. When the amount exceeds 80% by weight, in the production process of the first particles, Curing progresses,
Since the mixing is not uniform in the powder coating composition, the physical properties of the obtained coating film are poor. Preferably 40 to 75
%, More preferably 50 to 75% by weight. The amount of the curing agent in the powder coating composition excluding the content in the first particles is contained in the second particles.
【００２１】本発明の粉体塗料組成物に含まれる硬化触
媒としては、エポキシ樹脂に通常使用されるものを使用
することができ、例えば、ジブチルすずジラウレートを
含む脂肪酸すず塩等のルイス酸；パラトルエンスルホン
酸、りん酸等のプロトン酸；トリエチルアミン、Ｎ−メ
チルモルフォリン、Ｎ，Ｎ′−ジメチルピペラジン等の
３級アミン；２−メチルイミダゾール等のイミダゾール
系硬化触媒；２−メチルイミダゾリン等のイミダゾリン
系硬化触媒等を挙げることができる。これらのうち、イ
ミダゾール系硬化触媒、イミダゾリン系硬化触媒が好ま
しい。これらは１種又は２種以上を使用することができ
る。As the curing catalyst contained in the powder coating composition of the present invention, those usually used for epoxy resins can be used. For example, Lewis acids such as fatty acid tin salts containing dibutyltin dilaurate; Protonic acids such as toluenesulfonic acid and phosphoric acid; tertiary amines such as triethylamine, N-methylmorpholine and N, N'-dimethylpiperazine; imidazole curing catalysts such as 2-methylimidazole; imidazolines such as 2-methylimidazoline System curing catalyst and the like. Among these, an imidazole-based curing catalyst and an imidazoline-based curing catalyst are preferred. One or more of these can be used.
【００２２】上記粉体塗料組成物中の硬化触媒量は、上
述のエポキシ樹脂のエポキシ基１当量あたり０．０６〜
０．１５モルであることが好ましい。０．０６モル未満
であると、硬化が不充分となって低温での硬化が困難と
なりやすいほか、得られる塗膜の物性が低下する場合が
あり、０．１５モルを超えると、本発明における第１粒
子の混練過程等の早期に硬化反応が開始され、得られる
塗膜の耐衝撃性等の物性が低下する場合がある。より好
ましくは、０．０８〜０．１３モルであり、更に好まし
くは、０．１０〜０．１２モルである。The amount of the curing catalyst in the above powder coating composition is 0.06 to 1 per equivalent of epoxy group of the above epoxy resin.
Preferably it is 0.15 mol. When the amount is less than 0.06 mol, the curing becomes insufficient and the curing at a low temperature tends to be difficult, and in addition, the physical properties of the obtained coating film may be deteriorated. A curing reaction may be started early in the kneading process of the first particles and the like, and the physical properties such as impact resistance of the obtained coating film may be reduced. More preferably, it is 0.08 to 0.13 mol, and still more preferably, 0.10 to 0.12 mol.
【００２３】上記粉体塗料組成物中の硬化触媒は、その
合計量の０〜７０重量％が第１粒子に含有される。７０
重量％を超えると、第１粒子の混練工程において反応が
開始され、ゲル化する場合もあるので、上記粉体塗料組
成物中において完全に混合されず、得られる塗膜の物性
が低下する。好ましくは、３０〜７０重量％であり、よ
り好ましくは、５０〜６５重量％である。上記粉体塗料
組成物中の硬化触媒のうち、上記第１粒子中の含有量を
除く量は、第２粒子に含有される。The curing catalyst in the powder coating composition contains 0 to 70% by weight of the total amount in the first particles. 70
If the content is more than 10% by weight, the reaction is started in the kneading step of the first particles and gelation may occur, so that they are not completely mixed in the powder coating composition, and the physical properties of the obtained coating film are deteriorated. Preferably, it is 30 to 70% by weight, more preferably 50 to 65% by weight. The amount of the curing catalyst in the powder coating composition excluding the content in the first particles is contained in the second particles.
【００２４】本発明の粉体塗料組成物は、必要により、
例えば、アクリル樹脂及びポリエステル樹脂等の他の樹
脂、顔料、その他の添加剤を併用することができる。上
記他の樹脂としては、ポリエステル樹脂が好ましく、ポ
リエステル樹脂を用いる場合は、上記ポリエステル樹脂
は上記第２粒子に含有させることが好ましい。この場
合、得られる粉体塗料は、当該技術分野ではエポキシポ
リエステル系粉体塗料といわれるものであり、低温硬化
性を一層向上させることができる。The powder coating composition of the present invention may optionally contain
For example, other resins such as acrylic resins and polyester resins, pigments, and other additives can be used in combination. As the other resin, a polyester resin is preferable. When a polyester resin is used, the polyester resin is preferably contained in the second particles. In this case, the obtained powder coating is referred to as an epoxy polyester powder coating in the technical field, and can further improve the low-temperature curability.
