JPH1180602A - Preparation of powder slurry coating - Google Patents

Preparation of powder slurry coating

Info

Publication number
JPH1180602A
JPH1180602A JP25046297A JP25046297A JPH1180602A JP H1180602 A JPH1180602 A JP H1180602A JP 25046297 A JP25046297 A JP 25046297A JP 25046297 A JP25046297 A JP 25046297A JP H1180602 A JPH1180602 A JP H1180602A
Authority
JP
Japan
Prior art keywords
resin
aqueous medium
curing agent
melt
mixture
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
JP25046297A
Other languages
Japanese (ja)
Inventor
Yasuyoshi Kashiwagi
恭義 柏木
Munekazu Hayashi
宗和 林
Kinji Matsukuri
謹爾 真造
Hidenori Ishikawa
英宣 石川
Noboru Ogoshi
昇 小越
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.)
DIC Corp
Original Assignee
Dainippon Ink and Chemicals 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 Dainippon Ink and Chemicals Co Ltd filed Critical Dainippon Ink and Chemicals Co Ltd
Priority to JP25046297A priority Critical patent/JPH1180602A/en
Publication of JPH1180602A publication Critical patent/JPH1180602A/en
Pending legal-status Critical Current

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Abstract

PROBLEM TO BE SOLVED: To provide a process for preparing a powder slurry coating which can eliminate the need to provide the step of grinding and can improve heat stability and the appearance of coatings by comprising mixing a water dispersion of a curing agent with a water dispersion of fines particles of a resin prepd. by mixing a resin melt contg. a synthetic resin for a powder coating with an aq. medium. SOLUTION: A resin melt obtd. by heat-melting a, kneaded product of a synthetic resin for a powder coating and optionally a photoinitiator and a color pigment is mixed with an aq. medium heated to a temp. around the softening point of the resin under pressure. The resin melt is mechanically emulsified and dispersed in the aq. medium while maintaining the mixture at a temp. around the softening point of the resin. The system is rapidly cooled to obtain a water dispersion (A) of fines particles of the resin. Separately, a melt of a curing agent obtd. by heat melting a curing agent is mixed with an aq. medium heated to a temp. around the softening point of the curing agent. The melting of the curing agent is mechanically emulsified and dispersed in the aq. medium while maintaining the mixture at a temp. around the softening point of the curing agent. The system is rapidly cooled to obtain a water dispersion (B) of fine particles of the curing agent. Next, the component A is mixed with the component B.

Description

【発明の詳細な説明】DETAILED DESCRIPTION OF THE INVENTION

【0001】[0001]

【発明の属する技術分野】本発明は塗料等の技術分野に
おいて用いられる、粉体スラリー塗料の製造方法に関す
る。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing a powder slurry paint used in the technical field of paint and the like.

【0002】[0002]

【従来の技術】粉体塗料等の製造方法としては、従来か
ら湿式法と乾式法がある。湿式法は通常の溶剤型塗料と
ほとんど同じ方法で塗料を作った後、溶剤を留去して粉
砕するか、大量の非溶剤の中に噴出分散後、ろ別乾燥す
るか、あるいは加温空気中にスプレーして粉状にすると
同時に溶剤を除去する等の方法が行われている。しかし
技術上の問題が多い上に現状では後者に比べてコスト高
となる為、実用されていない。
2. Description of the Related Art Methods for producing powder coatings and the like include a wet method and a dry method. In the wet method, a paint is made in almost the same way as a normal solvent-based paint, and then the solvent is distilled off and pulverized. A method of spraying the powder into the powder and removing the solvent at the same time has been performed. However, it is not practically used because it has many technical problems and the cost is higher than the latter at present.

【0003】乾式法は各種原料を混合、加熱溶融、混練
し、さらに冷却、粉砕、分級する各工程からなる。有機
溶剤を使用しない塗料として今後さらなる発展が考えら
れる。 しかし乾式法には、下記の問題点が列記され
る。
[0003] The dry method comprises various steps of mixing, heating, melting and kneading various raw materials, and further cooling, pulverizing and classifying. Further development is expected in the future as a paint that does not use organic solvents. However, the following problems are listed in the dry method.

【0004】1)樹脂と硬化剤とを主原料とする粉体塗
料において、硬化剤を数十ミクロンに粉砕したものと樹
脂等とを混練する工程で、熱安定性を維持する為に、硬
化剤の軟化点以下の温度で行わねばならない為十分な混
練が出来ず、塗膜の外観が悪い。
[0004] 1) In a powder coating containing a resin and a curing agent as main raw materials, in a step of kneading a material obtained by pulverizing the curing agent to several tens of microns with a resin or the like, to maintain heat stability, Since the temperature must be lower than the softening point of the agent, sufficient kneading cannot be performed, and the appearance of the coating film is poor.

【0005】2)乾式法によって製造される粉体塗料
は、形状が不定形にならざるを得ず、特に体積平均径が
20ミクロン以下の粉体塗料の場合には粉体としての流
動性が極端に悪化する。
[0005] 2) Powder coatings produced by the dry method must be irregular in shape, and especially in the case of powder coatings having a volume average diameter of 20 microns or less, the fluidity as a powder is poor. Extremely worse.

【0006】3)粉体が小粒径になればなるほど粉体重
量当たりに必要な粉砕エネルギーが飛躍的に増大し、コ
スト高になってしまう。近年粉体塗料の動向として、表
面の平滑性および光沢性向上の要請から粉体塗料の平均
粒子径は益々小粒径化する方向にあり、近い将来10ミ
クロン以下の超微粒子粉体塗料の出現が期待されている
が、従来技術の粉砕法の粉体塗料では、非常に製造が困
難であり、またできたとしてもコスト高になる。
[0006] 3) The smaller the particle size of the powder, the more the pulverizing energy required per powder weight is drastically increased, resulting in an increase in cost. In recent years, the trend of powder coatings is that the average particle size of powder coatings is becoming smaller and smaller due to the demand for improved surface smoothness and gloss. However, it is very difficult to produce the powder coating by the conventional pulverization method, and even if it can be performed, the cost is high.

【0007】上記の問題を湿式法、乾式法で克服するの
は非常に困難である。本発明の粉体スラリー塗料は、従
来上記で得られる粉体塗料を水性媒体中に分散させるこ
とによって製造される。
[0007] It is very difficult to overcome the above problems by a wet method or a dry method. The powder slurry coating of the present invention is conventionally produced by dispersing the powder coating obtained above in an aqueous medium.

【0008】[0008]

【発明が解決しようとする課題】本発明は、樹脂と硬化
剤とを原料として含む粉体塗料を製造する場合、従来法
を抜本的に改良して、その問題点を解決した粉体スラリ
ー塗料の製造法を提供することを目的とするものであ
る。
DISCLOSURE OF THE INVENTION The present invention relates to a powder slurry coating material which solves the problem by radically improving the conventional method when producing a powder coating material containing a resin and a curing agent as raw materials. It is an object of the present invention to provide a production method of

【0009】具体的には、 本発明は、樹脂等と硬化剤を分けて加熱溶融するた
め、熱安定性の問題を避けることができ、製造し易い。
そして樹脂等と硬化剤の各々の軟化点以上の温度に容易
に加熱、溶融できるので、超微粒子のスラリーとなり、
塗膜の外観が向上する。
Specifically, in the present invention, a resin or the like and a curing agent are separately heated and melted, so that the problem of thermal stability can be avoided and the production is easy.
And since it can be easily heated and melted to a temperature above the softening point of each of the resin and the curing agent, it becomes a slurry of ultrafine particles,
The appearance of the coating film is improved.

【0010】本発明は、乾式法におけるコストのかか
る粉砕工程が全く不要な球形の粉体スラリー塗料の製造
方法を提供する。 本発明は、10ミクロン以下の超微粒子の粉体塗料を
容易に製造可能で、簡易でかつ生産性の高い連続製造方
法を提供する。
The present invention provides a method for producing a spherical powder slurry paint which does not require a costly pulverizing step in a dry process. The present invention provides a simple and highly productive continuous production method capable of easily producing powder coating of ultrafine particles of 10 microns or less.

