JP4292090B2 - Method for measuring pH of electrodeposition paint - Google Patents
Method for measuring pH of electrodeposition paint Download PDFInfo
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本発明は、電着塗料のｐＨを連続的に測定できる 電着塗料のｐＨを測定する方法に関する。 The present invention relates to a method for measuring the pH of an electrodeposition paint capable of continuously measuring the pH of the electrodeposition paint.
従来から電着塗料は、自動車ボディや部品などの下塗り塗料として用いられ、多くの塗装ラインにて用いられている。このような塗装ラインは、電着槽に電着塗料を満たし、被塗物をコンベアなどで搬送して電圧を印加して電着塗装を行った後、焼き付け乾燥することによって塗膜を得る自動化塗装が行われており、自動車ボディは連続的に塗装されて塗料が持ち出され、一定の塗装台数をカウントすると新たに塗料が補給され一定の塗料特性を保っている。 Conventionally, electrodeposition paints are used as undercoat paints for automobile bodies and parts, and are used in many painting lines. Such a coating line is an automation that fills an electrodeposition tank with an electrodeposition paint, conveys the object to be coated on a conveyor, etc., applies a voltage, performs electrodeposition coating, and then baked and dried to obtain a coating film. The car body is painted continuously, paint is taken out, and when a certain number of paints are counted, new paint is replenished and certain paint properties are maintained.
従来、電着塗料特性（例えば、ｐＨ、電導度、固形分、顔料分、酸濃度）を測定するためには、電着塗料槽から電着塗料をサンプリングし、その塗料を実験室に持ち帰って電着塗料特性を求めていた。しかしこれらのデータが揃うまでには、１時間〜３日間を要していた。その間にも塗装ラインが変化し続ける為、ライン対応が遅れることから仕上り性の異常が発生することがあった。 Conventionally, electrodeposition paint properties (eg, pH, conductivity, solid content, pigment content, acid concentration) are measured by sampling the electrodeposition paint tank from the electrodeposition paint tank and bringing the paint back to the laboratory. We were looking for electrodeposition paint properties. However, it took 1 hour to 3 days to gather these data. In the meantime, the painting line continued to change, and the line response was delayed, which sometimes resulted in abnormal finishing.
この電着塗料特性の中でもｐＨの測定は、例えば、ＨＭ−３０Ｇ、ＷＭ−５０ＥＧ（東亜ディーケーケー社製、商品名、ｐＨメーター）、又はＢ−２１１（ＨＯＲＩＢＡ社製、商品名、ｐＨメーター）のｐＨメーターのガラス電極と参照電極（比較電極ともいう）を浸漬し、測定後、参照電極とガラス電極に付着した電着塗料を洗浄し、次の測定に用いていた。 Among these electrodeposition paint properties, the measurement of pH is, for example, HM-30G, WM-50EG (trade name, pH meter, manufactured by Toa DKK Corporation), or B-211 (trade name, pH meter, manufactured by HORIBA). A glass electrode of a pH meter and a reference electrode (also referred to as a comparative electrode) were immersed, and after the measurement, the electrodeposition paint adhered to the reference electrode and the glass electrode was washed and used for the next measurement.
この作業の繰り返しによって、参照電極やガラス電極に電着塗料が付着したり（特に、参照電極におけるＫＣｌ水溶液が染み出すピンホールに付着し、ピンホールを塞ぐことがあった）、測定値にも誤差を生じることがあった。また参照電極やガラス電極の洗浄や管理にも手間のかかるものであった。 By repeating this operation, the electrodeposition paint adheres to the reference electrode and the glass electrode (particularly, the KCl aqueous solution on the reference electrode sticks to the pinhole where the KCl aqueous solution oozes out and closes the pinhole). An error may occur. In addition, it takes time and effort to clean and manage the reference electrode and the glass electrode.
従来の発明に、点在する塗装設備を遠隔地から管理できる塗装設備システムを開発した［特許文献１］。 In the conventional invention, a coating equipment system capable of managing scattered coating equipment from a remote location has been developed [Patent Document 1].