【００２５】上記粉体塗料組成物中の顔料としては特に
限定されず、例えば、沈降性硫酸バリウム、炭酸カルシ
ウム、クレー、タルク、シリカ、マイカ等の体質顔料；
二酸化チタン、べんがら、黄色酸化鉄、カーボンブラッ
ク、フタロシアニンブルー、フタロシアニングリーン、
キナクリドン系赤色顔料等の着色顔料を使用することが
できる。顔料を全く含まないで、透明な塗膜を形成しう
るクリアー塗料とすることもできる。上記粉体塗料組成
物中の顔料の含有量は、本発明の粉体塗料組成物１００
重量部に対して、１〜８０重量部が好ましい。含有量が
１重量部未満であると、着色等の顔料の効果が得られ
ず、８０重量部を超えると、外観に優れる塗膜が得られ
ない。The pigment in the powder coating composition is not particularly limited, and includes, for example, extender pigments such as precipitated barium sulfate, calcium carbonate, clay, talc, silica and mica;
Titanium dioxide, red iron oxide, yellow iron oxide, carbon black, phthalocyanine blue, phthalocyanine green,
Color pigments such as quinacridone red pigments can be used. A clear paint that can form a transparent coating film without containing any pigment can also be used. The content of the pigment in the powder coating composition is 100 powder coating composition of the present invention.
The amount is preferably 1 to 80 parts by weight with respect to parts by weight. If the content is less than 1 part by weight, the effect of the pigment such as coloring cannot be obtained, and if it exceeds 80 parts by weight, a coating film having excellent appearance cannot be obtained.
【００２６】上記粉体塗料組成物中のその他の添加剤と
しては、表面調整剤、可塑剤、紫外線吸収剤、酸化防止
剤、ワキ防止剤、顔料分散剤等を挙げることができ、こ
れらはエポキシ樹脂からなる粉体塗料に通常使用される
ものを使用することができる。上記粉体塗料組成物中の
顔料及びその他の添加剤は、第１粒子や第２粒子とは別
の粒子として添加することもできるが、第１粒子や第２
粒子の中に含まれていることが好ましい。Other additives in the powder coating composition include a surface conditioner, a plasticizer, an ultraviolet absorber, an antioxidant, an anti-peeling agent, a pigment dispersant, and the like. Those commonly used for resin powder coatings can be used. The pigment and other additives in the powder coating composition may be added as particles different from the first particles and the second particles, but the first particles and the second particles may be added.
Preferably, it is contained in the particles.
【００２７】上記粉体塗料組成物は、（１）エポキシ樹
脂、硬化剤及び硬化触媒からなる成分を混練し粉砕する
ことにより第１粒子を得る工程、（２）硬化剤及び硬化
触媒からなる成分を混練し粉砕することにより第２粒子
を得る工程、並びに、（３）上記第１粒子及び上記第２
粒子を均一に混合する工程からなる製造方法により製造
することができる。The above powder coating composition comprises: (1) a step of obtaining first particles by kneading and pulverizing a component comprising an epoxy resin, a curing agent and a curing catalyst, and (2) a component comprising a curing agent and a curing catalyst. Kneading and pulverizing to obtain second particles, and (3) the first particles and the second particles.
It can be produced by a production method comprising a step of uniformly mixing particles.
【００２８】上記（１）の工程及び上記（２）の工程と
しては、混練し粉砕することができる方法であれば特に
限定されず、例えば、上述の硬化剤、硬化触媒、エポキ
シ樹脂、及び、必要に応じて使用される顔料、その他の
添加剤をヘンシェルミキサー、スーパーミキサー等の混
合機により均一に混合し、次に、得られた混合物を、エ
クストルーダーや熱ロール等の混練機により溶融混練
し、溶融したエポキシ樹脂中にエポキシ樹脂以外の成分
を均一に分散させ、得られた分散物を必要に応じてハン
マーミル等の衝撃型粉砕機、ジェットミル等の気流粉砕
機等によって粉砕した後、分級することにより上記第１
粒子及び上記第２粒子が得られる。上記（１）の工程及
び上記（２）の工程は、何れを先に行ってもよく、ま
た、並行して行ってもよい。The step (1) and the step (2) are not particularly limited as long as they can be kneaded and pulverized. For example, the above-mentioned curing agent, curing catalyst, epoxy resin, The pigments and other additives used as necessary are uniformly mixed by a mixer such as a Henschel mixer or a super mixer, and then the obtained mixture is melt-kneaded by a kneader such as an extruder or a hot roll. Then, components other than the epoxy resin are uniformly dispersed in the molten epoxy resin, and the obtained dispersion is pulverized by an impact-type pulverizer such as a hammer mill or an air-flow pulverizer such as a jet mill as necessary. , By the classification
The particles and the second particles are obtained. Either the step (1) or the step (2) may be performed first, or may be performed in parallel.
【００２９】上記第１粒子及び上記第２粒子の製造方法
としては、上述の方法以外に、例えば、原料を溶剤中で
混合し、得られた混合物を乾燥、微粉砕するか、又は、
スプレードライ法により粉末にする方法を採用すること
もできる。得られた粉末は必要に応じて、上述の粉砕、
分級に供することができる。As a method for producing the first particles and the second particles, in addition to the above-mentioned methods, for example, raw materials are mixed in a solvent, and the obtained mixture is dried and pulverized, or
A method of forming a powder by a spray drying method can also be adopted. The obtained powder is, if necessary, crushed as described above,
Can be subjected to classification.
【００３０】上記（３）の工程としては通常の回転や高
剪断作用による発熱がなく均一に粉体混合することがで
きる方法を使用することができ、例えば、Ｖブレンダ
ー、コニカルスクリューミキサー等の一般的なミキサー
を適宜用いることができる。In the step (3), a method capable of uniformly mixing powder without generating heat due to ordinary rotation or high shearing action can be used. For example, general methods such as a V blender and a conical screw mixer can be used. A suitable mixer can be used as appropriate.
