JP2003286445A - Method for manufacturing heat-curing powder water dispersion coating composition - Google Patents

Method for manufacturing heat-curing powder water dispersion coating composition

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Publication number
JP2003286445A
JP2003286445A JP2002090441A JP2002090441A JP2003286445A JP 2003286445 A JP2003286445 A JP 2003286445A JP 2002090441 A JP2002090441 A JP 2002090441A JP 2002090441 A JP2002090441 A JP 2002090441A JP 2003286445 A JP2003286445 A JP 2003286445A
Authority
JP
Japan
Prior art keywords
resin
group
coating composition
heat
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.)
Pending
Application number
JP2002090441A
Other languages
Japanese (ja)
Inventor
Kazuo Soga
和夫 曽我
Isamu Takabayashi
勇 高林
Hirohisa Tsuda
裕久 津田
Hiroyuki Matsumoto
宏幸 松本
Mutsuo Kuramoto
睦雄 庫本
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Kansai Paint Co Ltd
Original Assignee
Kansai Paint Co Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Kansai Paint Co Ltd filed Critical Kansai Paint Co Ltd
Priority to JP2002090441A priority Critical patent/JP2003286445A/en
Publication of JP2003286445A publication Critical patent/JP2003286445A/en
Pending legal-status Critical Current

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Abstract

<P>PROBLEM TO BE SOLVED: To provide a method for manufacturing a heat-curing powder water dispersion coating composition. <P>SOLUTION: The method is characterized by combining a heat-curing base resin having a base resin such as an acrylic resin, a polyester resin, a fluororesin, a silicone resin, an epoxy resin, a amine-modified resin, a phenol resin, a urethane resin and the like introduced with a functional group such as a hydroxy group, a carboxy group, an epoxy group and an unsaturated group thereto with a curing agent having a functional group which is curable with these functional group, for example, such as a blocked ployisocyanate compound, a polyepoxide, a polycarboxylic acid compound, an acid anhydride, a carboxy group- and acid anhydride group-containing carboxylic acid compound, an amino resin, a phenol resin, a hydrazide compound, a peroxide and the like, melt-kneading the resultant to obtain a heatcuring powder resin composition and wet-dispersing the heat curing powder resin composition with a volume average particle diameter of 10-100 μm using a pipeline bead mill, thereby obtaining the heat-curing powder water dispersion coating composition having a volume average particle diameter of 5-20 μm. <P>COPYRIGHT: (C)2004,JPO