【0011】本発明は、粉体塗装ラインのような設備
が不要で、既存の水系塗装ラインであればほとんど手を
加えずに導入できる製造法を提供する。
The present invention provides a production method which does not require equipment such as a powder coating line and can be introduced with almost no modification in an existing water-based coating line.

【0012】[0012]

【課題を解決するための手段】本発明者らは、樹脂と硬
化剤とを主要原料として含む粉体塗料を製造する場合、
有機溶剤を全く使用しない乾式法のメリットと、湿式法
の球形で微粒子の粉体塗料のメリットの両方を併せ持つ
粉体塗料ができないかと鋭意試行検討を繰り返した結
果、樹脂等の原料と硬化剤とを分けてそれぞれ粉体スラ
リーを製造することにより上記課題が達成できることを
見出し、本発明を完成させるに至った。
Means for Solving the Problems The present inventors have proposed a method for producing a powder coating containing a resin and a curing agent as main raw materials.
As a result of intensive trials and examinations as to whether a powder coating having both the merits of the dry method using no organic solvent and the merits of the spherical, fine-grain powder coating of the wet method could be repeated, the raw materials such as resin and the curing agent were used. It has been found that the above-mentioned problems can be achieved by producing powder slurries separately for each of the above, and the present invention has been completed.

【0013】すなわち本発明は、粉体塗料用合成樹脂
と、必要に応じて光開始剤、着色顔料との混練物を加熱
熔融して成る樹脂熔融体(a)と、加熱し、必要に応じ
てさらに加圧することにより該合成樹脂の軟化点前後の
温度に加熱した水性媒体(b)とを混合し、該混合物の
温度を該合成樹脂の軟化点前後の温度に維持しながら、
前記樹脂熔融体(a)を水性媒体(b)中に機械的手段
により乳化分散させ、その後直ちに急速冷却することに
より得られる樹脂微粒子の水分散液(c)と、硬化剤を
加熱熔融して成る硬化剤熔融体(d)と、加熱し、必要
に応じてさらに加圧することにより該硬化剤の軟化点前
後の温度に加熱した水性媒体(e)とを混合し、該混合
物の温度を該硬化剤の軟化点前後の温度に維持しなが
ら、前記硬化剤熔融体(d)を水性媒体(e)中に機械
的手段により乳化分散させ、その後直ちに急速冷却する
ことにより得られる硬化剤微粒子の水分散液(f)とを
混合することを特徴とする粉体スラリー塗料の製造方法
を提供するものであり、好ましくは前記粉体塗料用合成
樹脂が、アクリル樹脂、エポキシ樹脂、ポリエステル樹
脂からなる群から選択される1種以上の樹脂からなる粉
体スラリー塗料の製造法であり、好ましくは乳化分散の
機械的手段として、スリットを有するリング状固定子と
スリットを有するリング状回転子とを、僅かな間隙を保
って、該固定子と該回転子が相互に咬み合うように同軸
上に設けた高速回転型連続式乳化分散機を使用し、好ま
しくは粉体塗料用合成樹脂と必要に応じて光開始剤、着
色顔料との混練物を加熱熔融して成る樹脂熔融体、又は
硬化剤を加熱熔融して成る硬化剤熔融体と、水性媒体と
の混合物を、前記高速回転型連続式乳化分散機に供給
し、該混合物を、前記回転子の高速回転により前記スリ
ットと前記間隙とを通して回転子の内心から遠心の方向
に流し、前記固定子のスリットと回転子のスリットを通
過する間にせん断力を与えるとともに、該混合物が該固
定子と該回転子との間の隙間を通過する間にズリ応力を
与えることによって、該樹脂熔融体を水性媒体中に乳化
分散し、一方同様な方法で硬化剤溶融体を水性媒体中に
乳化分散して、その両水分散液を混合する粉体スラリー
塗料の製造方法を提供する。
That is, the present invention provides a resin melt (a) obtained by heating and melting a kneaded product of a synthetic resin for powder coating and, if necessary, a photoinitiator and a coloring pigment, And further mixed with the aqueous medium (b) heated to a temperature around the softening point of the synthetic resin by further applying pressure, while maintaining the temperature of the mixture at a temperature around the softening point of the synthetic resin,
The resin melt (a) is emulsified and dispersed in an aqueous medium (b) by mechanical means, and then immediately cooled rapidly to obtain an aqueous dispersion (c) of resin fine particles and a curing agent, thereby heating and melting. And the aqueous medium (e) heated to a temperature around the softening point of the curing agent by heating and, if necessary, further pressurizing, and mixing the mixture with the aqueous medium (e). While maintaining the temperature around the softening point of the curing agent, the curing agent melt (d) is emulsified and dispersed in an aqueous medium (e) by mechanical means, and then immediately cooled rapidly to obtain the curing agent fine particles. It is intended to provide a method for producing a powder slurry coating, characterized by mixing with an aqueous dispersion (f), wherein the synthetic resin for powder coating preferably comprises an acrylic resin, an epoxy resin, or a polyester resin. Select from group A method for producing a powder slurry coating comprising at least one resin, wherein a ring-shaped stator having slits and a ring-shaped rotor having slits are preferably provided as a mechanical means for emulsification and dispersion. Using a high-speed rotation type continuous emulsifying and dispersing machine provided coaxially so that the stator and the rotor engage with each other, preferably with a synthetic resin for powder coating, and start light if necessary. A mixture of a resin melt obtained by heating and melting a kneaded material with a coloring pigment, or a curing agent melt obtained by heating and melting a curing agent, and an aqueous medium, into the high-speed rotation type continuous emulsifying and dispersing machine. The mixture is supplied, and the mixture is caused to flow in a centrifugal direction from the inner core of the rotor through the slit and the gap by the high-speed rotation of the rotor, and a shear force is generated while passing through the slit of the stator and the slit of the rotor. Give By applying shear stress while the mixture passes through the gap between the stator and the rotor, the resin melt is emulsified and dispersed in an aqueous medium, while the hardener melt is dispersed in an aqueous medium in the same manner. Disclosed is a method for producing a powder slurry paint which is emulsified and dispersed in a medium and then mixed with both aqueous dispersions.

【0014】[0014]

【発明の実施の態様】本発明は、溶剤を使わずに樹脂微
粒子を水性媒体中に分散させた水分散液と硬化剤微粒子
を水性媒体中に分散させた水分散液を製造し、この両水
分散液を混合することを特徴とする粉体スラリー塗料の
製造方法(水乳化分散法)であり、3つの工程を経るも
のである。第1工程及び第2工程は、樹脂等粒子の水分
散液の製造及び硬化剤粒子の水分散液の製造であり、第
3工程は両水分散液を混合する工程である。
DETAILED DESCRIPTION OF THE INVENTION The present invention produces an aqueous dispersion in which fine resin particles are dispersed in an aqueous medium without using a solvent and an aqueous dispersion in which fine particles of a curing agent are dispersed in an aqueous medium. This is a method for producing a powder slurry paint (water emulsification dispersion method), which comprises mixing an aqueous dispersion, and includes three steps. The first step and the second step are the production of an aqueous dispersion of particles of resin and the like and the production of an aqueous dispersion of hardener particles, and the third step is a step of mixing both aqueous dispersions.

【0015】まず本発明の第1工程について説明する。
すなわち第1工程は、粉体塗料用合成樹脂と、必要に応
じて光開始剤、着色顔料との混練物を加熱熔融して成る
樹脂熔融体(a)と、加熱し、必要に応じてさらに加圧
することにより該合成樹脂の軟化点前後の温度に加熱し
た水性媒体(b)とを混合し、該混合物の温度を該合成
樹脂の軟化点前後の温度に維持しながら、前記樹脂熔融
体(a)を水性媒体(b)中に機械的手段により乳化分
散させ、その後直ちに急速冷却することにより樹脂微粒
子の水分散液(c)を製造する工程である。
First, the first step of the present invention will be described.
That is, in the first step, a resin melt (a) obtained by heating and melting a kneaded product of a synthetic resin for powder coating material, and, if necessary, a photoinitiator and a coloring pigment, is heated, and further, if necessary. An aqueous medium (b) heated to a temperature around the softening point of the synthetic resin by pressurization is mixed, and while maintaining the temperature of the mixture at a temperature around the softening point of the synthetic resin, the resin melt ( This is a step of producing an aqueous dispersion (c) of fine resin particles by emulsifying and dispersing a) in an aqueous medium (b) by mechanical means and then immediately cooling the mixture.