【００３１】本発明の粉体塗料組成物の適用対象として
は特に限定されず、例えば、自動車用、家電機器用、建
材用、雑貨用等の鋼板、リン酸亜鉛処理鋼板、リン酸鉄
処理鋼板、アルミニウム又はアルミニウム合金材等を挙
げることができるが、高温焼付けに不適切なコンクリー
ト、スレートのような感熱性基材にも好ましく使用され
る。本発明の粉体塗料組成物の塗装方法としては、例え
ば、静電スプレー法、流動浸漬法等の周知の方法により
本発明の粉体塗料を被塗物の表面に所望の厚みで塗布
し、その後焼き付けることにより行うことができるし、
予熱された被塗物に前述した周知の方法により所望の厚
さで塗布することができる。The application target of the powder coating composition of the present invention is not particularly limited. For example, steel sheets for automobiles, home appliances, building materials, miscellaneous goods, etc., zinc phosphate treated steel sheets, iron phosphate treated steel sheets And aluminum or aluminum alloy materials, but are also preferably used for heat-sensitive substrates such as concrete and slate which are unsuitable for high-temperature baking. As a coating method of the powder coating composition of the present invention, for example, the powder coating of the present invention is applied to the surface of the object to be coated with a desired thickness by a known method such as an electrostatic spray method or a fluid immersion method, Then you can do it by baking,
The preheated object can be applied to a desired thickness by the known method described above.
【００３２】本発明の粉体塗料組成物は、第１粒子にお
けるエポキシ樹脂と溶融混練する硬化剤及び硬化触媒の
量が従来よりも少ないので、通常１００〜１２０℃で行
われる溶融混練の熱による樹脂の硬化反応を抑えること
ができる。その結果、塗料の貯蔵安定性が向上するほ
か、通常の焼付け温度である１６０〜１８０℃よりも低
温、例えば１１０〜１６０℃未満、好ましくは１２０〜
１５０℃で焼付ける場合において、本発明の粉体塗料組
成物の溶融粘度が低くなり、フロー性や基材との濡れ性
が向上し、塗膜の付着性が良好となる。本発明の粉体塗
料組成物は、また、上述のように、硬化剤及び硬化触媒
を第１粒子と第２粒子とに配分し、しかも溶融混練時の
熱によるエポキシ樹脂と硬化剤との反応を抑えることが
できるので、上記硬化触媒を従来の粉体塗料よりも増量
することができる結果、低温であっても硬化を促進し、
しかも速硬化が可能となる。In the powder coating composition of the present invention, since the amounts of the curing agent and the curing catalyst to be melt-kneaded with the epoxy resin in the first particles are smaller than in the conventional case, the heat of the melt-kneading usually carried out at 100 to 120 ° C. The curing reaction of the resin can be suppressed. As a result, the storage stability of the coating material is improved, and the temperature is lower than the normal baking temperature of 160 to 180 ° C, for example, less than 110 to 160 ° C, preferably 120 to 180 ° C.
In the case of baking at 150 ° C., the melt viscosity of the powder coating composition of the present invention is reduced, the flow property and the wettability with the substrate are improved, and the adhesion of the coating film is improved. As described above, the powder coating composition of the present invention also distributes the curing agent and the curing catalyst between the first particles and the second particles, and furthermore, the reaction between the epoxy resin and the curing agent due to heat during melt-kneading. As a result, it is possible to increase the amount of the curing catalyst as compared with the conventional powder coating, thereby accelerating the curing even at a low temperature,
Moreover, quick curing becomes possible.
【００３３】本発明の粉体塗料組成物は、特に各粒子の
平均体積粒子径は小さいこと、及び、予め上記第１粒子
と上記第２粒子とに分けて混練しておくことから、これ
らの粒子、更には各原料成分を均一に混合することがで
きる結果、硬化反応の反応性が高まり、焼付け後の耐衝
撃性、低粘着性等の物性に優れた塗膜を得ることができ
る。以上のように、本発明の粉体塗料組成物は、上記低
温での焼付け硬化を貯蔵安定性や塗膜の物性を損なうこ
となく行うことができる。In the powder coating composition of the present invention, in particular, since the average volume particle diameter of each particle is small, and the first and second particles are separately kneaded in advance, these particles are used. As a result of uniform mixing of the particles and the respective raw material components, the reactivity of the curing reaction is increased, and a coating film having excellent physical properties such as impact resistance and low tackiness after baking can be obtained. As described above, the powder coating composition of the present invention can perform the above-mentioned baking and curing at a low temperature without impairing the storage stability and the physical properties of the coating film.
【００３４】[0034]
【実施例】以下、具体的な実施例を挙げて本発明を詳細
に説明するが、本発明は以下の実施例により限定される
ものではない。実施例１ ビスフェノールＡ型エポキシ樹脂（エピコート１００３
Ｆ、軟化点９６℃、エポキシ当量７００〜８００ｇ／ｅ
ｑ．、油化シェルエポキシ社製）を粉砕機（クリプトロ
ン、川崎重工業社製）で粉砕し、得られた粉体を分級機
（ターボクラシファイア、日清エンジニアリング社製）
を用いて微小粒子と粗大粒子を除去して、平均粒径１２
μｍの第１粒子を得た。また、フェノール系硬化剤（エ
ピキュアー１７０、軟化点９０℃、活性水素当量２８６
〜４００ｇ／ｅｑ．、油化シェルエポキシ社製）／イミ
ダゾール系硬化触媒（キュアゾール２ＭＺ、四国化成工
業社製）を２７．４５／０．７５の重量比になるようス
ーパーミキサー（日本スピンドル製造社製）で混合攪拌
し、コニーダー（ブス社製）で溶融混合し（溶融混練温
度１１０℃、ただし、溶融混練物のコニーダー出口温
度）、冷却固化物を粗粉砕し、粉体塗料用ペレットを得
た。得られた粉体塗料用ペレットを上記第１粒子と同様
に同一条件で粉砕、分級を行い、平均粒径１２μｍの第
２粒子を得た。得られた第１粒子５９．５重量部と第２
粒子２８．２重量部をＶブレンダー（フジパウダル社
製）で混合し、粉体塗料組成物を得た。得られた粉体塗
料組成物において、上記エポキシ樹脂のエポキシ当量に
対する上記硬化剤の活性水素当量の比は、ほぼ１であ
る。なお、平均体積粒子径は、粒径測定装置（日機装社
製マイクロトラックＨＲＡＸ−１００）を用いて測定し
た。The present invention will now be described in detail with reference to specific examples.