Description

【発明の詳細な説明】 【0001】 【発明の属する技術分野】本発明は、新規な熱硬化型粉
体水分散液塗料組成物の製造方法に関する。 【0002】 【従来の技術】近年、有機溶剤削減、安全性等の面か
ら、水溶性樹脂を塗料中の主ビヒクルとした水性塗料
が、有機溶剤系塗料に置換わる動きが高まっている。し
かしながら、これらの水性塗料は樹脂を水媒体中に溶解
させる為に、多くの親水基を持たせるなどにより、その
塗膜は耐水性などの性能面で劣るし、高揮発分濃度に調
整することも難しいことから、塗装時にタレやすく作業
性面に問題があるし、また、貯蔵劣化も起こしやすい。 【0003】また、粉体塗料組成物を水媒体中に分散せ
しめた粉体水分散液塗料組成物が種々提案されている。
ところが、この粉体水分散液塗料組成物は粉体塗料を先
ず作成した後に、水媒体中にサンドミル等を用いること
によって分散させるが、通常の40〜60μm程度の粉
体塗料を使用する際は、ミキシングタンク等で調合時に
沈降が生じ易く、水分散を行なうことが難しい。 【0004】この時、水溶性の増粘剤を添加して沈降を
防ぐ方法もあるが、この場合、サンドミル等の分散機で
粉体塗料を粉砕し細かくするに従い、粘度が急激に上昇
するといった問題がある。 【0005】また予め、10〜20μm程度の粒子径を
もつ粉体塗料を水分散する手段もあるが、この粒子径の
粉体塗料を得るにはコストがかかる。 【0006】 【発明が解決しようとする課題】粉体塗料を水媒体中に
分散する工程において、調合時に沈降を起こすことなく
連続的に水分散が可能な、新たな分散機を用いて粉体水
分散液塗料の生産効率を高めることにある。 【0007】 【課題を解決するための手段】本発明者は、上記目的を
達成すべく鋭意努力し、種々検討した結果、本発明を見
出した。通常の粉体塗料をパイプラインビーズミルを用
いることにより、粉体水分散液塗料組成物を容易に製造
方法を提供するものである。 【0008】 【発明の実施の形態】該粉体水分散液塗料組成物におい
て、水中に分散させるために使用する熱硬化型粉体粒子
は、従来から公知の熱硬化型粉体塗料を使用することが
できる。具体的には、例えば、基体樹脂として、アクリ
ル系樹脂、ポリエステル系樹脂、フッ素系樹脂、シリコ
ン系樹脂、エポキシ系樹脂、アミン変性樹脂、フェノー
ル系樹脂、ウレタン系樹脂等の基体樹脂に水酸基、カル
ボキシル基、エポキシ基、不飽和基等の官能基を導入し
た熱硬化性基体樹脂にこれらの官能基と硬化する官能基
を有する、例えば、ブロックポリイソシアネート化合
物、ポリエポキシド、ポリカルボン酸化合物、酸無水
物、カルボキシル基及び酸無水基含有カルボン酸化合
物、アミノ樹脂、フェノール樹脂、ヒドラジド系化合
物、過酸化物等の硬化剤を配合してなるものが挙げられ
る。これらの基体樹脂及び硬化剤に挙げた原料は1種も
しくは2種以上組み合せて使用することができる。 【0009】また、熱硬化型粉体粒子には、必要に応じ
て着色顔料、体質顔料、防錆顔料、表面調整剤、粘度調
整剤等も配合することが可能である。 【0010】こうして得られた粉体塗料塗料組成物平均
粒子径は、50%累積粒子径(該累積粒子径はマイクロ
トラックFRA(LEEDS&NORTHRUP社製)を用いて測定し
た。)は、40〜60μmの間にある。 【0011】次にこの粉体塗料樹脂組成物をパイプライ
ンビーズミルにて製造する方法を説明する。パイプライ
ンビーズミル(井上製作所(株)製)は図1に示したよう
に縦形のアニュラー型ビーズミルであり、図2に示した
特殊なローターの働きにより、従来のビーズミルの数十
倍の処理流量が得られることを特徴としている。入口配
管5より入った水分散液は、ローター1の外周部とベセ
ル2の内壁の間隙を下降する。この間に、ガラスビーズ
等のメジアと伴に強力に攪拌され、粉体塗料粒子は粉砕
される。また、ローター外周面のスパイク状突起のスク
リュー作用によりメジアはローター下部を通ってロータ
ー内側とスクリーン面の間隙に送り込まれる。そして遠
心力により比重の大きいメジアと水分散液は分離され、
比重の大きいメジアはスリットを通ってローター外周面
とベセル内壁の間隙に戻される。ミルベースはスクリー
ンを通って出口配管より排出される。このようにメジア
がローター外周面のスパイク状突起のスクリュー作用と
遠心力の効果により、ローター下部を通ってローター外
側から内側へ、そしてスリットを通って内側から外側へ
と循環される。このローターの回転により生ずる強力な
メジアの循環により、高濃度の水分散液でもメジアを偏
在させることなく高流量の処理が可能となる。このパイ
プラインミルを使った図3に示したような循環分散シス
テムにより、高流量による循環分散を行う。高流量であ
るため、配管での沈降が防止できる。さらに、循環槽に
おいて冷水を通したジャケットによって冷却された水分
散液の顕熱により、ミル内での温度上昇を抑えることが
できる。 【0012】 【実施例】以下、実施例により具体的に説明するが、本
発明は実施例に限定されるものではない。部及び%はそ
れぞれ重量基準である。 【0013】熱硬化型粉体塗料組成物の製造例 軟化温度110℃、水酸基価30のポリエステル樹脂6
0部、NCO=15%のε−カプロラクタムブロックイ
ソホロンジイソシアネ−ト化合物9部、酸化チタン顔料
30部、表面調整剤0.9部、硬化促進剤0.1部を上
記配合物をドライブレンド(ヘンシェルミキサ−)、溶
融混合分散(2軸エクストル−ダ−混練機)、冷却、粗
粉砕、微粉砕(アトマイザ−)、濾過を行って熱硬化型
ポリエステル粉体塗料組成物を製造した。 【0014】熱硬化型粉体水分散液塗料組成物の製造例
(実施例) パイプラインミルのタンク部に、水100部を取り、H
LB=12のノニオン系界面活性剤0.2部、消泡剤
0.5部、防腐剤0.2を添加し、溶解して水媒体を準
備した。ここに上記熱硬化型粉体塗料組成物100部を
攪拌しながら添加した。ベセル内にガラスビーズ(ハイ
ビーD16)を充填率80%で加え、パイプラインミル
の循環層内を25℃に保ちながら、周速10m/sで、
平均粒子径が約8μmとなるまで湿式分散を行ない、ろ
過を経て熱硬化型粉体水分散液塗料組成物を得た。この
熱硬化型粉体水分散液塗料組成物100部に、増粘剤を
1部添加し、該熱硬化型粉体水分散液塗料組成物を得
た。この得られた熱硬化型粉体水分散液塗料組成物の体
積平均粒子径は7.3μm、最大粒子径は22.3μm
であった。また、20℃にて粘度を測定(B型粘度計:
60rpm)したところ1980mPa・sであった。 【0015】塗膜試験 上記のようにして作成した、熱硬化型粉体水分散液組成
物をSPCC・SD(リン酸亜鉛処理)板上にエアース
プレーで塗装を行なった。塗装後10分間放置した後、
乾燥炉で180℃で20分間素材温度を保持して30〜
40μmの焼付塗膜を得た。この各塗装板で、40℃の
高温水槽中に240時間の浸漬試験、沸騰水に4時間浸
漬の浸漬試験を行なった後、1mm碁盤目試験を行ない、
セロファンテープではくり試験を行なったところ、実施
例は、良好な密着性を示した。また、実施例のものは耐
塩水噴霧試験(JIS Z−2371に従って試験し、
カット(線状切きず)部からのクリープ巾片側2.0mm
以内及びカット部以外の塗膜のフクレが8F(AST
M)以下のとき合格とする。)で良好な結果を示した。 【0016】 【発明の効果】本発明により粉体水分散液塗料組成物
を、効率よく容易に製造が可能となる。
Description: BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a novel thermosetting powdery water-based dispersion coating composition. 2. Description of the Related Art In recent years, from the viewpoints of reduction of organic solvents, safety, and the like, there has been an increasing movement to replace water-based paints, which use a water-soluble resin as a main vehicle in the paints, with organic solvent-based paints. However, these water-based paints have many hydrophilic groups in order to dissolve the resin in the aqueous medium, so that the coating film is inferior in performance such as water resistance and should be adjusted to a high volatile concentration. Is difficult, so that it is easy to sag at the time of painting, and there is a problem in workability, and storage deterioration is apt to occur. [0003] Also, there have been proposed various water-based dispersion coating compositions in which the powder coating composition is dispersed in an aqueous medium.