【0016】この工程で用いる粉体塗料用合成樹脂は、
粉体塗料に適していれば、どのようなものであってもか
まわない。例えばアクリル樹脂、エポキシ樹脂、アミン
変性樹脂、フェノール樹脂、キシレン樹脂、ポリエステ
ル樹脂、尿素樹脂、ウレタン樹脂、ブロックイソシアネ
ート樹脂およびこれらの混合物等が挙げられる。これら
のうち、アクリル樹脂、ポリエステル樹脂、エポキシ樹
脂が好ましい。
The synthetic resin for powder coating used in this step is:
Any material may be used as long as it is suitable for a powder coating. For example, acrylic resins, epoxy resins, amine-modified resins, phenol resins, xylene resins, polyester resins, urea resins, urethane resins, blocked isocyanate resins, and mixtures thereof, and the like. Of these, acrylic resins, polyester resins, and epoxy resins are preferred.

【0017】光開始剤は、粉体塗料に適しているもので
あればどのようなものであってもかまわない。光開始剤
としては、例えばアセトフェノン、ベンゾフェノン、ミ
ヒラーケトン、ベンジル、ベンゾイン、ベンゾインイソ
ブチルエーテル、ベンジルジメチルケタール、1−ヒド
ロキシシクロヘキシルフェニルケトン、2−ヒドロキシ
−2−ジメチル−1−フェニルプロパン−1−オン、1
−(4−イソプロピルフェニル)−2−ヒドロキシ−2
−メチルプロパン−1−オン、アゾビスイソブチルニト
リル、ベンゾイルパーオキサイド、ジ−tert−ブチルパ
ーオキサイド等が挙げられる。上記ベンジルジメチルケ
タールの市販品としては、イルガキュア−651(チバ
ガイギー社製)が挙げられ、上記1−ヒドロキシシクロ
ヘキシルフェニルケトンの市販品としては、イルガキュ
ア−184(チバガイギー社製)が挙げられる。
The photoinitiator can be any one which is suitable for powder coatings. Examples of the photoinitiator include acetophenone, benzophenone, Michler's ketone, benzyl, benzoin, benzoin isobutyl ether, benzyldimethyl ketal, 1-hydroxycyclohexyl phenyl ketone, 2-hydroxy-2-dimethyl-1-phenylpropan-1-one,
-(4-isopropylphenyl) -2-hydroxy-2
-Methylpropan-1-one, azobisisobutylnitrile, benzoyl peroxide, di-tert-butyl peroxide and the like. The commercially available benzyldimethyl ketal includes Irgacure-651 (manufactured by Ciba-Geigy), and the commercially available 1-hydroxycyclohexylphenyl ketone includes Irgacure-184 (manufactured by Ciba-Geigy).

【0018】合成樹脂には、光開始剤の他、必要に応じ
て、着色顔料等を添加することができる。着色顔料とし
ては、有機顔料、無機顔料等が挙げられる。有機顔料と
しては、例えばアゾ系顔料、フタロシアニン系顔料、縮
合多環系顔料、ニトロソ系顔料等が挙げられ、無機顔料
としては、例えば酸化物系顔料、フタロシアニン化物、
クロム酸塩系顔料、炭素系顔料、マイカ系顔料、金属粉
末顔料等が挙げられる。これらの顔料は、顔料分散剤に
よって被覆されてもよい。
In addition to the photoinitiator, a coloring pigment or the like can be added to the synthetic resin, if necessary. Examples of the coloring pigment include an organic pigment and an inorganic pigment. Examples of the organic pigment include an azo pigment, a phthalocyanine pigment, a condensed polycyclic pigment, a nitroso pigment, and the like.Examples of the inorganic pigment include an oxide pigment, a phthalocyanine compound,
Chromate pigments, carbon pigments, mica pigments, metal powder pigments and the like can be mentioned. These pigments may be coated with a pigment dispersant.

【0019】その他、添加剤として、必要に応じて充填
剤、防錆剤、紫外線安定剤、紫外線吸収剤、流動調整
剤、ハジキ防止剤等が配合される。上記の原料を混練
し、加熱熔融し、樹脂熔融体を製造する。具体的には合
成樹脂、必要に応じて光開始剤、着色顔料、添加剤をミ
キサーでドライブレンドした後、攪拌機付きの加熱溶融
槽で完全に溶融させ、樹脂溶融体タンクに送られる。
In addition, as additives, fillers, rust inhibitors, ultraviolet stabilizers, ultraviolet absorbers, flow regulators, cissing inhibitors and the like are added as required. The above raw materials are kneaded and melted by heating to produce a resin melt. Specifically, a synthetic resin, and if necessary, a photoinitiator, a color pigment, and an additive are dry-blended by a mixer, then completely melted in a heating and melting tank equipped with a stirrer, and sent to a resin melt tank.

【0020】次に本発明の水性媒体について説明する。
一般に水性媒体は基本的には水であり、安定な樹脂溶融
体の水分散液をつくるために、必要により分散剤、界面
活性剤を添加してもよい。分散剤としては、例えば、ス
チレン等の懸濁重合で良く用いられているポリビニルア
ルコール、ヒドロキシエチルセルローズなどの水溶性高
分子分散安定剤、あるいは燐酸カルシウムなど難水溶性
の無機系分散安定剤等が挙げられ、これらの中から適当
なものを使用すればよい。また界面活性剤としては、例
えば2,6,8ートリメチルー4ーノニルオキシポリエ
チレンオキシエタノール等が挙げられる。
Next, the aqueous medium of the present invention will be described.
Generally, the aqueous medium is basically water, and if necessary, a dispersant and a surfactant may be added in order to form a stable aqueous dispersion of the resin melt. As the dispersant, for example, polyvinyl alcohol, which is often used in suspension polymerization of styrene, a water-soluble polymer dispersion stabilizer such as hydroxyethyl cellulose, or a poorly water-soluble inorganic dispersion stabilizer such as calcium phosphate, etc. Any of these may be used. Examples of the surfactant include 2,6,8-trimethyl-4-nonyloxypolyethyleneoxyethanol and the like.

【0021】合成樹脂に対する水性媒体の比率は水系乳
化分散液を作るのに充分な量である必要がある。本発明
の無溶剤水乳化分散法においては、前記の合成樹脂熔融
体と水性媒体とを樹脂の軟化点前後の温度に加熱してお
くことを特徴とする。軟化点前後の温度は、特に限定さ
れないが、合成樹脂を熔融状態に維持するために軟化点
±30℃以内の温度が好ましい。
The ratio of the aqueous medium to the synthetic resin must be an amount sufficient to produce an aqueous emulsion dispersion. The solvent-free water emulsification dispersion method of the present invention is characterized in that the synthetic resin melt and the aqueous medium are heated to a temperature around the softening point of the resin. The temperature around the softening point is not particularly limited, but is preferably a temperature within ± 30 ° C. of the softening point in order to maintain the synthetic resin in a molten state.

【0022】上記の水性媒体は、加熱し、必要により加
圧した高温の水性媒体である。加熱用熱交換器等の使用
により、粉体塗料用合成樹脂を熔融させるために合成樹
脂の軟化点前後の温度まで加熱される。このため、水性
媒体は、使用する合成樹脂の軟化点によって、工程中に
設けられた1Kg/cm2〜20Kg/cm2程度の加圧
手段によって圧力をかけ、適性温度に調整される。特に
合成樹脂の軟化点が低い場合は必ずしも加圧手段を用い
る必要はないが、軟化点が100℃以上の場合には、水
性媒体が沸騰しないように加圧する必要がある。
The above-mentioned aqueous medium is a high-temperature aqueous medium which is heated and optionally pressurized. By using a heat exchanger for heating or the like, the synthetic resin for powder coating is heated to a temperature around the softening point of the synthetic resin in order to melt it. Therefore, the aqueous medium, the softening point of the synthetic resin used, pressured by 1Kg / cm 2 ~20Kg / cm 2 of about pressurizing means provided in the process, is adjusted to proper temperature. In particular, when the softening point of the synthetic resin is low, it is not always necessary to use a pressurizing means. However, when the softening point is 100 ° C. or higher, it is necessary to pressurize the aqueous medium so as not to boil.