そのためｐＨセンサーを塗装ラインに設置し、インラインで適時にｐＨを把握できる装置が求められていた。
発明が解決しようとする課題は、塗装ラインに設置しても参照電極やガラス電極に電着塗料が付着しづらく、長期間に渡ってｐＨの測定が可能なｐＨ測定方法を見出すこと。 The problem to be solved by the present invention is to find a pH measurement method capable of measuring pH over a long period of time because it is difficult for electrodeposition paint to adhere to a reference electrode or a glass electrode even if it is installed in a painting line.
上記の課題を解決するために本発明者等は鋭意検討した結果、電着塗料を循環するための配管と、参照電極とガラス電極とを一体化した複合電極を有するｐＨセンサー（Ａ）を具備するｐＨ測定装置によって、電着塗料のｐＨを適時に測定することを見出し、発明を完成するに至った。 In order to solve the above-mentioned problems, the present inventors have intensively studied, and as a result, have a pH sensor (A) having a composite electrode in which a pipe for circulating an electrodeposition paint and a reference electrode and a glass electrode are integrated. The inventors have found that the pH of the electrodeposition paint can be measured in a timely manner by the pH measuring device, and have completed the invention.
即ち、本発明は、
１．電着槽と共に循環路を形成する配管内を、流速０．０１〜０．７ｍ／秒で電着塗料を移動せしめること、
照電極とガラス電極とを一体化した複合電極を有するｐＨセンサーを、該配管内に配置して、該ｐＨセンサーに電着塗料を接触せしめて、電着塗料のｐＨを測定すること
を含むことを特徴とする電着塗料のｐＨを測定する方法、
２．該ｐＨセンサーの該ガラス電極の電極面が、配管内における電着塗料の移動方向に平行に、設置してある１項に記載の方法、
３．該ｐＨセンサーの該参照電極の面積が０．１〜３ｃｍ２の範囲である１又は２項に記載の方法、
４．該ｐＨセンサーの該ガラス電極の面積が０．５〜７ｃｍ２の範囲で、かつ平面である１〜３のいずれか１項に記載の方法、
５．該配管の管径が、１０〜１００ｍｍφである１〜４のいずれか１項に記載の方法、
６．電着塗料を、塗料が摺れる摺動部分がないポンプによって移動せしめることを含む請求項１〜５のいずれか１項に記載の方法、
に関する。
That is, the present invention
1. Moving the electrodeposition paint at a flow rate of 0.01 to 0.7 m / sec in a pipe forming a circulation path with the electrodeposition tank;
Disposing a pH sensor having a composite electrode in which a reference electrode and a glass electrode are integrated in the pipe, bringing the electrodeposition paint into contact with the pH sensor, and measuring the pH of the electrodeposition paint A method of measuring the pH of an electrodeposition paint characterized by
2. The method according to 1, wherein the electrode surface of the glass electrode of the pH sensor is installed in parallel with the moving direction of the electrodeposition paint in the pipe,
3. The method according to 1 or 2, wherein the area of the reference electrode of the pH sensor is in the range of 0.1 to 3 cm 2 ,
4). The method according to any one of 1 to 3, wherein the area of the glass electrode of the pH sensor is in the range of 0.5 to 7 cm 2 and is flat.
5. The method according to any one of 1 to 4, wherein the pipe has a pipe diameter of 10 to 100 mmφ,
6). The method according to any one of claims 1 to 5, comprising moving the electrodeposition paint by a pump having no sliding portion on which the paint slides.
About.
本発明のｐＨを測定する方法は、複合電極を有するｐＨセンサーで、塗装ラインに設置してインラインでの測定が可能である。従来のｐＨメーターは、センサー部分の電極に塗料が付着してメンテナンスがかかる。また、塗装ラインから塗料をサンプリングして実験室で電着特性を測定するのに膨大な時間と手間を要していた。 The method for measuring pH of the present invention is a pH sensor having a composite electrode, which can be installed in a painting line and measured in-line. Conventional pH meters require maintenance because the paint adheres to the electrodes of the sensor portion. In addition, it takes a lot of time and labor to sample the paint from the painting line and measure the electrodeposition characteristics in the laboratory.
それに対し、本発明のｐＨ測定装置を用いた電着特性評価方法は、遠隔地の塗装ラインにｐＨ測定装置を設置した場合でも洗浄やセンサー交換などのメンテナンスに手間がかからず、インターネットを介したデータの送受信によって浴管理が可能となった。 On the other hand, the electrodeposition characteristic evaluation method using the pH measuring device of the present invention does not require time and effort for maintenance such as cleaning and sensor replacement even when the pH measuring device is installed in a remote painting line. The bath management became possible by sending and receiving data.
