JP5224168B2 - Concentrated magnetic powder dispersion for wet magnetic particle testing - Google Patents
Concentrated magnetic powder dispersion for wet magnetic particle testing Download PDFInfo
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- 229910002012 Aerosil® Inorganic materials 0.000 description 1
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Description
本発明は、自動車メーカーの製造ラインにおけるシャフトなどの鋼製部品や鋼材メーカーの鋼材製造ラインにおけるビレットなどの鋼材の表面欠陥部探傷に汎用されている湿式磁粉探傷試験の実施に当たって使用される検査液の調製に用いられる湿式磁粉探傷試験用濃厚磁粉分散液に関するものである。 Checking the present invention, when used in the practice of wet magnetic powder Sagukizu試test which is generally in the surface defect inspection of steel materials such as billets in steel parts or steel manufacturers steel production line, such as a shaft in a motor vehicle manufacturer manufacturing line it relates concentrated magnetic particle dispersion for wet magnetic particle Sagukizu試test used in the preparation of the liquid.
周知のとおり、前記湿式磁粉探傷試験は、JIS-Z-2320に規格化されており、当該試験は、磁化されている検査物（例えば、前記シャフトなどの鋼製部品：磁性体や前記ビレットなどの鋼材：磁性体）に市販の湿式磁粉探傷試験用磁粉（四三酸化鉄粒子や純鉄粒子などの導磁性粒子に酢酸セルローズ系合成樹脂やビニルブチラール系合成樹脂などの合成樹脂バインダーを用いてルモゲンイエロー50790：商品名：BASF社製やフエスタA：商品名：Swada社製などの蛍光顔料を付着させてなるメジアン径３〜70μm：体積基準分布表示−以下、同じ−で真比重２〜５g／cm3の粉末；以下「磁粉」という）を水に分散させて調製した検査液を接触させ、当該検査物の表面欠陥部（検査物の表面乃至表面近傍に存在する微細なワレやピンホール）に当該検査液に分散している当該磁粉を集合せしめて磁粉模様を形成させ、当該磁粉模様によって表面欠陥部を探傷するもの（以下、この試験を「湿式磁粉探傷試験」という）であり、当該検査液の調製に当たっては、前出JIS規格に『…水を分散媒とする場合には，検出媒体の中には界面活性剤及び防せい（錆）剤も含むものとする。…』とされているとおり、界面活性剤が使用されている。 As is well known, the wet magnetic particle Sagukizu試test is standardized in JIS-Z-2320, the test, the test product are magnetized (e.g., steel parts such as the shaft: magnetic and the Magnetic powder for wet magnetic particle flaw detection test (steel material such as billet: magnetic material) (synthetic resin binders such as cellulose acetate synthetic resin and vinyl butyral synthetic resin) Use Lummogen Yellow 50790: Product name: BASF or Festa A: Product name: Median diameter formed by attaching fluorescent pigment such as Swada, etc. 3-70 μm: Volume standard distribution display-the same below-true specific gravity 2-5 g / cm 3 powder; hereinafter referred to as “magnetic powder”) is contacted with a test solution prepared by dispersing in water, and the surface defect portion of the test object (the fine crack present on or near the surface of the test object) Or pinhole) in the test solution To form a magnetic powder pattern the magnetic powder and has allowed the set, which flaw detection surface defects portion by the magnetic powder pattern (hereinafter, the test referred to as "wet magnetic particle inspection"), and when the preparation of the test solution is According to the above-mentioned JIS standard, “... When water is used as a dispersion medium, the detection medium shall also contain a surfactant and an antirust (rust) agent. As indicated by “...”, a surfactant is used.