【0023】次に上記の工程で得られる樹脂熔融体と高
温水性媒体との混合直後に、樹脂溶融体を水性媒体に機
械的に乳化分散させる。樹脂熔融体を水性媒体に機械的
に乳化分散させるための装置としては、スリットを有す
るリング状固定子とスリットを有するリング状回転子と
を、僅かな間隙を保って、該固定子と該回転子が相互に
咬み合うように同軸上に設けた構造を有する高速回転型
連続式乳化分散機を用いるのが好ましい。
Next, immediately after mixing the resin melt obtained in the above step with the high-temperature aqueous medium, the resin melt is mechanically emulsified and dispersed in the aqueous medium. As an apparatus for mechanically emulsifying and dispersing a resin melt in an aqueous medium, a ring-shaped stator having a slit and a ring-shaped rotor having a slit are maintained with a slight gap, and the stator and the rotor are rotated. It is preferable to use a high-speed rotation type continuous emulsifying and dispersing machine having a structure provided coaxially so that the daughters bite each other.

【0024】この本発明の高速回転型連続式乳化分散機
は、樹脂熔融体と高温高圧の水性媒体とを連続的に圧入
して、合成樹脂の軟化点前後の温度で、合成樹脂の分解
温度以下の高温高圧下で急速に均一混合して乳化分散
し、連続的に排出できる構造の装置である。
The high-speed rotation type continuous emulsifying and dispersing machine of the present invention continuously injects a resin melt and a high-temperature and high-pressure aqueous medium, and at a temperature around the softening point of the synthetic resin, the decomposition temperature of the synthetic resin. It is a device with a structure that can be rapidly and uniformly mixed, emulsified and dispersed under the following high temperature and high pressure, and continuously discharged.

【0025】高速回転型連続式乳化分散機は、前記回転
子を高速回転させることによって合成樹脂熔融体を水性
媒体中に乳化分散することができる。この乳化分散機の
温度は、合成樹脂を一定の熔融状態に保持するため、加
熱する必要があり、このため乳化分散機には保温のため
のジャケットを設置することが好ましい。合成樹脂の最
適温度は、目的とする粒子の粒子径、樹脂の分子量など
によって異なるが、80℃〜220℃に設定するのが好
ましい。
The high-speed rotation type continuous emulsifying and dispersing machine can emulsify and disperse a synthetic resin melt in an aqueous medium by rotating the rotor at a high speed. It is necessary to heat the temperature of the emulsifying and dispersing machine in order to maintain the synthetic resin in a constant molten state. Therefore, it is preferable that the emulsifying and dispersing machine be provided with a jacket for keeping the temperature. The optimum temperature of the synthetic resin varies depending on the particle diameter of the target particles, the molecular weight of the resin, and the like, but is preferably set to 80 ° C to 220 ° C.

【0026】高速回転型連続式乳化分散機内の温度は、
供給する樹脂熔融体の温度、供給する水性媒体の温度、
ジャケットの保温効果と機内でのせん断力による発熱量
のバランスで、一定温度に制御される。
The temperature in the high-speed rotation type continuous emulsifying and dispersing machine is as follows:
Temperature of the resin melt to be supplied, temperature of the aqueous medium to be supplied,
The temperature is controlled to be constant by the balance between the heat retention effect of the jacket and the amount of heat generated by the shearing force inside the machine.

【0027】また高速回転型連続式乳化分散機内の圧力
は、水性媒体の機内温度における蒸気圧と回転子のポン
プ機能による吐出圧で決まる。通常、樹脂微粒子の水分
散液を冷却した後に自動圧力制御弁を設け、内部圧を一
定に保ち、該水分散液を大気圧下に連続的に取り出す方
法が好ましい。
The pressure in the high-speed rotary type continuous emulsifying and dispersing machine is determined by the vapor pressure of the aqueous medium at the machine temperature and the discharge pressure by the pump function of the rotor. Usually, it is preferable to provide an automatic pressure control valve after cooling the aqueous dispersion of resin fine particles, keep the internal pressure constant, and continuously take out the aqueous dispersion under atmospheric pressure.

【0028】高速回転型連続式乳化分散機内では、樹脂
熔融体と、高温水性媒体との混合物を、高速回転型連続
式乳化分散機に供給し、該混合物を、前記回転子の高速
回転により前記スリットと前記間隙とを通して回転子の
内心から遠心の方向に流し、前記固定子のスリットと回
転子のスリットを通過する間にせん断力を与えるととも
に、該混合物が該固定子と該回転子との間の隙間を通過
する間にズリ応力を与えることによって、微分散がなさ
れる。この固定子及び回転子のスリットはノズルでも、
同様な効果を奏することができるので、固定子、回転子
の両方、又はいずれか一方のスリットをノズルに変える
こともできる。
In the high-speed rotation type continuous emulsifying and dispersing machine, a mixture of a resin melt and a high-temperature aqueous medium is supplied to a high-speed rotation type continuous emulsifying and dispersing machine, and the mixture is rotated by the high-speed rotation of the rotor. It flows in a centrifugal direction from the inner core of the rotor through the slit and the gap, and applies a shearing force while passing through the slit of the stator and the slit of the rotor, and the mixture is formed between the stator and the rotor. By applying shear stress while passing through the gap between them, fine dispersion is achieved. The stator and rotor slits are nozzles,
Since a similar effect can be obtained, both the stator and the rotor, or one of the slits can be changed to a nozzle.

【0029】以下図面により本発明の機械的微分散に好
ましく用いられる高速回転型連続式乳化分散機について
説明する。高速回転型乳化分散機の固定子1は、同一中
心で固着され、その中心が原料入口と連通する液入口2
となって開口している。固定子1の円形面には、固定子
と同心円でリング状の突起3が1段又は2段以上の多段
状に突設されている。突起同士の間隙には、円周溝4が
形成されており、それぞれの突起に複数のスリット5が
形成されている。これらのスリットの幅は、0.6mm
〜3.0mmであり、スリットは各リング状突起に12
〜72本付いていて櫛の歯状となっている。このスリッ
トの幅は、供給された液の粒子径を小さくするため、外
周の突起ほど小さくなるのが好ましい。
The high-speed rotation type continuous emulsifying and dispersing machine preferably used for mechanical fine dispersion of the present invention will be described below with reference to the drawings. The stator 1 of the high-speed rotation type emulsifying and dispersing machine is fixed at the same center, and the center thereof is connected to the liquid inlet 2 communicating with the raw material inlet.
It is open. On the circular surface of the stator 1, ring-shaped projections 3 which are concentric with the stator and are provided in multiple stages of one stage or two or more stages. A circumferential groove 4 is formed in the gap between the projections, and a plurality of slits 5 are formed in each projection. The width of these slits is 0.6 mm
~ 3.0 mm, and the slit is 12
There are up to 72 comb-shaped teeth. The width of the slit is preferably smaller toward the outer periphery of the projection in order to reduce the particle diameter of the supplied liquid.

【0030】高速回転型連続式乳化分散機内の他方の内
壁の中心には駆動軸6が付設され、駆動部に接続され
て、高速回転される。高速回転型連続式乳化分散機の回
転子7は、この駆動部の先端に、固定子と平行にかつ同
一中心軸上に固定されている。固定子に対向する回転子
の対向面には、回転子と同心円で円環状の1段又は2段
以上の多段状突起8が突設されている。それぞれの回転
突起は固定子と同様に、突起同士の間隙には円周溝9が
形成され、それぞれの突起には複数のスリット10が形
成されている。
A driving shaft 6 is provided at the center of the other inner wall in the high-speed rotating type continuous emulsifying and dispersing machine, and is connected to a driving unit to rotate at high speed. The rotor 7 of the high-speed rotation type continuous emulsifying and dispersing machine is fixed to the tip of the driving unit in parallel with the stator and on the same central axis. On the opposing surface of the rotor facing the stator, there are provided one or two or more multistage projections 8 which are concentric with the rotor and annular. As in the case of the stator, each rotating projection has a circumferential groove 9 formed in the gap between the projections, and a plurality of slits 10 formed in each projection.