However, this powder aqueous dispersion coating composition is prepared by first preparing a powder coating, and then dispersed in an aqueous medium by using a sand mill or the like, but when using a normal powder coating of about 40 to 60 μm, It is easy for sedimentation to occur during mixing in a mixing tank or the like, and it is difficult to disperse in water. At this time, there is a method of adding a water-soluble thickener to prevent sedimentation. In this case, as the powder coating material is pulverized by a dispersing machine such as a sand mill and made finer, the viscosity sharply increases. There's a problem. There is a means for dispersing a powder coating having a particle diameter of about 10 to 20 μm in water in advance, but it is costly to obtain a powder coating having this particle diameter. [0006] In the process of dispersing the powder coating material in an aqueous medium, the powder is prepared using a new dispersing machine capable of continuous water dispersion without causing sedimentation during preparation. An object of the present invention is to increase the production efficiency of a water dispersion paint. The inventor of the present invention has made intensive efforts to achieve the above object, and as a result of various studies, have found the present invention. An object of the present invention is to provide a method for easily producing a powdery aqueous dispersion coating composition by using a pipeline bead mill for a usual powder coating. [0008] In the water-based powder dispersion coating composition, as the thermosetting powder particles used for dispersing in water, a conventionally known thermosetting powder coating is used. be able to. Specifically, for example, as a base resin, an acrylic resin, a polyester resin, a fluorine resin, a silicon resin, an epoxy resin, an amine-modified resin, a phenol resin, a urethane resin, etc. Group, epoxy group, thermosetting base resin into which a functional group such as an unsaturated group is introduced, having a functional group that cures with these functional groups, for example, block polyisocyanate compound, polyepoxide, polycarboxylic acid compound, acid anhydride And a carboxylic acid compound containing a carboxyl group and an acid anhydride group, an amino resin, a phenol resin, a hydrazide compound, and a curing agent such as a peroxide. The raw materials listed as the base resin and the curing agent can be used alone or in combination of two or more. [0009] The thermosetting powder particles may also contain a coloring pigment, an extender pigment, a rust preventive pigment, a surface conditioner, a viscosity adjuster, and the like, if necessary. The powder coating composition thus obtained has a 50% cumulative particle size (measured using a Microtrac FRA (manufactured by LEEDS & NORTHHRUP)) having an average particle size of 40 to 60 μm. between. Next, a method of producing the powder coating resin composition by a pipeline bead mill will be described. A pipeline bead mill (manufactured by Inoue Seisakusho Co., Ltd.) is a vertical annular type bead mill as shown in FIG. 1, and a special rotor as shown in FIG. It is characterized by being obtained. The aqueous dispersion that has entered through the inlet pipe 5 descends between the outer peripheral portion of the rotor 1 and the inner wall of the vessel 2. During this time, the mixture is vigorously stirred with the media such as glass beads, and the powder coating particles are crushed. Further, the media is fed into the gap between the inside of the rotor and the screen surface through the lower portion of the rotor by the screw action of the spike-shaped projections on the outer peripheral surface of the rotor. Then, the centrifugal force separates the media with large specific gravity and the aqueous dispersion,