なお、磁粉の製造法には、当業者間において「粉砕法」と呼ばれているものと「噴霧法」と呼ばれているものがあり、前者は、最も早く提案されて現在に到るも実用されているものであって、この製造法は、有機溶媒可溶性合成樹脂をバインダーとし、これを揮発性有機溶剤に溶解した溶液中に蛍光顔料を分散させて置き、これに導磁性粒子粉末を混合して練合せてペースト状物とし、当該ペースト状物を乾燥して塊状物とした後、当該塊状物をボールミルなどの粉砕機を用いて微粒子状にまで粉砕した後、篩などによって分級して所要粒径の磁粉を得る方法（以下、この製造法を「粉砕法」という）であり、後者は、特許文献１に開示されているように、この製造法は、水分散性合成樹脂又は水溶性合成樹脂をバインダーとし、当該樹脂と蛍光顔料と導磁性粒子粉末とを水に加え攪拌してスラリー状物とした後、当該スラリー状物をスプレーノズル又は遠心ディスクを用いて空気中に噴霧又は飛散させて乾燥・造粒した後、篩などによって分級して所要粒径の磁粉を得る方法（以下、この製造法を「噴霧法」という）である。 There are two methods for producing magnetic powder, one called a “pulverization method” and another called a “spraying method” by those skilled in the art. The former is the earliest proposal and reaches the present day. In this manufacturing method, an organic solvent-soluble synthetic resin is used as a binder, a fluorescent pigment is dispersed in a solution in which the resin is dissolved in a volatile organic solvent, and the magnetically conductive particle powder is placed on the fluorescent pigment. After mixing and kneading to make a paste-like material, the paste-like product is dried into a lump, and then the lump is pulverized into fine particles using a pulverizer such as a ball mill and then classified by a sieve or the like. Thus, a magnetic particle having a required particle size is obtained (hereinafter, this production method is referred to as “pulverization method”). As the latter method is disclosed in Patent Document 1, this production method comprises a water-dispersible synthetic resin or Using a water-soluble synthetic resin as a binder, After adding the photopigment and the magnetically conductive particle powder to water and stirring to form a slurry, the slurry is sprayed or scattered in the air using a spray nozzle or a centrifugal disk, dried and granulated, This is a method of classifying with a sieve or the like to obtain magnetic powder having a required particle size (hereinafter, this production method is referred to as “spraying method”).
そして、自動車メーカーの製造ラインや鉄鋼メーカーの製造ラインにおける湿式磁粉探傷試験の実施に当たって使用されている検査液は、通常、界面活性剤が300〜1000ppm含まれている水１ｌ当たり磁粉0.5〜２gを分散させたものであり、当該検査液の調製は自動車メーカーや鉄鋼メーカーの工場内において行われている。 And the inspection liquid used in the implementation of the wet magnetic particle flaw detection test in the production line of the automobile manufacturer and the steel manufacturer is usually 0.5-2g of magnetic powder per liter of water containing 300-1000ppm of surfactant. The test solution is prepared in a factory of an automobile manufacturer or a steel manufacturer.
自動車メーカーや鉄鋼メーカーの工場内では、通常、市販の湿式磁粉探傷試験用磁粉分散剤（水にHLB９〜16のノニオン系界面活性剤を２〜10重量％溶解、乳化又は分散させてなる液体。なお、必要に応じて防錆剤が添加されている）を用い、その所定量と所定量の磁粉とをよく練合させてペースト状物とした後、当該ペースト状物を攪拌下において所定量の水に投入するという手法によって前記検査液を調製している。 In a factory of an automobile manufacturer or a steel manufacturer, a commercially available magnetic particle dispersant for wet magnetic particle flaw detection test (a liquid obtained by dissolving, emulsifying or dispersing 2 to 10% by weight of a nonionic surfactant of HLB 9 to 16 in water). In addition, a rust preventive agent is added as necessary), and the predetermined amount and a predetermined amount of magnetic powder are kneaded well to obtain a paste-like material, and then the paste-like material is stirred under a predetermined amount. The test solution is prepared by a method of putting it in water.
前記検査液の調製手法は、秤取作業及び練合せ作業を必須とするために調製に時間と手間がかかるので、これを改良すべく種々調製手法が提案されており、古くは、特許文献２に開示されている鉄粉、蛍光顔料、合成樹脂バインダー、有機溶剤及び界面活性剤を混合した後に有機溶剤を蒸発させて磁粉を得る技術や特許文献３に開示されている鉄粉に蛍光顔料を含む合成樹脂バインダーを被覆した後に界面活性剤を被覆して磁粉を得る技術に見られるとおり、磁粉に界面活性剤を付着させて磁粉自体に水分散性を付与する手法が提案されている。 Since the preparation method of the test solution requires a weighing operation and a kneading operation, it takes time and labor to prepare. Various preparation methods have been proposed to improve this, and in the past, Patent Document 2 Technology to obtain magnetic powder by evaporating the organic solvent after mixing the iron powder, fluorescent pigment, synthetic resin binder, organic solvent and surfactant disclosed in JP As seen in the technique of obtaining a magnetic powder by coating a surfactant after coating a synthetic resin binder, a technique has been proposed in which a surfactant is attached to the magnetic powder to impart water dispersibility to the magnetic powder itself.