適時にｐＨの変化を把握できることから（例えば、警告表示と組み合わせて）、被塗物に析出した塗膜が有機酸で再溶解したり、ＧＡ材の塗装時におけるピンホールの発生などを抑制することにつながる。 Since the change in pH can be grasped in a timely manner (for example, in combination with a warning display), the coating film deposited on the object to be coated is re-dissolved with an organic acid and the occurrence of pinholes during the coating of GA materials is suppressed. It leads to things.
本発明のｐＨを測定する方法を実施する装置は、参照電極とガラス電極とを一体化した複合電極を有するｐＨセンサー（図１の１）と、電着塗料を循環するための配管（図１の３）とを具備し、電着槽（図１の４）の電着塗料を配管内を循環させて、ｐＨを適時に測定するｐＨ測定装置である。モデル図としては、図１で示される。 An apparatus for carrying out the method for measuring pH of the present invention includes a pH sensor (1 in FIG. 1) having a composite electrode in which a reference electrode and a glass electrode are integrated, and a pipe for circulating an electrodeposition paint (FIG. 1). 3), and the electrodeposition paint (4 in FIG. 1) is circulated in the pipe to measure the pH in a timely manner. The model diagram is shown in FIG.
ｐＨセンサー（図１の１）の詳細について、図２に示す。ｐＨセンサー（図２の１）は、参照電極（図２の９）とガラス電極（図２の１０）が一体型の複合電極で、配管内における電着塗料の移動方向に平行に設けられた電極面を設置する。このことによって電極面が、電着塗料の循環による洗浄効果から長期間にわたって塗装ラインに設置しても連続した使用が可能である。 Details of the pH sensor (1 in FIG. 1) are shown in FIG. The pH sensor (1 in FIG. 2) is a composite electrode in which a reference electrode (9 in FIG. 2) and a glass electrode (10 in FIG. 2) are integrated, and is provided in parallel with the moving direction of the electrodeposition paint in the pipe. Install the electrode surface. As a result, the electrode surface can be continuously used even if it is installed in the coating line for a long period of time due to the cleaning effect by circulation of the electrodeposition paint.
ｐＨセンサー（図２の１）における参照電極（図２の９）の面積としては、０．１ｃｍ２〜３ｃｍ２、好ましくは２ｃｍ２〜３ｃｍ２の範囲、ガラス電極の面積としては、０．５〜７ｃｍ２、好ましくは６ｃｍ２〜７ｃｍ２の範囲であることが、電着塗料が電極に付着せずに、かつ精度の高いｐＨを得るのに好ましい。参照電極及びガラス電極は、円形の薄い板状である。 The area of the reference electrode (9 in FIG. 2) in the pH sensor (1 in FIG. 2) is 0.1 cm 2 to 3 cm 2 , preferably in the range of 2 cm 2 to 3 cm 2 , and the area of the glass electrode is 0.5 ～7Cm 2, preferably in the range of 6cm 2 ~7cm 2, without adhering electrodeposition paint to the electrode, and preferably to obtain a pH higher accuracy. The reference electrode and the glass electrode have a thin circular plate shape.
参照電極は、比較電極とも呼ばれ、ガラス電極との間で発生する電位を標準水素電極の電位に換算する作用を有する。 The reference electrode is also called a comparison electrode, and has an effect of converting a potential generated between the reference electrode and the glass electrode into a potential of a standard hydrogen electrode.
上記のｐＨセンサーの市販品としては、センサー８７１Ａ（Ｆｏｘｂｏｒｏ Ｃｏｍｐａｎｙ製、商品名、ｐＨセンサー）が挙げられる。 Examples of commercially available pH sensors include sensor 871A (manufactured by Foxboro Company, trade name, pH sensor).
次に、ｐＨセンサー（図２の１）から得られたｐＨのデータは、ケーブル（図１及び図２の１）を通じてパソコン等に取り込むことができ、インターネットを介して測定データを遠隔地に配信することも可能である。 Next, the pH data obtained from the pH sensor (1 in FIG. 2) can be taken into a personal computer or the like through a cable (1 in FIGS. 1 and 2), and the measurement data is distributed to a remote location via the Internet. It is also possible to do.