However, the present invention is limited by the following examples.
Not something.Example 1 Bisphenol A type epoxy resin (Epicoat 1003
F, softening point 96 ° C, epoxy equivalent 700-800 g / e
q. , Yuka Shell Epoxy Co., Ltd.) crusher (Cryptoro)
, Manufactured by Kawasaki Heavy Industries, Ltd.) and the obtained powder is classified by a classifier.
(Turbo Classifier, manufactured by Nisshin Engineering)
The fine particles and the coarse particles are removed by using
μm first particles were obtained. In addition, phenolic curing agents (d
Picure 170, softening point 90 ° C, active hydrogen equivalent 286
~ 400 g / eq. , Yuka Shell Epoxy) / Imi
Dazole curing catalyst (Curesol 2MZ, Shikoku Chemicals
Scan so that the Gosha Ltd.) in a weight ratio of 27.45 / 0.75
Mixing and stirring with a paper mixer (manufactured by Nippon Spindle Manufacturing Co., Ltd.)
And it was melted and mixed at a co-kneader (manufactured by Buss) (melt-kneaded temperature
110 ° C, but the temperature at the exit of the co-kneader of the melt-kneaded product
Degree), the solidified product is coarsely pulverized to obtain pellets for powder coating.
Was. The obtained pellet for powder coating is the same as the first particle.
And crushing and classification under the same conditions,
Two particles were obtained. 59.5 parts by weight of the obtained first particles and the second particles
28.2 parts by weight of the particles were blended with a V blender (Fuji Paudal Co., Ltd.)
) To obtain a powder coating composition. The resulting powder coating
The epoxy equivalent of the epoxy resin
The ratio of the active hydrogen equivalent of the curing agent to the curing agent is approximately 1.
You. The average volume particle size is measured by a particle size measuring device (Nikkiso Co., Ltd.)
Using Microtrac HRAX-100
Was.
【００３５】実施例２ 第２粒子の原料として、エピキュアー１７０／キュアゾ
ール２ＭＺ／ジシアンジアミド系硬化剤（ＤＩＣＹ７、
活性水素当量２１ｇ／ｅｑ．、油化シェルエポキシ社
製）を１３．５３／０．６７／１．０の重量比で用い
て、平均粒径１５μｍの第１粒子と第２粒子とを得、第
１粒子５９．５重量部と第２粒子１５．２重量部とを混
合することのほかは、実施例１と同様にして粉体塗料組
成物を得た。上記エポキシ樹脂のエポキシ当量に対する
上記硬化剤の活性水素当量の比はほぼ１．１である。[0035]Example 2 Epicure 170 / Cuazo as raw material for the second particles
2MZ / dicyandiamide-based curing agent (DICY7,
Active hydrogen equivalent 21 g / eq. , Yuka Shell Epoxy
Was used at a weight ratio of 13.53 / 0.67 / 1.0.
To obtain a first particle and a second particle having an average particle size of 15 μm,
59.5 parts by weight of one particle and 15.2 parts by weight of the second particle are mixed.
Except for the combination, the powder coating
A product was obtained. Based on the epoxy equivalent of the above epoxy resin
The ratio of active hydrogen equivalents of the curing agent is approximately 1.1.
【００３６】実施例３ 第１粒子の原料として、エピコート１００３Ｆ／エピキ
ュアー１７０／キュアゾール２ＭＺを５９．５／２０．
５９／０．４６の重量比で用い、第２粒子の原料とし
て、エピキュアー１７０／キュアゾール２ＭＺを６．８
６／０．２９の重量比で用いて、平均粒径２０μｍの第
１粒子と第２粒子とを得、第１粒子８０．５５重量部と
第２粒子７．１５重量とを混合することのほかは、実施
例１と同様にして粉体塗料組成物を得た。[0036]Example 3 As a raw material of the first particles, Epicoat 1003F / Epicoat
Cure 170 / Curesol 2MZ at 59.5 / 20.
It is used in a weight ratio of 59 / 0.46 and is used as a raw material for the second particles.
6.8 from EpiCure 170 / Curesol 2MZ
Using a weight ratio of 6 / 0.29, an average particle size of 20 μm
Obtaining 1 particle and 2nd particle, 80.55 parts by weight of 1st particle
Other than mixing 7.15 weight of the second particles
A powder coating composition was obtained in the same manner as in Example 1.
【００３７】実施例４ 平均粒径３９μｍの第１粒子と第２粒子とを得ることの
ほかは、実施例３と同様にして粉体塗料組成物を得た。[0037]Example 4 Obtaining first and second particles having an average particle size of 39 μm.