しかし、磁粉を水に充分に分散させた検査液を調製するためにはHLB９〜16のノニオン系界面活性剤を用いる必要があり、この界面活性剤は不揮発性の粘性液体であるため、これを付着させた磁粉は貯蔵中に凝集してしまうので、検査液の調製時に充分な分散状態が得られないという問題があり、本出願人が知る限り、界面活性剤を付着させた磁粉が自動車メーカーや鉄鋼メーカーの製造ラインにおける湿式磁粉探傷試験に実用された例はない。 However, in order to prepare a test solution in which magnetic powder is sufficiently dispersed in water, it is necessary to use a nonionic surfactant of HLB 9-16, and this surfactant is a non-volatile viscous liquid. Since the adhering magnetic powder aggregates during storage, there is a problem that a sufficiently dispersed state cannot be obtained at the time of preparing the test solution. As far as the present applicant knows, the magnetic powder adhering the surfactant is an automobile manufacturer. There are no examples of practical use in wet magnetic particle flaw testing on the production lines of steel makers.
本出願人は、前記問題点に鑑み、特許文献４に開示されている磁粉の粒子表面に平均粒径0.01〜0.05μmの親水性無定形二酸化珪素微粒子（例えば、アエロジル200：商品名：日本アエロジル株式会社製）を付着させた磁粉100重量部に対して粉末状フッ素系界面活性剤（例えば、ユニダインDS-101：商品名：ダイキン工業株式会社製）0.05〜１重量部を添加してなる湿式磁粉探傷試験用水分散性磁粉配合物を提案しており、当該磁粉配合物は、貯蔵安定性に優れ６ケ月貯蔵後も凝集することなく、その所定量を攪拌下において所定量の水（界面活性剤を含まない）に投入すれば、前記ペースト状物を投入する手法を採る場合と同等の分散状態の検査液が調製できるものであるが、粉末であるために秤取作業に手間がかかる点で自動車メーカーや自動車メーカーの工場内における前記検査液調製従事者の要求を100％満たすには到っていない。 In view of the above problems, the applicant of the present invention has disclosed hydrophilic amorphous silicon dioxide fine particles (for example, Aerosil 200: trade name: Nippon Aerosil) having an average particle size of 0.01 to 0.05 μm on the surface of the magnetic powder particles disclosed in Patent Document 4. Wet powder obtained by adding 0.05 to 1 part by weight of powdery fluorosurfactant (for example, Unidyne DS-101: trade name: Daikin Industries, Ltd.) to 100 parts by weight of magnetic powder to which Co., Ltd. is attached A water-dispersible magnetic powder composition for magnetic particle testing is proposed, and the magnetic powder composition is excellent in storage stability and does not aggregate after storage for 6 months. If it is put into a non-containing agent), it is possible to prepare a test solution in a dispersed state equivalent to the method of feeding the paste-like material. However, since it is a powder, it takes time to do the weighing work. At automakers and car manufacturers The test liquid prepared personnel requirements within the car factory not led to meet 100%.
何故なら、我が国の自動車メーカーや鉄鋼メーカーでは、製造ラインのスピートアップに懸命の努力がなされ、各工程において「秒」単位のスピードアップがはかられており、製造ラインにおける湿式磁粉探傷試験の実施についても可及的に時間と手間が掛らない検査液の調製手法が求められているからである。 Because, in Japan's automobile manufacturers and steel makers, the production line vinegar Pete up the hard work is done, and speed-up of the "second" unit is worn in each step, the wet magnetic particle Sagukizu試experience in the manufacturing line This is because there is a demand for a method for preparing a test solution that takes as little time and effort as possible.
そこで、本出願人は、特許文献５に開示されている磁粉20〜50重量％、HLB値10〜12のアルキルエーテル型非イオン界面活性剤８〜20重量％、アルコール２〜15重量％及び水残部からなる湿式磁粉探傷試験用濃厚磁粉分散液を提案した。当該濃厚磁粉液は、計量コップやメスシリンダーを用いてその所定量を秤取し、攪拌下において所定量の水（界面活性剤を含まない）に投入して希釈すれば、前記ペースト状物を投入する手法を採る場合と同等の分散状態の検査液が調製できるものであり、前記水分散性磁粉配合物（粉末）の秤取作業と比較して秤取作業を格段にスピートアップできるが、夏期などの高温環境下における長期保存や容器の開閉により、処方中のアルコール成分が徐々に揮発して所要濃度以下になると急激に安定性が損なわれ、容器底部に磁粉が沈降・沈澱してしまうという問題がある。なお、常温（20°〜25℃）環境下においては、かかる問題は発生しない。 Therefore, the applicant of the present invention has disclosed 20 to 50% by weight of magnetic powder disclosed in Patent Document 5, 8 to 20% by weight of an alkyl ether type nonionic surfactant having an HLB value of 10 to 12, 2 to 15% by weight of alcohol and water. A concentrated magnetic powder dispersion for wet magnetic particle testing was proposed. The concentrated magnetic powder solution is weighed in a predetermined amount using a measuring cup or graduated cylinder, poured into a predetermined amount of water (not containing a surfactant) and diluted with stirring, and the paste-like material is removed. It is possible to prepare a test solution in a dispersed state equivalent to the case of adopting the method of charging, and the weighing work can be dramatically sped up compared to the weighing work of the water-dispersible magnetic powder composition (powder), If the alcohol component in the formulation gradually evaporates and falls below the required concentration due to long-term storage in a high temperature environment such as summer, or opening and closing of the container, the stability is suddenly impaired, and magnetic powder settles and settles at the bottom of the container There is a problem. Note that such a problem does not occur in a room temperature (20 ° to 25 ° C.) environment.