The media with a large specific gravity is returned to the gap between the outer peripheral surface of the rotor and the inner wall of the vessel through the slit. The mill base is discharged from the outlet pipe through the screen. In this way, the media is circulated from the outside of the rotor to the inside through the lower part of the rotor and from the inside to the outside through the slit by the effect of the screw action and the centrifugal force of the spike-shaped projections on the outer peripheral surface of the rotor. Due to the strong circulation of the media caused by the rotation of the rotor, a high flow rate treatment can be performed without uneven distribution of the media even in a highly concentrated aqueous dispersion. The circulating dispersion system using the pipeline mill as shown in FIG. 3 performs circulating dispersion at a high flow rate. Because of the high flow rate, sedimentation in the piping can be prevented. Further, the sensible heat of the aqueous dispersion cooled by the jacket through which the cold water flows in the circulation tank can suppress the temperature rise in the mill. Hereinafter, the present invention will be described in detail with reference to examples, but the present invention is not limited to the examples. Parts and percentages are each by weight. Preparation Example of Thermosetting Powder Coating Composition Polyester resin 6 having a softening temperature of 110 ° C. and a hydroxyl value of 30
0 parts, 9 parts of an ε-caprolactam block isophorone diisocyanate compound having an NCO of 15%, 30 parts of a titanium oxide pigment, 0.9 parts of a surface conditioner, and 0.1 parts of a curing accelerator are dry-blended with the above composition. (Henschel mixer), melt mixing and dispersion (biaxial extruder kneader), cooling, coarse pulverization, fine pulverization (atomizer), and filtration to produce a thermosetting polyester powder coating composition. Preparation Example of Thermosetting Powdered Water Aqueous Dispersion Coating Composition (Example) 100 parts of water was placed in a tank of a pipeline mill.
An aqueous medium was prepared by adding and dissolving 0.2 part of a nonionic surfactant having an LB of 12, 0.5 part of an antifoaming agent, and 0.2 of a preservative. Here, 100 parts of the thermosetting powder coating composition was added with stirring. At a peripheral speed of 10 m / s, glass beads (Hibee D16) were added at a filling rate of 80% into the vessel, and the inside of the circulating layer of the pipeline mill was maintained at 25 ° C.
Wet dispersion was performed until the average particle diameter became about 8 μm, and filtration was performed to obtain a thermosetting powder aqueous dispersion coating composition. One part of a thickener was added to 100 parts of the thermosetting powder aqueous dispersion coating composition to obtain the thermosetting powder aqueous dispersion coating composition. The volume average particle diameter of the obtained thermosetting powder aqueous dispersion coating composition is 7.3 μm, and the maximum particle diameter is 22.3 μm.
Met. The viscosity was measured at 20 ° C. (B-type viscometer:
The pressure was 1980 mPa · s at 60 rpm). Coating Film Test The thermosetting powder aqueous dispersion composition prepared as described above was applied to an SPCC SD (zinc phosphate treatment) plate by air spray. After leaving for 10 minutes after painting,
Keep the material temperature at 180 ° C for 20 minutes in a drying oven and
A baked film of 40 μm was obtained. Each coated plate was subjected to a 240-hour immersion test in a high-temperature water bath at 40 ° C. and a 4-hour immersion test in boiling water, followed by a 1 mm grid test.
When a peeling test was performed using cellophane tape, the example showed good adhesion. Moreover, the thing of an Example tests according to the salt spray test (JISZ-2371),
Creep width from cut (linear cut) 2.0 mm on one side
8F (AST)
M) Pass if: ) Showed good results. According to the present invention, it is possible to efficiently and easily produce a water-based powder dispersion coating composition.