Otherwise in the same manner as in Example 3, a powder coating composition was obtained.
【００３８】実施例５ 第１粒子の原料として、エピコート１００３Ｆ／エピキ
ュアー１７０／キュアゾール２ＭＺを５９．５／６．８
６／０．２４の重量比で用い、第２粒子の原料として、
エピキュアー１７０／キュアゾール２ＭＺを２０．５９
／０．５１の重量比で用いて、平均粒径２３μｍの第１
粒子と第２粒子とを得、第１粒子６６．６重量部と第２
粒子２１．１重量とを混合することのほかは、実施例１
と同様にして粉体塗料組成物を得た。[0038]Example 5 As a raw material of the first particles, Epicoat 1003F / Epicoat
Cure 170 / Curesol 2MZ 59.5 / 6.8
It is used in a weight ratio of 6 / 0.24, and as a raw material of the second particles,
Epicure 170 / Curesol 2MZ 20.59
/0.51 weight ratio and the first particle having an average particle size of 23 μm.
Particles and second particles, 66.6 parts by weight of first particles and second particles
Example 1 except that 21.1 weight of particles were mixed.
In the same manner as in the above, a powder coating composition was obtained.
【００３９】実施例６ 第１粒子に、更にカーボンブラック（三菱カーボンＭＡ
１００、三菱化学社製）を重量比で０．８含有させて、
平均粒径２１μｍの第１粒子と第２粒子とを得、第１粒
子８１．３５重量部と第２粒子７．１５重量部とを混合
することのほかは、実施例３と同様にして粉体塗料組成
物を得た。[0039]Example 6 Carbon black (Mitsubishi Carbon MA)
100, manufactured by Mitsubishi Chemical Corporation) in a weight ratio of 0.8,
First particles and second particles having an average particle size of 21 μm were obtained, and the first particles
81.35 parts by weight of the particles and 7.15 parts by weight of the second particles
Powder coating composition in the same manner as in Example 3 except that
I got something.
【００４０】実施例７ 第１粒子に、更にチタン白（タイペークＣＲ−５０、石
原産業社製）を重量比で２０含有させて、平均粒径１９
μｍの第１粒子と第２粒子とを得、第１粒子１００．５
５重量部と第２粒子７．１５重量部とを混合することの
ほかは、実施例３と同様にして粉体塗料組成物を得た。[0040]Example 7 Titanium white (Taipec CR-50, stone
(Produced by Hara Sangyo Co., Ltd.) at a weight ratio of 20 to give an average particle size of 19
μm of the first particles and the second particles, and the first particles 100.5
Mixing 5 parts by weight and 7.15 parts by weight of the second particles.
Otherwise in the same manner as in Example 3, a powder coating composition was obtained.
【００４１】比較例１ ビスフェノールＡ型エポキシ樹脂（エピコート１００３
Ｆ、軟化点９６℃、エポキシ当量７００〜８００ｇ／ｅ
ｑ．、油化シェルエポキシ株式会社製）５９．５重量
部、フェノール系硬化剤（エピキュアー１７０、軟化点
９０℃、活性水素当量２８６〜４００ｇ／ｅｑ．、油化
シェルエポキシ株式会社製）２７．４５重量部及びイミ
ダゾール系硬化触媒（キュアゾール２ＭＺ、四国化成工
業株式会社製）０．７５重量部をスーパーミキサー（日
本スピンドル製造社製）で攪拌混合し、コニーダー（ブ
ス社製）で溶融混合し、冷却固化物を粗粉砕し、粉体塗
料用ペレットを得た。得られた粉体塗料ペレットを粉砕
機で粉砕し、得られた粉体を分級機を用いて微小粒子と
粗大粒子とを除去して平均粒径４０μｍの粒子を得た。
上記エポキシ樹脂のエポキシ当量に対する上記硬化剤の
活性水素当量の比はほぼ１である。[0041]Comparative Example 1 Bisphenol A type epoxy resin (Epicoat 1003
F, softening point 96 ° C, epoxy equivalent 700-800 g / e
q. Manufactured by Yuka Shell Epoxy Co., Ltd.) 59.5 weight
Part, phenolic curing agent (Epicure 170, softening point
90 ° C., active hydrogen equivalent 286-400 g / eq. ,oiled
27.45 parts by weight of Shell Epoxy Co., Ltd. and Imi
Dazole curing catalyst (Curesol 2MZ, Shikoku Chemicals
0.75 parts by weight of Super Mixer
Stir and mix with a spindle manufacturing company,
And melt-mixed, and the cooled and solidified product is roughly pulverized and powder coated.
A pellet for use was obtained. Pulverize the obtained powder coating pellets
And pulverize the resulting powder into fine particles using a classifier.
The coarse particles were removed to obtain particles having an average particle diameter of 40 μm.
Of the curing agent to the epoxy equivalent of the epoxy resin
The ratio of active hydrogen equivalents is approximately 1.
【００４２】比較例２ エピコート１００３Ｆ、エピキュアー１７０、キュアゾ
ール２ＭＺの３つの原料について、別々に実施例１の第
１粒子製造の工程どおり粉砕、分級を行って、平均粒径
１２μｍの粒子を得、次いで、エピコート１００３Ｆ／
エピキュアー１７０／キュアゾール２ＭＺを５９．５／
２７．４５／０．７５の重量比でＶブレンダーで混合
し、粉体塗料組成物を得た。[0042]Comparative Example 2 Epicoat 1003F, EpiCure 170, Cureazo
The three raw materials of 2MZ
Pulverize and classify according to the process of 1-particle production, average particle size
12 μm particles were obtained, followed by Epicoat 1003F /
Epicure 170 / Curesol 2MZ 59.5 /
Mix by V blender at a weight ratio of 27.45 / 0.75
Thus, a powder coating composition was obtained.