電着塗料を循環するための配管（図１の３）の管径は、１０ｍｍφ〜１００ｍｍφ、好ましくは２０ｍｍφ〜８０ｍｍφの範囲が、電着塗料を沈降せずに、かつ一定の流速を得るためにも好ましい。配管内の電着塗料の流速は、電着塗料が配管内で塗料が沈降することなく、かつｐＨセンサーに塗料が凝集して付着しないことが必要で、流速としては０．０１ｍ／秒〜０．７ｍ／秒、好ましくは０．１ｍ／秒〜０．５ｍ／秒で、電着塗料槽（図１の４）から配管を通じて電着塗料（図１の５）を配管内に循環させ、ｐＨを測定する。配管内の流速は、０．０１ｍ／秒であると電着塗料が沈降し易く、流速が０．７ｍ／秒を超えるとｐＨセンサーの測定値が安定しなくなり、測定誤差が生じ易くなる。 The pipe diameter for circulating the electrodeposition paint (3 in FIG. 1) is in the range of 10 mmφ to 100 mmφ, preferably 20 mmφ to 80 mmφ in order to obtain a constant flow rate without sinking the electrodeposition paint. Is also preferable. The flow rate of the electrodeposition paint in the pipe must be such that the electrodeposition paint does not settle in the pipe and the paint does not aggregate and adhere to the pH sensor, and the flow rate is 0.01 m / second to 0. The electrodeposition paint (5 in FIG. 1) is circulated in the pipe from the electrodeposition paint tank (4 in FIG. 1) through the pipe at a pH of 0.7 m / sec, preferably 0.1 m / sec to 0.5 m / sec, and pH Measure. When the flow velocity in the pipe is 0.01 m / sec, the electrodeposition paint tends to settle, and when the flow velocity exceeds 0.7 m / sec, the measured value of the pH sensor becomes unstable and a measurement error tends to occur.
電着塗料は、配管内を塗料が擦れる摺動部分がないポンプによって一定の流速で移動せしめされるのが好ましい。この塗料が擦れる摺動部分がないポンプは、インペラが磁気によって浮上し、電着塗料を循環するために、ポンプを回転した時に、ポンプ内に擦れる部分がないポンプであり、市販品としては、レヒドロポンプ（イワキ社製、商品名）が挙げられる。 The electrodeposition paint is preferably moved at a constant flow rate by a pump having no sliding portion where the paint rubs in the pipe. This pump with no sliding part where the paint rubs is a pump that does not rub within the pump when the pump is rotated in order to circulate the electrodeposition paint because the impeller floats by magnetism. A rehydro pump (product name) manufactured by Iwaki Co., Ltd. may be mentioned.
このｐＨ測定装置は、配管内を一定の流速にて電着塗料を循環し、適時にｐＨを求めることができる。従来のｐＨ測定装置は、電極部分が塗料で汚れるため塗装ラインでの連続測定には、メンテナンスに手間のかかるものであったが、本発明によりこれらを解消することができた。 This pH measuring device can circulate the electrodeposition paint at a constant flow rate in the pipe and obtain the pH in a timely manner. In the conventional pH measuring apparatus, since the electrode portion is contaminated with the paint, continuous measurement in the painting line is troublesome for maintenance. However, these problems can be solved by the present invention.
例えば、昨日の電着塗料のｐＨが６．６であったが、電着塗料に有機酸を添加したので、本日はｐＨが６．３であるとか、急にｐＨが５．６まで低下しているので隔膜電極やＵＦ設備の見直しが必要、との判断が適時で行えるようになった。 For example, the pH of the electrodeposition paint yesterday was 6.6, but since an organic acid was added to the electrodeposition paint, the pH is 6.3 today, or the pH suddenly drops to 5.6. As a result, it is now possible to make a timely judgment that the diaphragm electrode and UF equipment need to be reviewed.
また、急な生産量の増加により有機酸が電着槽内の電着塗料中に蓄積し、膜厚が低下するトラブルも、管理幅内でのｐＨの低下を事前に検出し、隔膜の流量を上げるなどの事前処置を行い、ライントラブルを未然に防止することができる。その他被塗装物による隔膜の破損などの事故もリアルタイムに検出し、大きなライントラブルになる前に対策を打つことができる。 In addition, troubles that organic acids accumulate in the electrodeposition paint in the electrodeposition tank due to a sudden increase in production volume and the film thickness decreases can also be detected in advance by detecting a decrease in pH within the control range. It is possible to prevent line troubles by taking pre-treatment such as raising Other accidents such as membrane damage due to the object to be painted can also be detected in real time, and measures can be taken before a major line trouble occurs.