また、前記HLB値10〜12のアルキルエーテル型非イオン界面活性剤として用いているポリオキシエチレンノニルフェニルエーテル及びポリオキシエチレンオクチルフェニルエーテルが、環境ホルモン問題に鑑み、近年規定されたPRTR法の対象物質であるという問題がある。 In addition, polyoxyethylene nonylphenyl ether and polyoxyethylene octylphenyl ether used as alkyl ether type nonionic surfactants having an HLB value of 10 to 12 are subject to the PRTR law that has recently been defined in view of environmental hormone problems. There is a problem of being a substance.
本発明は、前記諸問題点を解決するために、特許文献５に開示されている湿式磁粉探傷試験用濃厚磁粉分散液を用いて検査液を調製する場合と同様に、前記ペースト状物を投入する手法を採る場合と同等の分散状態の検査液を調製でき、秤取作業が格段にスピードアップし、かつ、夏期などの高温（30°〜38℃）環境下における長期保存や容器の開閉によっても磁粉の沈降・沈澱が生じないことを保証でき、しかも、環境ホルモン問題が生じない湿式磁粉探傷試験用濃厚磁粉分散液を提供することを技術的課題とする。 In order to solve the above-mentioned problems, the present invention introduces the paste-like material in the same manner as when preparing a test liquid using a concentrated magnetic powder dispersion for wet magnetic particle flaw detection disclosed in Patent Document 5. The test solution can be prepared in the same dispersion state as when using the above method, the weighing operation is significantly accelerated, and long-term storage and opening / closing of the container in a high temperature (30 ° to 38 ° C) environment such as summer It is a technical problem to provide a concentrated magnetic powder dispersion for a wet magnetic powder flaw detection test that can guarantee that no sedimentation or precipitation of magnetic powder occurs and that does not cause environmental hormone problems.
本発明者は、前記技術的課題を達成するため、分散剤と磁粉との組合せについて、思考錯誤的な数多くの試作・実験を重ねた結果、分散剤としてポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤と陰イオン活性剤を用いて噴霧法によって製造された湿式磁粉探傷試験用磁粉を水に分散させる場合には、高温（30°〜38℃）環境下における長期保存や容器の開閉による磁粉の沈降・沈澱が生じないという刮目すべき知見を得、前記技術的課題を達成したものである。 In order to achieve the above technical problem, the present inventor has made numerous trials and experiments on the combination of a dispersing agent and magnetic powder, and as a result, has made polyoxyalkylene allyl phenyl ether type nonionic system as a dispersing agent. When dispersing magnetic powder for wet magnetic particle testing, which is manufactured by spraying method using surfactant and anionic surfactant, in water, by long-term storage under high temperature (30 ° -38 ° C) environment or opening / closing of container The above technical problem has been achieved by obtaining a remarkable knowledge that no sedimentation or precipitation of magnetic powder occurs.
前記技術的課題は、次のとおりの本発明によって解決できる。 The technical problem can be solved by the present invention as follows.
すなわち、本発明は、ポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤５〜20重量％及び陰イオン活性剤0.5〜５重量％を分散剤として導磁性粒子粉末の粒子表面が合成樹脂バインダーと蛍光顔料とによって被覆されている湿式磁粉探傷試験用磁粉10〜20重量％を水に分散させてなり、当該分散液を液温４０℃で９０日静置後に当該磁粉が沈降・沈澱せずに分散していることを特徴とする湿式磁粉探傷試験用濃厚磁粉分散液である（請求項１）。 That is, according to the present invention, the surface of the magnetically conductive particle powder is made of a synthetic resin binder with 5 to 20% by weight of a polyoxyalkylene allyl phenyl ether type nonionic surfactant and 0.5 to 5% by weight of an anionic surfactant as a dispersant. 10-20 wt% powder for wet magnetic particle Sagukizu試test which is covered by the fluorescent pigment becomes dispersed in water, the magnetic powder the dispersion to 90 days standing at liquid temperature 40 ° C. does not settle, sedimentation A dense magnetic powder dispersion for a wet magnetic particle flaw detection test, characterized in that the liquid is dispersed in a magnetic particle (claim 1).