【００４３】比較例３ 実施例２と同様の配合で得た平均粒径３３μｍの第１粒
子と第２粒子とをそれぞれ５９．５重量部、１５．２重
量部とり、Ｖブレンダーで混合し、粉体塗料組成物を得
た。[0043]Comparative Example 3 First particles having an average particle diameter of 33 μm obtained by the same composition as in Example 2.
59.5 parts by weight and 15.2 parts by weight of the particles and the second particles, respectively.
Measure and mix with a V blender to obtain a powder coating composition
Was.
【００４４】比較例４ キュアゾール２ＭＺを第１粒子に０．５６重量部、第２
粒子に０．１９重量部含有させて、平均粒径１５μｍの
第１粒子と第２粒子とを得、第１粒子８０．６５重量部
と第２粒子７．０５重量部とを混合することのほかは、
実施例３と同様にして粉体塗料組成物を得た。[0044]Comparative Example 4 Curesol 2MZ was added to the first particles in an amount of 0.56 parts by weight,
0.19 parts by weight of the particles, having an average particle size of 15 μm.
First particles and second particles are obtained, and the first particles are 80.65 parts by weight.
And 7.05 parts by weight of the second particles,
A powder coating composition was obtained in the same manner as in Example 3.
【００４５】比較例５ エピキュアー１７０を第１粒子に６．８６重量部、第２
粒子に２０．５９重量部、キュアゾール２ＭＺを第１粒
子に０．１９重量部、第２粒子に０．５６重量部含有さ
せて、平均粒径３５μｍの第１粒子と第２粒子とを得、
第１粒子６６．５５重量部と第２粒子２１．１５重量部
とを混合することのほかは、実施例４と同様にして粉体
塗料組成物を得た。[0045]Comparative Example 5 6.86 parts by weight of epicure 170 to the first particle, second
20.59 parts by weight, 2MZ of Curesol 1st particle
0.19 parts by weight in the powder and 0.56 parts by weight in the second particles.
To obtain first particles and second particles having an average particle diameter of 35 μm,
66.55 parts by weight of first particles and 21.15 parts by weight of second particles
And powdered in the same manner as in Example 4 except that
A coating composition was obtained.
【００４６】評価用塗膜の作製 実施例１〜７と比較例１〜５で得られた各粉体塗料組成
物を、静電塗装法により乾燥膜厚６０±１０μｍとなる
ように板厚が０．８ｍｍのリン酸亜鉛処理した冷間圧延
鋼板に均一に塗布し、１２０℃×２０分、１４０℃×２
０分の２通りの条件で焼き付けてそれぞれ２種類の塗膜
を形成した。[0046]Preparation of coating film for evaluation Each powder coating composition obtained in Examples 1 to 7 and Comparative Examples 1 to 5
The product is dried to a thickness of 60 ± 10 μm by electrostatic coating.
Rolled with zinc phosphate treated 0.8mm thick
Uniformly applied on steel plate, 120 ℃ × 20min, 140 ℃ × 2
Baking under 2/0 conditions, 2 types of coatings each
Was formed.
【００４７】評価方法 結果は、実施例については表１に示し、比較例について
は表２に示す。１．密着性 １２０℃の焼き付け温度により得られた塗膜及び１４０
℃の焼き付け温度により得られた塗膜に、予めカッター
ナイフで下地に達する１ｍｍ幅の１０×１０のゴバン目
の切り傷を入れ、セロハンテープに密着させてから一気
に引き剥がし、下地から剥離しなかった目の数を数え
て、塗料の密着性の評価を行った。[0047]Evaluation method The results are shown in Table 1 for Examples and for Comparative Examples.
Is shown in Table 2.1. Adhesion Coatings obtained with a baking temperature of 120 ° C. and 140
The coating film obtained at the baking temperature of
1 × 10 × 10 mm gobang with a knife
Make a cut and make a close contact with the cellophane tape, then
Count the number of eyes that did not peel off from the substrate
The paint adhesion was evaluated.
【００４８】２．耐衝撃性 １２０℃の焼き付け温度により得られた塗膜及び１４０
℃の焼き付け温度により得られた塗膜について、デュポ
ン式衝撃試験機を用い、１／２インチの撃芯に荷重５０
０ｇ及び１０００ｇを塗膜の上１０ｃｍ、２０ｃｍ、３
０ｃｍ、４０ｃｍ、５０ｃｍの高さからそれぞれ落下
し、塗膜に変化がなかったときの落下の高さを調べて、
耐衝撃性を評価した。評価は、下記の基準により行っ
た。 ◎ 良好 ○ やや良好 △ やや不良 × 不良[0048]2. Impact resistance Coatings obtained with a baking temperature of 120 ° C. and 140
The coating obtained at a baking temperature of
Using a half-inch impact tester and a load of 50
0 g and 1000 g are applied on the coating at 10 cm, 20 cm, 3
Drops from 0cm, 40cm, 50cm height respectively
Then, check the height of the drop when there is no change in the coating film,
The impact resistance was evaluated. Evaluation is based on the following criteria
Was. ◎ Good ○ Somewhat good △ Somewhat bad × Bad
【００４９】３．粘着性 １２０℃の焼き付け温度により得られた塗膜及び１４０
℃の焼付け温度により得られた塗膜について、粘着性を
指触により評価した。評価は、下記の基準により行っ
た。 ○ 良好 △ やや不良 × 不良[0049]3. Tackiness Coatings obtained with a baking temperature of 120 ° C. and 140
The coating film obtained at a baking temperature of
It was evaluated by finger touch. Evaluation is based on the following criteria
Was. ○ Good △ Somewhat poor × Bad
【００５０】４．貯蔵安定性 得られた粉体塗料組成物について、貯蔵開始時と４０℃
で１週間貯蔵した後でそれぞれ１６０℃におけるゲル化
時間（秒）を測定し、ゲル化時間の減率を次式により算
出し、下記の基準により評価した。 ○ 減率が２０％未満 × 減率が２０％以上[0050]4. Storage stability About the obtained powder coating composition, at the time of storage start and 40 degreeC
Gel at 160 ° C after storage for 1 week at
Measure the time (seconds) and calculate the reduction rate of gel time by the following formula.