次に本発明に適用できる電着塗料としては、従来から既知の電着塗料を用いることができ、カチオン電着塗料でもアニオン電着塗料のいずれでもかまわないが防錆性の面からカチオン電着塗料が主流となってきており、カチオン電着塗料について説明する。 Next, as the electrodeposition paint applicable to the present invention, a conventionally known electrodeposition paint can be used, and either a cationic electrodeposition paint or an anion electrodeposition paint may be used. Paints have become mainstream, and cationic electrodeposition paints will be described.
カチオン電着塗料は、基体樹脂として、例えば、アミン付加型エポキシ樹脂やアミン付加型アクリル樹脂を用い、例えば、硬化剤としてのブロック化ポリイソシアネート、表面調整剤、触媒、界面活性剤、有機溶剤、有機酸を加えて水分散してなるエマルションと、着色顔料、体質顔料、触媒を分散樹脂とともに顔料分散してなる顔料ペーストを加え、脱イオン水で希釈して製造されたものを例示できる。 The cationic electrodeposition paint uses, for example, an amine addition type epoxy resin or an amine addition type acrylic resin as a base resin, for example, a blocked polyisocyanate as a curing agent, a surface conditioner, a catalyst, a surfactant, an organic solvent, An emulsion prepared by adding an organic acid and dispersing in water and a pigment paste obtained by dispersing a pigment, a extender pigment, and a catalyst together with a dispersion resin, and diluting with deionized water can be exemplified.
このようなカチオン電着塗料の固形分としては、０．１〜４０重量％、好ましくは５〜３０重量％、さらに好ましくは１５〜２５重量、ｐＨは５．０〜７．５、好ましくは５．５〜７．０範囲が適している。本発明における測定に必要な電着塗料の量としては、１０ｍｌ〜３００ｍ３の間で任意に調整することができる。このことから塗装ラインサイドや塗装ラインに隣接した管理室等においても測定できる。 The solid content of such a cationic electrodeposition coating is 0.1 to 40% by weight, preferably 5 to 30% by weight, more preferably 15 to 25% by weight, and pH is 5.0 to 7.5, preferably 5 A range of .5 to 7.0 is suitable. The amount of electrodeposition paint required for the measurement in the present invention can be arbitrarily adjusted between 10 ml and 300 m 3 . Therefore, it can be measured in the control room adjacent to the painting line side or the painting line.
以下、実施例を挙げて本発明をさらに詳細に説明する。本発明はこれによって限定されるものではない。尚、「部」及び「％」は「重量部」及び「重量％」を示す。 Hereinafter, the present invention will be described in more detail with reference to examples. The present invention is not limited thereby. “Parts” and “%” indicate “parts by weight” and “% by weight”.
実施例１
塗装ラインＡにおいて、センサー８７１Ａ（Ｆｏｘｂｏｒｏ Ｃｏｍｐａｎｙ製、商品名、複合電極を有するインライン型ｐＨセンサー）、及び配管（管径５０ｍｍφ）を図１のように結線し、電着塗料を流速０．３ｍ／秒で流し、ｐＨ値を自動的に計測した。その時のｐＨ値＝６．３であった。
Example 1
In the painting line A, the sensor 871A (manufactured by Foxboro Company, product name, in-line pH sensor having a composite electrode) and pipe (tube diameter 50 mmφ) are connected as shown in FIG. The pH value was automatically measured. The pH value at that time was 6.3.