【0031】この固定子1と回転子7とは、固定子の突
起3及び円周溝4、回転子の突起8及び円周溝10が僅
かな間隙を維持しつつ挿入状態で咬み合わされた状態で
使用に供される。
The stator 1 and the rotor 7 are engaged with each other while the protrusion 3 and the circumferential groove 4 of the stator, the protrusion 8 and the circumferential groove 10 of the rotor are inserted while maintaining a small gap. Served for use.

【0032】本発明で用いる高速回転型連続式乳化分散
機は、この咬み合わせによって形成された間隙に樹脂溶
融体と高温高圧水性媒体との混合物が供給され、該混合
物が回転子の内心から遠心方向へ流れ、前記回転子の高
速回転によってせん断力を受け、及び該混合物が該固定
子と該回転子との間の隙間を通過する間にズリ応力を受
けることによって樹脂熔融体が水性媒体中に乳化分散す
るものである。
In the high-speed rotation type continuous emulsifying and dispersing machine used in the present invention, a mixture of the resin melt and the high-temperature and high-pressure aqueous medium is supplied to the gap formed by the engagement, and the mixture is centrifuged from the inner core of the rotor. Flows in the direction, undergoes shearing force due to the high speed rotation of the rotor, and undergoes shear stress while the mixture passes through the gap between the stator and the rotor, thereby causing the resin melt to move in the aqueous medium. Is emulsified and dispersed.

【0033】この高速回転型連続式乳化分散機の主液入
口2に供給された樹脂溶融体と高温高圧水性媒体は、回
転子7が高速回転すると、最内側の回転子の突起のスリ
ットに入り、遠心力により該回転子の突起の外周から吐
出され、最内側の固定子の突起に押しつけられ、その固
定子の突起のスリットに入る。このスリットに入った混
合液は、遠心力により最内側の回転子のスリットに入っ
た混合物に押されて第2回転子の円周溝に押し出され
る。このとき該混合物は、最内側の固定子の突起と第2
回転子の突起によってせん断力を加えられるとともに、
固定子と回転子との間隔を通過するに伴って、ズリ応力
が加えられる。混合液が合流するとさらにせん断力が加
えられ、後の混合液に押されて第2固定子の突起のスリ
ットに入り、前記と同様のことを繰り返して受けなが
ら、混合物が順次遠心方向に移動され、乳化分散が完了
される。
When the rotor 7 rotates at a high speed, the resin melt and the high-temperature and high-pressure aqueous medium supplied to the main liquid inlet 2 of the high-speed rotary type continuous emulsifying and dispersing machine enter slits of protrusions of the innermost rotor. Is discharged from the outer circumference of the rotor projection by centrifugal force, pressed against the innermost stator projection, and enters the slit of the stator projection. The liquid mixture entering this slit is pushed by the mixture entering the slit of the innermost rotor by centrifugal force and is pushed out into the circumferential groove of the second rotor. At this time, the mixture is formed by the protrusion of the innermost stator and the second
Shear force can be applied by the rotor projections,
Shear stress is applied along the passage between the stator and the rotor. When the mixed liquids join together, further shearing force is applied, and the mixture is pushed by the subsequent mixed liquid and enters the slits of the projections of the second stator, and the mixture is sequentially moved in the centrifugal direction while repeatedly receiving the same as described above. The emulsification and dispersion are completed.

【0034】この混合物の流れと、せん断力及びズリ応
力の関係については、図4に示されるとおりである。高
速回転型連続式乳化分散機の回転子の回転数は駆動軸に
接続された駆動モーターで制御される。回転数が大きく
周速が大きいほど大きいせん断力を受けて、合成樹脂の
粒子径が小さくなる。直径10cmの回転子を使用し
て、好ましい回転数は3,000〜10,000rpmで
ある。
The relationship between the flow of the mixture and the shearing force and shear stress is as shown in FIG. The rotation speed of the rotor of the high-speed continuous emulsifying and dispersing machine is controlled by a drive motor connected to a drive shaft. The larger the rotation speed and the higher the peripheral speed, the greater the shearing force, and the smaller the particle size of the synthetic resin. Using a 10 cm diameter rotor, the preferred speed is 3,000-10,000 rpm.

【0035】本発明の高速回転型連続式乳化分散機とし
て市販されている装置の例としては、キャビトロン(株
式会社ユーロテック)を挙げることができる。次いで上
記高速回転型連続式乳化分散機の出口から得られた樹脂
微粒子の水分散液を、生成した樹脂粒子同士が衝突して
凝集物が発生しない間に、出来るだけ速やかに合成樹脂
のガラス転移温度以下の温度まで急速に冷却する。
An example of an apparatus commercially available as the high-speed rotation type continuous emulsifying and dispersing machine of the present invention is Cavitron (Eurotech Co., Ltd.). Next, the aqueous dispersion of the resin fine particles obtained from the outlet of the high-speed rotation type continuous emulsifying and dispersing machine is mixed with the glass transition of the synthetic resin as quickly as possible while the generated resin particles do not collide with each other and generate aggregates. Cools rapidly to a temperature below the temperature.

【0036】急速に冷却する装置としては、市販されて
いる熱交換器を用いることができ、冷却水と熱交換させ
ながら冷却する。冷却速度は特に限定しないが、凝集物
が発生しないようにするためには、10℃/秒以上であ
ることが好ましい。
As a device for rapidly cooling, a commercially available heat exchanger can be used, and cooling is performed while exchanging heat with cooling water. The cooling rate is not particularly limited, but is preferably 10 ° C./sec or more in order to prevent generation of aggregates.

【0037】合成樹脂のガラス転移温度付近まで急速に
冷却した後は、圧力制御弁により圧力を大気圧にまで戻
すことにより、樹脂微粒子のスラリ−として得られる。
次に本発明の第2工程について説明する。
After the synthetic resin is rapidly cooled to around the glass transition temperature, the pressure is returned to atmospheric pressure by a pressure control valve to obtain a slurry of fine resin particles.
Next, the second step of the present invention will be described.

【0038】すなわち第2工程は、硬化剤を加熱熔融し
て成る硬化剤熔融体(d)と、加熱し、必要に応じてさ
らに加圧することにより該硬化剤の軟化点前後の温度に
加熱した水性媒体(e)とを混合し、該混合物の温度を
該硬化剤の軟化点前後の温度に維持しながら、前記硬化
剤熔融体(d)を水性媒体(e)中に機械的手段により
乳化分散させ、その後直ちに急速冷却することにより硬
化剤微粒子の水分散液(f)を得る工程である。
That is, in the second step, the curing agent melt (d) obtained by heating and melting the curing agent was heated, and further heated, if necessary, to a temperature around the softening point of the curing agent. An aqueous medium (e) is mixed and the hardener melt (d) is emulsified in the aqueous medium (e) by mechanical means while maintaining the temperature of the mixture at a temperature around the softening point of the hardener. This is a step of obtaining an aqueous dispersion (f) of fine particles of the curing agent by dispersing and immediately cooling the dispersion immediately.

【0039】この工程で用いる硬化剤は、粉体塗料に適
してしればどのようなものであってもかまわない。第1
工程で用いる粉体塗料用合成樹脂と反応するような官能
基を有する必要があり、合成樹脂の種類によって相違す
る。硬化剤としては、例えばポリカルボン酸(ドデカン
二酸、トリメリット酸等)、アミノ樹脂やブロックポリ
イソシアネート、ポリエポキシド、ポリオール等が挙げ
られる。
The curing agent used in this step may be any one as long as it is suitable for a powder coating. First
It is necessary to have a functional group that reacts with the synthetic resin for powder coating used in the process, and it differs depending on the type of the synthetic resin. Examples of the curing agent include polycarboxylic acids (such as dodecane diacid and trimellitic acid), amino resins, block polyisocyanates, polyepoxides, and polyols.

【0040】硬化剤を熔融して硬化剤熔融体を製造する
方法は、上記の樹脂熔融体を製造する第1工程と同様で
ある。また水性媒体、機械的手段による乳化分散の方
法、急速冷却の方法は上記の第1工程と同様である。
The method for producing a hardener melt by fusing the hardener is the same as in the first step of producing the above resin melt. The aqueous medium, the method of emulsification and dispersion by mechanical means, and the method of rapid cooling are the same as those in the first step.