And evaluated according to the following criteria.○ Reduction rate is less than 20% × Reduction rate is 20% or more
【００５１】[0051]
【表１】 [Table 1]
【００５２】[0052]
【表２】 [Table 2]
【００５３】表１及び表２において、第１粒子に、粉体
塗料組成物中の硬化剤の合計量の何重量％が含有され、
粉体塗料組成物中の硬化触媒の合計量の何重量％が含有
されているかを記入した。表１と表２とを比較すると、
硬化剤又は硬化触媒の第１粒子中の含有量（％）が本発
明の範囲内にない比較例では、評価項目の少なくとも何
れかについて劣るのに対し、硬化剤及び硬化触媒の第１
粒子中の含有量（％）が本発明の範囲内にある実施例で
は、各評価項目について優れていることがわかった。In Tables 1 and 2, the first particles contained a percentage by weight of the total amount of the curing agent in the powder coating composition,
What weight% of the total amount of the curing catalyst of the powder coating composition is filled out or is contained. Comparing Table 1 and Table 2,
In Comparative Examples in which the content (%) of the curing agent or the curing catalyst in the first particles is not within the range of the present invention, at least one of the evaluation items is inferior, whereas
In Examples in which the content (%) in the particles was within the range of the present invention, it was found that each evaluation item was excellent.
【００５４】[0054]
【発明の効果】本発明の粉体塗料組成物は、上述の構成
よりなるので、低温硬化性の粉体塗料であっても貯蔵安
定性に優れるとともに、塗膜焼付け後の密着性、耐衝撃
性、低粘着性等の物性が良好な塗膜が得られる。As described above, the powder coating composition of the present invention has the above-mentioned constitution, so that even if it is a low-temperature curable powder coating composition, it has excellent storage stability, adhesion after coating film baking, and impact resistance. A coating film having good physical properties such as properties and low tackiness can be obtained.
フロントページの続き (72)発明者 鈴木 誠 大阪府寝屋川市池田中町19番17号 日本ペ イント株式会社内 (72)発明者 山辺 勲 大阪府寝屋川市池田中町19番17号 日本ペ イント株式会社内 Ｆターム(参考） 4J038 DB031 DB041 DB061 DB071 GA07 JA42 JA64 JB03 JB30 JB32 JB39 JC13 JC22 JC38 JC39 KA04 MA02 MA14 NA11 NA12 NA26 PA19 Continued on the front page (72) Inventor Makoto Suzuki 19-17 Ikedanakamachi, Neyagawa-shi, Osaka Japan Paint Co., Ltd. F term (reference) 4J038 DB031 DB041 DB061 DB071 GA07 JA42 JA64 JB03 JB30 JB32 JB39 JC13 JC22 JC38 JC39 KA04 MA02 MA14 NA11 NA12 NA26 PA19
Claims (5)
なる第１粒子と、硬化剤及び硬化触媒からなる第２粒子
とからなる粉体塗料組成物であって、前記第１粒子及び
前記第２粒子の平均体積粒子径が５μｍ以上２５μｍ未
満であり、前記粉体塗料組成物中の硬化剤の合計量の０
〜８０重量％が前記第１粒子に含有され、前記粉体塗料
組成物中の硬化触媒の合計量の０〜７０重量％が前記第
１粒子に含有されていることを特徴とする粉体塗料組成
物。1. A powder coating composition comprising: first particles comprising an epoxy resin, a curing agent and a curing catalyst; and second particles comprising a curing agent and a curing catalyst, wherein the first particle and the second particle The particles have an average volume particle diameter of 5 μm or more and less than 25 μm, and the total volume of the curing agent in the powder coating composition is 0
A powder coating composition characterized in that the first particles comprise about 80% by weight of the first particles, and the first particles comprise 0 to 70% by weight of the total amount of the curing catalyst in the powder coating composition. Composition.
なる第１粒子と、硬化剤及び硬化触媒からなる第２粒子
とからなる粉体塗料組成物であって、前記第１粒子及び
前記第２粒子の平均体積粒子径が２５〜５０μｍであ
り、前記粉体塗料組成物中の硬化剤の合計量の３０〜８
０重量％が前記第１粒子に含有され、前記粉体塗料組成
物中の硬化触媒の合計量の０〜７０重量％が前記第１粒
子に含有されていることを特徴とする粉体塗料組成物。2. A powder coating composition comprising: first particles comprising an epoxy resin, a curing agent and a curing catalyst; and second particles comprising a curing agent and a curing catalyst, wherein the first particles and the second particles comprise the second particles. The particles have an average volume particle diameter of 25 to 50 μm and a total amount of 30 to 8 of the curing agent in the powder coating composition.