【図面の簡単な説明】 【図1】本発明で使用するパイプラインビーズミルの断
面概略図を示す。 【図2】パイプラインビーズミルのロータの断面概略図
を示す。 【図3】パイプラインビーズミルを使用した分散システ
ムの概略図を示す。 【符号の説明】 1、ローター 2、ベセル 3、シャフト 4、軸シール 5、入口配管 6、スクリーン 7、出口配管 8、スリット 9、スパイク状突起
BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 shows a schematic sectional view of a pipeline bead mill used in the present invention. FIG. 2 shows a schematic sectional view of a rotor of a pipeline bead mill. FIG. 3 shows a schematic diagram of a dispersion system using a pipeline bead mill. [Description of References] 1, rotor 2, vessel 3, shaft 4, shaft seal 5, inlet pipe 6, screen 7, outlet pipe 8, slit 9, spike-shaped projection

───────────────────────────────────────────────────── フロントページの続き (72)発明者 松本 宏幸 神奈川県平塚市東八幡4丁目17番1号 関 西ペイント株式会社内 (72)発明者 庫本 睦雄 神奈川県平塚市東八幡4丁目17番1号 関 西ペイント株式会社内 Fターム(参考) 4J038 CD091 CG001 DA061 DA062 DA112 DD001 DG001 DG302 DL031 GA01 GA03 GA06 GA07 JA35 JA66 JB17 KA03 MA08 MA10 MA14 PA02 PA19   ────────────────────────────────────────────────── ─── Continuation of front page    (72) Inventor Hiroyuki Matsumoto             4-17-1, Higashi-Hachiman, Hiratsuka-shi, Kanagawa             Nishi Paint Co., Ltd. (72) Inventor Mutsuo Kuromoto             4-17-1, Higashi-Hachiman, Hiratsuka-shi, Kanagawa             Nishi Paint Co., Ltd. F term (reference) 4J038 CD091 CG001 DA061 DA062                       DA112 DD001 DG001 DG302                       DL031 GA01 GA03 GA06                       GA07 JA35 JA66 JB17 KA03                       MA08 MA10 MA14 PA02 PA19

Claims (1)

【特許請求の範囲】 【請求項1】溶融混練により得られた熱硬化型粉体塗料
組成物の体積平均粒子径が10〜100μmのものをパ
イプラインビーズミルを用いて湿式分散させることによ
り、体積平均粒子径が5〜20μmの熱硬化型粉体水分
散液塗組成物を得ることを特徴とする製造方法。
Claims: 1. A thermosetting powder coating composition obtained by melt-kneading and having a volume average particle diameter of 10 to 100 μm is wet-dispersed using a pipeline bead mill to obtain a volume. A method for producing a thermosetting powder aqueous dispersion coating composition having an average particle diameter of 5 to 20 μm.
JP2002090441A 2002-03-28 2002-03-28 Method for manufacturing heat-curing powder water dispersion coating composition Pending JP2003286445A (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH02239911A (en) * 1989-03-14 1990-09-21 Daikin Ind Ltd Continuous manufacture of polytetrafluoroethylene wet powder
JPH0751590A (en) * 1993-08-11 1995-02-28 Nittetsu Mining Co Ltd Method for wet type dispersion and pulverization
JPH11343432A (en) * 1998-06-02 1999-12-14 Dainippon Toryo Co Ltd Production of aqueous disperse coating material and production of powder coating material
JP2001343517A (en) * 2000-06-01 2001-12-14 Dainippon Printing Co Ltd Pigment dispersion composition for color filter, method for manufacturing the same and color filter for display
JP2002028529A (en) * 2000-07-18 2002-01-29 Tokin Corp Grinding method and device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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