【0041】次に本発明の第3工程について説明する。
すなわち樹脂微粒子の水分散液と硬化剤微粒子の水分散
液とを決められた比率で混合し、必要に応じて粘度調整
剤を入れる工程である。
Next, the third step of the present invention will be described.
That is, this is a step of mixing the aqueous dispersion of the resin fine particles and the aqueous dispersion of the hardener fine particles at a predetermined ratio, and adding a viscosity modifier as necessary.

【0042】樹脂微粒子の水分散液と硬化剤微粒子の水
分散液との混合比率は、特に限定されず、合成樹脂の種
類によって異なる。粘度調整剤としては、例えばアクリ
ル樹脂等が挙げられ、具体的製品としては、プライマル
ASEー60(日本アクリル化学製)が挙げられる。
The mixing ratio of the aqueous dispersion of the resin fine particles and the aqueous dispersion of the hardener fine particles is not particularly limited, and differs depending on the type of the synthetic resin. Examples of the viscosity modifier include an acrylic resin and the like, and specific products include Primal ASE-60 (manufactured by Nippon Acrylic Chemicals).

【0043】以上の第1工程から第3工程までのフロー
の1例を図5により説明する。すなわち上記の方法で製
造された樹脂熔融体を入れたタンク12からポンプ13
を介して高速回転型連続式乳化分散機11に樹脂熔融体
を供給すると同時に、水性媒体を入れた水性媒体タンク
14から加熱用熱交換器15を通して高温水性媒体を
得、この高温水性媒体をポンプ16を介して高速回転型
連続式乳化分散機11に供給する。樹脂熔融体と高温水
性媒体はこの乳化分散機11内で乳化分散され、樹脂熔
融体水分散液が得られる。この水分散液を直ちに冷却用
熱交換器17に通し冷却し、圧力調整弁18を経て樹脂
スラリータンク19に送られる。この樹脂のフロー全工
程の圧力を圧力調整弁18で調整する。
An example of the flow from the first step to the third step will be described with reference to FIG. That is, the pump 13 is moved from the tank 12 containing the resin melt produced by the above method.
At the same time, the resin melt is supplied to the high-speed rotation type continuous emulsifying and dispersing machine 11 through the, and a high-temperature aqueous medium is obtained from the aqueous medium tank 14 containing the aqueous medium through the heat exchanger 15 for heating. The mixture is supplied to the high-speed rotation type continuous emulsifying and dispersing machine 11 through the line 16. The resin melt and the high-temperature aqueous medium are emulsified and dispersed in the emulsifier / disperser 11 to obtain a resin melt aqueous dispersion. This aqueous dispersion is immediately cooled by passing through a cooling heat exchanger 17, and sent to a resin slurry tank 19 via a pressure adjusting valve 18. The pressure in all steps of the resin flow is adjusted by the pressure adjusting valve 18.

【0044】同様に上記の方法で製造された硬化剤熔融
体を入れたタンク22からポンプ23を介して高速回転
型連続式乳化分散機21に硬化剤熔融体を供給すると同
時に、水性媒体を入れた水性媒体タンク24から加熱用
熱交換器25を通して高温水性媒体を得、この高温水性
媒体をポンプ26を介して高速回転型連続式乳化分散機
21に供給する。硬化剤熔融体と高温水性媒体はこの乳
化分散機21内で乳化分散され、硬化剤熔融体水分散液
が得られる。この水分散液を直ちに冷却用熱交換器27
に通し冷却し、圧力調整弁28を経て硬化剤スラリータ
ンク29に送られる。この硬化剤のフロー全工程の圧力
を圧力調整弁28で調整する。
Similarly, the hardener melt is supplied from a tank 22 containing the hardener melt produced by the above-described method to a high-speed rotary type continuous emulsifying and dispersing machine 21 via a pump 23, and at the same time, an aqueous medium is charged. A high-temperature aqueous medium is obtained from a heated aqueous medium tank 24 through a heating heat exchanger 25, and the high-temperature aqueous medium is supplied to a high-speed rotation type continuous emulsifying and dispersing machine 21 via a pump 26. The hardener melt and the high-temperature aqueous medium are emulsified and dispersed in the emulsifier / disperser 21 to obtain a hardener melt aqueous dispersion. The aqueous dispersion is immediately cooled by a heat exchanger 27 for cooling.
And is sent to a hardener slurry tank 29 via a pressure adjusting valve 28. The pressure of the entire flow of the curing agent is adjusted by the pressure adjusting valve 28.

【0045】本発明の粉体スラリー塗料の製造方法は、
樹脂溶融体と高温水性媒体から、高速回転型連続式乳化
分散機を経て冷却までの一連の工程と硬化剤溶融体と高
温水性媒体から、高速回転型連続式乳化分散機を経て冷
却までの一連の工程とを連続で行うことができるもので
ある。もちろん急速冷却までを連続プロセスにし、合成
樹脂スラリ及び硬化剤スラリーを得た後は、各々のスラ
リータンク19、29から樹脂スラリーポンプ20、硬
化剤スラリーポンプ30を経て、粉体スラリータンク3
1で混合され、必要に応じて粘度調整剤を添加してもよ
い。
The method for producing a powder slurry paint of the present invention comprises:
A series of steps from a resin melt and a high-temperature aqueous medium to cooling through a high-speed rotary type continuous emulsifying and dispersing machine, and a series of steps from a curing agent melt and a high-temperature aqueous medium to cooling through a high-speed rotary type continuous emulsifying and dispersing machine And can be performed continuously. Of course, the process up to rapid cooling is a continuous process, and after obtaining the synthetic resin slurry and the curing agent slurry, the powder slurry tank 3 is passed from each of the slurry tanks 19 and 29 through the resin slurry pump 20 and the curing agent slurry pump 30.
1 and a viscosity modifier may be added as necessary.

【0046】本発明は、上記のとおり樹脂及び硬化剤熔
融体と高温高圧水性媒体との混合物を高速回転型乳化分
散機で高せん断力、ズリ応力及び高周波レベルの圧力変
動を発生させ、強力な攪拌・破砕作用を利用して無溶剤
乳化分散を行うものである。
According to the present invention, as described above, a mixture of a resin and a curing agent melt and a high-temperature and high-pressure aqueous medium is subjected to high shear force, shear stress and high-frequency pressure fluctuation by a high-speed rotary emulsifying and dispersing machine. Solvent-free emulsification and dispersion are performed by utilizing the stirring and crushing actions.

【0047】生成する樹脂微粒子及び硬化剤微粒子の平
均粒子径の支配因子は、乳化分散機の回転子の回転速
度、合成樹脂、硬化剤および水性媒体の温度である。
これらの支配因子はすべてその数値を大きくしてやると
合成樹脂及び硬化剤の水分散性がアップし、合成樹脂微
粒子及び硬化剤微粒子の粒子径は小さくなる。
The controlling factors of the average particle size of the resin fine particles and the hardener fine particles to be formed are the rotation speed of the rotor of the emulsifying and dispersing machine and the temperatures of the synthetic resin, the hardener and the aqueous medium.
When the values of all these controlling factors are increased, the water dispersibility of the synthetic resin and the curing agent is increased, and the particle diameter of the synthetic resin fine particles and the curing agent fine particles is reduced.

【0048】[0048]

【実施例】以下本発明の実施例を示すが、本発明はこれ
らの実施例によって制限されるものではない。また実施
例中の部、%はすべて重量基準によるものとする。
EXAMPLES Examples of the present invention will be described below, but the present invention is not limited to these examples. All parts and percentages in the examples are on a weight basis.