0% by weight is contained in the first particles, and 0 to 70% by weight of the total amount of the curing catalyst in the powder coating composition is contained in the first particles. object.
合物及び酸化合物からなる群より選択される少なくとも
１つであり、エポキシ樹脂のエポキシ当量に対する粉体
塗料組成物中の全硬化剤の活性水素当量の比は、０．７
〜１．３である請求項１又は２記載の粉体塗料組成物。3. The curing agent is at least one selected from the group consisting of an amine compound, a phenol compound and an acid compound, and has an active hydrogen equivalent of all curing agents in the powder coating composition with respect to an epoxy equivalent of the epoxy resin. Is 0.7
The powder coating composition according to claim 1, wherein the composition is from 1.3 to 1.3.
〜２２００ｇ／ｅｑであって、ビスフェノールＡ型エポ
キシ樹脂又はビスフェノールＦ型エポキシ樹脂である請
求項１、２又は３記載の粉体塗料組成物。4. An epoxy resin having an epoxy equivalent of 600
The powder coating composition according to claim 1, 2 or 3, wherein the composition is a bisphenol A type epoxy resin or a bisphenol F type epoxy resin.
組成物の製造方法であって、エポキシ樹脂、硬化剤及び
硬化触媒からなる成分を混練し粉砕することにより第１
粒子を得る工程；硬化剤及び硬化触媒からなる成分を混
練し粉砕することにより第２粒子を得る工程；前記第１
粒子及び前記第２粒子を均一に混合する工程；からなる
ことを特徴とする粉体塗料組成物の製造方法。5. The method for producing a powder coating composition according to claim 1, wherein the first component is formed by kneading and pulverizing a component comprising an epoxy resin, a curing agent and a curing catalyst.
A step of obtaining particles; a step of kneading and pulverizing a component comprising a curing agent and a curing catalyst to obtain second particles;
Mixing the particles and the second particles uniformly. A method for producing a powder coating composition, comprising:
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001066457A JP2002265864A (en) | 2001-03-09 | 2001-03-09 | Powder coating composition and method for producing the same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2001066457A JP2002265864A (en) | 2001-03-09 | 2001-03-09 | Powder coating composition and method for producing the same |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JP2002265864A true JP2002265864A (en) | 2002-09-18 |
Family
ID=18924940
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2001066457A Withdrawn JP2002265864A (en) | 2001-03-09 | 2001-03-09 | Powder coating composition and method for producing the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2002265864A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009220328A (en) * | 2008-03-14 | 2009-10-01 | Nippon Steel Corp | Polyolefin-coated steel material |
| WO2020159048A1 (en) * | 2019-01-28 | 2020-08-06 | 주식회사 케이씨씨 | Powder coating composition |
-
2001
- 2001-03-09 JP JP2001066457A patent/JP2002265864A/en not_active Withdrawn
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009220328A (en) * | 2008-03-14 | 2009-10-01 | Nippon Steel Corp | Polyolefin-coated steel material |
| WO2020159048A1 (en) * | 2019-01-28 | 2020-08-06 | 주식회사 케이씨씨 | Powder coating composition |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP4405938B2 (en) | Raw material mixed powder composition and manufacturing method thereof | |
| US6905778B2 (en) | Powder coating composition, method for the curing thereof, and articles derived therefrom | |
| JPH0578605A (en) | Powder coating giving uneven pattern, its production, production device and coating method therefor, and coating film therefrom | |
| CN114316752B (en) | Powder coating composition with stable pearlescent texture, preparation method and coating thereof | |
| JPS62292869A (en) | Powder coating | |
| CA2289794C (en) | Granulated powdery paint and process for producing the same | |
| JP2711036B2 (en) | Powder coatings and raw materials for powder coatings | |
| WO1999057209A1 (en) | Thermosetting powder coating composition | |
| WO1995025145A1 (en) | Powder paint, method of manufacturing the same, and method of painting using the paint | |
| JP2002265864A (en) | Powder coating composition and method for producing the same | |
| JPS6332827B2 (en) | ||
| CN108473816A (en) | Powder coating, the manufacturing method of powder coating and coated article | |
| MXPA01009105A (en) | Powder coating compositions. | |
| JP2899966B2 (en) | Powder paint | |
| JP4484291B2 (en) | Toning method and manufacturing method of powder coating | |
| JP4939022B2 (en) | Method for producing powder coating | |
| JP2001062385A (en) | Coating method | |
| KR20120077167A (en) | Epoxy semi-matt powder coatings for engine block, manufacturing method thereof and coating method | |
| JP2008063581A (en) | Method for manufacturing silver-metallic powder coating for tribocharging spray gun | |
| JP2005263939A (en) | Epoxy resin powder coating | |
| JP2003213216A (en) | Silver metallic powder coating material | |
| JP2001070874A (en) | Coating method | |
| JP2004018827A (en) | Method for producing powder coating | |
| JPS6228194B2 (en) | ||
| JPH08302241A (en) | Powdery coating material |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| RD04 | Notification of resignation of power of attorney |
Free format text: JAPANESE INTERMEDIATE CODE: A7424 Effective date: 20040323 |
|
| A621 | Written request for application examination |
Free format text: JAPANESE INTERMEDIATE CODE: A621 Effective date: 20080219 |
|
| A761 | Written withdrawal of application |
Effective date: 20090915 Free format text: JAPANESE INTERMEDIATE CODE: A761 |