実施例２
塗装ラインＢにおいて、センサー８７３Ａ（Ｆｏｘｂｏｒｏ Ｃｏｍｐａｎｙ製、商品名、複合電極を有するインライン型ｐＨセンサー）、及びレヒドロポンプ（イワキ社製、商品名、塗料が擦れる摺動部分がないポンプ）を図１の（６）のように設置し、配管（管径５０ｍｍφ）を図１のように結線し、電着塗料を流速０．５ｍ／秒で流した。１日３回のｐＨの測定を行い、１回目のｐＨ値＝６．４、２回目のｐＨ値＝６．５、３回目のｐＨ値＝６．５を自動的に計測し、インターネットを介して遠隔地の塗料管理者側へ配信した。
Example 2
In the painting line B, a sensor 873A (manufactured by Foxboro Company, product name, in-line pH sensor having a composite electrode) and a rehydro pump (manufactured by Iwaki Co., Ltd., product name, pump having no sliding part where the paint rubs) are shown in FIG. 6), pipes (tube diameter 50 mmφ) were connected as shown in FIG. 1, and the electrodeposition paint was allowed to flow at a flow rate of 0.5 m / sec. The pH is measured three times a day, the first pH value = 6.4, the second pH value = 6.5, and the third pH value = 6.5 are automatically measured, via the Internet. Distributed to the remote paint manager.
比較例１
実施例１と同様の塗装ラインＡの電着塗料をサンプリングし、ＨＭ−３０Ｇ（東亜ディーケーケー社製、商品名、ｐＨ測定装置）を用いて、ｐＨ値＝６．３を測定した。サンプリング、及び測定に要した時間は、１０分間であった。
Comparative Example 1
The electrodeposition paint of the same coating line A as in Example 1 was sampled, and the pH value = 6.3 was measured using HM-30G (trade name, pH measuring device manufactured by Toa DKK Corporation). The time required for sampling and measurement was 10 minutes.
比較例２
実施例２と同様の塗装ラインＢの電着塗料をサンプリングし、ＨＭ−３０Ｇ（東亜ディーケーケー社製、商品名、ｐＨ測定装置）を用いた。１日３回のｐＨの測定を行い、１回目のｐＨ値＝６．４を得た後、次に電極を洗浄して測定して２回目の測定値ｐＨ値＝６．５を得た。また電極を洗浄して測定して３回目の測定値ｐＨ値＝６．５を得た。サンプリング、及び測定に要した時間は、トータル３０分間であった。
Comparative Example 2
An electrodeposition paint on the same coating line B as in Example 2 was sampled, and HM-30G (trade name, pH measuring device manufactured by Toa DKK Corporation) was used. The pH was measured three times a day to obtain a first pH value = 6.4, then the electrode was washed and measured to obtain a second measured value pH value = 6.5. The electrode was washed and measured to obtain the third measured value pH value = 6.5. The time required for sampling and measurement was 30 minutes in total.
実施例、比較例の結果を表１に示す。 The results of Examples and Comparative Examples are shown in Table 1.
本発明は、電着塗料の浴管理において、ｐＨを適時に算出できる。そのため電着塗料の変化に対しての対応や対策を早急に図れ、品質に優れる塗装物品を供給できる。 In the present invention, the pH can be calculated in a timely manner in the bath management of the electrodeposition paint. Therefore, it is possible to promptly take measures and countermeasures against changes in the electrodeposition paint, and to supply coated articles with excellent quality.
１．ｐＨセンサー
２．ケーブル
３．配管
４．電着槽
５．電着塗料
６．配管
１０．参照電極
１１．ガラス電極
1. 1. pH sensor Cable 3. Piping 4. 4. Electrodeposition tank Electrodeposition paint6. Piping 10. Reference electrode 11. Glass electrode
Claims (6)
参照電極とガラス電極とを一体化した複合電極を有するｐＨセンサーを、該配管内に配置して、該ｐＨセンサーに電着塗料を接触せしめて、電着塗料のｐＨを測定すること
を含むことを特徴とする電着塗料のｐＨを測定する方法。 Moving the electrodeposition paint at a flow rate of 0.01 to 0.7 m / sec in a pipe forming a circulation path with the electrodeposition tank;
Disposing a pH sensor having a composite electrode in which a reference electrode and a glass electrode are integrated in the pipe, bringing the electrodeposition paint into contact with the pH sensor, and measuring the pH of the electrodeposition paint A method for measuring the pH of an electrodeposition paint characterized by the above.
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| JP2004033658A JP4292090B2 (en) | 2004-02-10 | 2004-02-10 | Method for measuring pH of electrodeposition paint |
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| JP2004033658A JP4292090B2 (en) | 2004-02-10 | 2004-02-10 | Method for measuring pH of electrodeposition paint |
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