【0049】実施例1 合成樹脂等の微粒子のスラリーの製造 ファインデックA−207S(アクリル樹脂:大日本イ
ンキ化学工業製)を99.4部、アクロナール4F(流
動調節剤:BASF社製)を0.6部をミキサーで予備
混合し、攪拌機付加熱溶融槽で完全に溶融した後に、図
5の12の樹脂溶融体タンクにホールドする。13のポ
ンプで、200℃に加熱しながら、キャビトロンCD1
010に毎分100gの速度で送り込んだ。図5の水性
媒体タンクのイオン交換水(PVA0.1%含有)を、
熱交換器で180℃に加熱しながら毎分1リットルの速
度でキャビトロンに送り込んだ。回転子の回転速度は8
000rpm、圧力は10Kg/cm2で運転し、製造
したスラリーは180℃から65℃まで15秒以内に冷
却して取り出し、平均粒径2ミクロン、最大粒径10ミ
クロン以下のほぼ球形の樹脂微粒子のスラリーを得た。
Example 1 Production of slurry of fine particles of synthetic resin and the like 99.4 parts of Finedec A-207S (acrylic resin: manufactured by Dainippon Ink and Chemicals) and 0 of Acronal 4F (flow control agent: manufactured by BASF) were used. .6 parts were premixed with a mixer, completely melted in a heat melting tank with a stirrer, and then held in the resin melt tank of FIG. Cavitron CD1 while heating to 200 ° C. with a pump of No. 13.
010 was fed at a rate of 100 g / min. The ion exchange water (containing 0.1% of PVA) in the aqueous medium tank of FIG.
While heating to 180 ° C. with a heat exchanger, the mixture was fed into the Cavitron at a rate of 1 liter per minute. Rotor speed is 8
000 rpm, pressure was operated at 10 Kg / cm 2, slurry prepared is taken out and cooled within 15 seconds to 65 ° C. from 180 ° C., an average particle diameter of 2 microns, a maximum particle size of 10 microns or less in substantially spherical resin particles A slurry was obtained.

【0050】硬化剤の微粒子のスラリーの製造 ドデカン二酸(硬化剤)100部をミキサーで予備混合
し、攪拌機付加熱溶融槽で完全に溶融した後に、図5の
22の硬化剤溶融タンクにホールドする。23の硬化剤
ポンプで、140℃に加熱しながら、キャビトロンCD
1010に毎分100gの速度で送り込んだ。図5の2
4の水性媒体タンクのイオン交換水(PVA0.1%含
有)を、熱交換器で110℃に加熱しながら毎分1リッ
トルの速度でキャビトロンに送り込んだ。回転子の回転
速度は8000rpm、圧力は2Kg/cm2で運転
し、製造したスラリーは110℃から65℃まで10秒
以内に冷却して取り出し、平均粒径2ミクロン、最大粒
径10ミクロン以下のほぼ球形の硬化剤微粒子のスラリ
ーを得た。
Preparation of Slurry of Hardener Fine Particles 100 parts of dodecane diacid (hardener) are premixed with a mixer, completely melted in a heat melting tank with a stirrer, and then held in a hardener melting tank 22 in FIG. I do. Cavitron CD while heating to 140 ° C with a 23 hardener pump
The 1010 was fed at a rate of 100 g / min. 5 of FIG.
The ion-exchanged water (containing 0.1% of PVA) in the aqueous medium tank of No. 4 was fed into the Cavitron at a rate of 1 liter per minute while heating to 110 ° C. with a heat exchanger. The rotating speed of the rotor is 8000 rpm, the pressure is 2 kg / cm 2 , and the produced slurry is cooled and taken out from 110 ° C. to 65 ° C. within 10 seconds, and has an average particle diameter of 2 μm and a maximum particle diameter of 10 μm or less. A slurry of substantially spherical hardener particles was obtained.

【0051】合成樹脂等スラリーと硬化剤スラリーの
混合 合成樹脂等スラリーと硬化剤スラリーを84:16の比
率で混合し、このスラリーにプライマル ASE−60
(粘度調整剤:日本アクリル化学製)を1wt%(Solid
換算)入れて、平均粒径2ミクロン、最大粒径10ミク
ロン以下のほぼ球形の粉体スラリー塗料を得た。このス
ラリー塗料を冷間圧延鋼のパネルに厚さ約1ミルにスプ
レー塗装をした。このパネルを100℃で15分間前焼
き付けした後、150℃で20分間焼き付けたところ、
透明で硬く、平滑性のある塗膜を得た。
Mixing of Slurry of Synthetic Resin etc. and Slurry of Hardening Agent Slurry of synthetic resin etc. and hardening agent slurry are mixed at a ratio of 84:16, and this slurry is mixed with Primal ASE-60.
1% by weight (viscosity modifier: Nippon Acrylic Chemicals)
In addition, a substantially spherical powder slurry paint having an average particle size of 2 microns and a maximum particle size of 10 microns or less was obtained. The slurry paint was spray painted on cold rolled steel panels to a thickness of about 1 mil. This panel was pre-baked at 100 ° C. for 15 minutes and then baked at 150 ° C. for 20 minutes.
A transparent, hard and smooth coating film was obtained.

【0052】[0052]

【発明の効果】本発明によれば、樹脂と硬化剤とを別々
に加熱熔融するため、粉体スラリー塗料を塗布して得ら
れる塗膜の外観が良好である。また有機溶剤を使わず
に、極めて容易かつ生産性が高い連続製法で小粒径の硬
化性の粉体スラリー塗料が製造でき、従来の粉砕手段で
は粉体化できなかったような樹脂でも経済的に粉体化で
きる。
According to the present invention, since the resin and the curing agent are separately heated and melted, the appearance of the coating film obtained by applying the powder slurry coating is good. In addition, it is possible to produce a curable powder slurry coating with a small particle size by an extremely easy and highly productive continuous process without using an organic solvent.Economical even for resins that could not be powdered by conventional pulverization means Can be powdered.

【図面の簡単な説明】[Brief description of the drawings]

【図1】本発明に用いる回転型連続式乳化分散機の固定
子及び回転子の斜視図である。
FIG. 1 is a perspective view of a stator and a rotor of a rotary continuous emulsifying and dispersing machine used in the present invention.

【図2】本発明に用いる回転型連続式乳化分散機の要部
断面を表した図である。
FIG. 2 is a diagram showing a cross section of a main part of a rotary continuous emulsifying and dispersing machine used in the present invention.

【図3】図2のA−A'部を側面から見たときの固定子
突起と回転子突起の組み合わせ状態を表した図である。
FIG. 3 is a diagram showing a combination state of a stator protrusion and a rotor protrusion when the AA ′ part of FIG. 2 is viewed from a side surface.

【図4】本発明に用いる回転型連続式乳化分散機の回転
子の回転より固定子と回転子の間を流れる流体にかかる
力を表した図である。
FIG. 4 is a diagram showing a force applied to a fluid flowing between a stator and a rotor due to rotation of the rotor of the rotary continuous emulsifying and dispersing machine used in the present invention.

【図5】本発明にかかる粉体スラリー塗料の製造方法の
説明図である。
FIG. 5 is an explanatory diagram of a method for producing a powder slurry paint according to the present invention.

【符号の説明】[Explanation of symbols]

1 固定子 2 液入口 3 固定子の突起 4 固定子の円周溝 5 突起のスリット 6 駆動軸 7 回転子 8 回転子の突起 9 回転子の円周溝 10 突起のスリット 11 回転型連続式微分散機 12 樹脂熔融体タンク 13 樹脂ポンプ 14 水性媒体タンク 15 加熱用熱交換器 16 水性媒体ポンプ 17 冷却用熱交換器 18 圧力制御弁 19 樹脂スラリータンク 20 樹脂スラリーポンプ 21 回転型連続式微分散機 22 硬化剤溶融体タンク 23 硬化剤ポンプ 24 水性媒体タンク 25 加熱用熱交換器 26 水性媒体ポンプ 27 冷却用熱交換器 28 圧力制御弁 29 硬化剤スラリータンク 30 硬化剤スラリーポンプ 31 粉体スラリー塗料タンク DESCRIPTION OF SYMBOLS 1 Stator 2 Liquid inlet 3 Stator protrusion 4 Stator circumferential groove 5 Protrusion slit 6 Drive shaft 7 Rotor 8 Rotor protrusion 9 Rotor circumferential groove 10 Protrusion slit 11 Rotary continuous fine dispersion Machine 12 Resin melt tank 13 Resin pump 14 Aqueous medium tank 15 Heat exchanger for heating 16 Aqueous medium pump 17 Heat exchanger for cooling 18 Pressure control valve 19 Resin slurry tank 20 Resin slurry pump 21 Rotary continuous fine disperser 22 Curing Agent melt tank 23 hardener pump 24 aqueous medium tank 25 heating heat exchanger 26 aqueous medium pump 27 cooling heat exchanger 28 pressure control valve 29 hardener slurry tank 30 hardener slurry pump 31 powder slurry paint tank

フロントページの続き (72)発明者 小越 昇 千葉県袖ヶ浦市長浦駅前4−16−15Continued on front page (72) Inventor Noboru Kogoshi 4-16-15, Nagaura Station, Sodegaura City, Chiba Prefecture

Claims (5)

【特許請求の範囲】[Claims] 【請求項1】(1)粉体塗料用合成樹脂と、必要に応じ
て光開始剤、着色顔料との混練物を加熱熔融して成る樹
脂熔融体(a)と、加熱し、必要に応じてさらに加圧す
ることにより該合成樹脂の軟化点前後の温度に加熱した
水性媒体(b)とを混合し、該混合物の温度を該合成樹
脂の軟化点前後の温度に維持しながら、前記樹脂熔融体
(a)を水性媒体(b)中に機械的手段により乳化分散
させ、その後直ちに急速冷却することにより得られる樹
脂微粒子の水分散液(c)と、(2)硬化剤を加熱熔融
して成る硬化剤熔融体(d)と、加熱し、必要に応じて
さらに加圧することにより該硬化剤の軟化点前後の温度
に加熱した水性媒体(e)とを混合し、該混合物の温度
を該硬化剤の軟化点前後の温度に維持しながら、前記硬
化剤熔融体(d)を水性媒体(e)中に機械的手段によ
り乳化分散させ、その後直ちに急速冷却することにより
得られる硬化剤微粒子の水分散液(f)とを(3)混合
することを特徴とする粉体スラリー塗料の製造方法。
(1) A resin melt (a) obtained by heating and melting a kneaded product of a synthetic resin for powder coating and, if necessary, a photoinitiator and a coloring pigment; The mixture is further mixed with the aqueous medium (b) heated to a temperature around the softening point of the synthetic resin by further applying pressure, and the mixture is melted while maintaining the temperature of the mixture at a temperature around the softening point of the synthetic resin. The body (a) is emulsified and dispersed in an aqueous medium (b) by mechanical means and then immediately cooled to obtain an aqueous dispersion (c) of resin fine particles, and (2) a curing agent, which is heated and melted. And the aqueous medium (e) heated to a temperature around the softening point of the curing agent by heating and, if necessary, further pressurizing, and mixing the mixture with the aqueous medium (e). While maintaining the temperature around the softening point of the hardener, the hardener melt (d) A powder slurry paint characterized by mixing (3) an aqueous dispersion (f) of hardener fine particles obtained by emulsifying and dispersing in an aqueous medium (e) by mechanical means and then rapidly cooling the mixture. Manufacturing method.
【請求項2】樹脂微粒子の水分散液(c)と硬化剤微粒
子の水分散液(f)とを混合後、粘度調整剤を添加する
請求項1記載の製造方法。
2. The production method according to claim 1, wherein a viscosity modifier is added after mixing the aqueous dispersion of resin fine particles (c) and the aqueous dispersion of hardener fine particles (f).
【請求項3】前記粉体塗料用合成樹脂が、アクリル樹
脂、エポキシ樹脂、ポリエステル樹脂からなる群から選
択される1種以上の樹脂を含む請求項1又は2記載の製
造方法。
3. The method according to claim 1, wherein the synthetic resin for powder coating contains at least one resin selected from the group consisting of an acrylic resin, an epoxy resin, and a polyester resin.
【請求項4】乳化分散の機械的手段として、スリットを
有するリング状固定子とスリットを有するリング状回転
子とを、僅かな間隙を保って、該固定子と該回転子が相
互に咬み合うように同軸上に設けた高速回転型連続式乳
化分散機を使用する請求項1〜3のいずれか1項記載の
製造方法。
4. As a mechanical means for emulsification and dispersion, a ring-shaped stator having a slit and a ring-shaped rotor having a slit are interposed between the stator and the rotor while maintaining a small gap. The method according to any one of claims 1 to 3, wherein a high-speed rotation type continuous emulsifying and dispersing machine provided coaxially is used.
【請求項5】粉体塗料用合成樹脂と必要に応じて光開始
剤、着色顔料との混練物を加熱熔融して成る樹脂熔融
体、又は硬化剤を加熱熔融して成る硬化剤熔融体と、水
性媒体との混合物を、前記高速回転型連続式乳化分散機
に供給し、該混合物を、前記回転子の高速回転により前
記スリットと前記間隙とを通して回転子の内心から遠心
の方向に流し、前記固定子のスリットと回転子のスリッ
トを通過する間にせん断力を与えるとともに、該混合物
が該固定子と該回転子との間の隙間を通過する間にズリ
応力を与えることによって、該樹脂熔融体を水性媒体中
に乳化分散し、一方同様な方法で硬化剤溶融体を水性媒
体中に乳化分散して、その両分散液を混合する請求項4
記載の製造方法。
5. A resin melt obtained by heating and melting a kneaded product of a synthetic resin for a powder coating material and, if necessary, a photoinitiator and a coloring pigment, or a curing agent melt obtained by heating and melting a curing agent. A mixture with an aqueous medium is supplied to the high-speed rotation type continuous emulsifying and dispersing machine, and the mixture is caused to flow in a centrifugal direction from the inner core of the rotor through the slit and the gap by the high-speed rotation of the rotor, By applying a shearing force while passing through the slit of the stator and the slit of the rotor, and applying a shear stress while the mixture passes through a gap between the stator and the rotor, the resin 5. A method according to claim 4, wherein the melt is emulsified and dispersed in an aqueous medium, and the hardener melt is emulsified and dispersed in an aqueous medium in the same manner, and the two dispersions are mixed.
The manufacturing method as described.
JP25046297A 1997-09-16 1997-09-16 Preparation of powder slurry coating Pending JPH1180602A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP25046297A JPH1180602A (en) 1997-09-16 1997-09-16 Preparation of powder slurry coating

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP25046297A JPH1180602A (en) 1997-09-16 1997-09-16 Preparation of powder slurry coating

Publications (1)

Publication Number Publication Date
JPH1180602A true JPH1180602A (en) 1999-03-26

Family

ID=17208239

Family Applications (1)

Application Number Title Priority Date Filing Date
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Country Status (1)

Country Link
JP (1) JPH1180602A (en)

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US6512024B1 (en) 1999-05-20 2003-01-28 Dow Global Technologies Inc. Continuous process of extruding and mechanically dispersing a polymeric resin in an aqueous or non-aqueous medium
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6512024B1 (en) 1999-05-20 2003-01-28 Dow Global Technologies Inc. Continuous process of extruding and mechanically dispersing a polymeric resin in an aqueous or non-aqueous medium
WO2001004230A1 (en) * 1999-07-12 2001-01-18 Sumitomo Seika Chemicals Co., Ltd. Process for producing adhesive for fusion bonding, adhesive for fusion bonding obtained by the process, and adhesive fabric containing the adhesive for fusion bonding
JP2001019937A (en) * 1999-07-12 2001-01-23 Sumitomo Seika Chem Co Ltd Hot-melt adhesive agent and adhesive cloth
US6743741B1 (en) 1999-07-12 2004-06-01 Sumitomo Seika Chemicals Co., Ltd. Process for producing adhesive for fusion bonding, adhesive for fusion bonding obtained by the process, and adhesive fabric containing the adhesive for fusion bonding
JP2002256077A (en) * 2001-02-28 2002-09-11 Dainippon Ink & Chem Inc Production method for dispersion for thermoplastic resin grains
JP2008069247A (en) * 2006-09-13 2008-03-27 Toyota Motor Corp Aqueous disperse slurry coating, method for producing the same, and coating film
JP2014237083A (en) * 2013-06-07 2014-12-18 アシザワ・ファインテック株式会社 High speed rotation type disperser
CN112717795A (en) * 2020-12-07 2021-04-30 深圳市尚水智能设备有限公司 Pulping equipment for preparing high-solid-content slurry and slurry mixing system

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