また、本発明は、前記ポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤が、ポリオキシエチレンポリスチリルフェニルエーテル、ポリオキシエチレンジスチリルフェニルエーテル及びポリオキシエチレンモノスチリルフェニルエーテルのいずれかである湿式磁粉探傷試験用濃厚磁粉分散液である（請求項２）。 Further, the present invention, the polyoxyalkylene allyl phenyl ether-type nonionic surfactant, is either polyoxyethylene polystyrylphenyl ether, polyoxyethylene di styryl phenyl ether and polyoxyethylene monostyryl phenyl ether It is a concentrated magnetic powder dispersion for wet magnetic particle testing.
また、本発明は、前記陰イオン活性剤が、多環フェニルポリエトキシスルホサクシネート、スルホコハク酸ジオクチルナトリウム、アルキルアリルスルホン酸ナトリウム、パルミチン酸ナトリウム及びラウリルエーテルリン酸のいずれかである湿式磁粉探傷試験用濃厚磁粉分散液である（請求項３）。 Further, the present invention provides a wet magnetic particle flaw detection test wherein the anionic activator is any one of polycyclic phenyl polyethoxysulfosuccinate, dioctyl sodium sulfosuccinate, sodium alkylallylsulfonate, sodium palmitate and lauryl ether phosphate. A concentrated magnetic powder dispersion for use (claim 3).
本発明に係る湿式磁粉探傷試験用濃厚磁粉分散液は、湿式磁粉探傷試験用磁粉が10〜20重量％という高濃度で分散している濃厚磁粉分散液であるにもかかわらず、後出実施例に示すとおり、当該濃厚磁粉分散液を容器に入れて該容器内の液温を40℃に保って90日間静置後にも、当該磁粉は沈降・沈澱せずに安定して分散している。 The concentrated magnetic powder dispersion for wet magnetic particle testing is according to the present invention, although it is a concentrated magnetic powder dispersion in which the magnetic powder for wet magnetic particle testing is dispersed at a high concentration of 10 to 20% by weight. As shown in FIG. 5, even after the concentrated magnetic powder dispersion is placed in a container and the liquid temperature in the container is kept at 40 ° C. and left for 90 days, the magnetic powder is stably dispersed without being settled or precipitated.
従って、本発明に係る湿式磁粉試験用濃厚磁粉分散液は、夏期などの高温（30°〜38℃）環境下における長期保存や容器の開閉によっても磁粉の沈降・沈澱が生じないことを保証できる。 Therefore, the concentrated magnetic powder dispersion for wet magnetic powder testing according to the present invention can guarantee that the magnetic powder does not settle or precipitate even when stored for a long time in a high temperature (30 ° to 38 ° C.) environment such as summer or when the container is opened and closed. .
本発明者は、本発明に係る湿式磁粉試験用濃厚磁粉液が液温40℃に保って90日間静置後にも、磁粉が沈降・沈澱せずに安定して分散しているのは、次の作用によるものと推定している。 The inventor of the present invention is that the concentrated magnetic powder liquid for wet magnetic powder test according to the present invention is kept at a liquid temperature of 40 ° C. and allowed to stand for 90 days. It is presumed to be due to the action of
すなわち、前記の安定した分散状態を実現するためには、磁粉を一次粒子のまま充分に分散させる分散力と分散させた磁粉が経時的に沈降しないように液中に留める必要があり、本発明においては、当該分散力がポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤によって付与されており、当該界面活性剤の働きによって磁粉を分散させている濃厚磁粉分散液における磁粉の沈降は比重差と磁粉粒子間の凝集力により発生するが、陰イオン活性剤を加えることによって静電反発力が高くなって沈降が抑制されており、さらに、磁粉の粒子表面が合成樹脂バインダーによって被覆されているので、磁粉粒子間の凝集力が低いことも沈降抑制に役立っている。 That is, in order to realize the above-described stable dispersion state, it is necessary to keep the dispersion force in the liquid so that the dispersion force for sufficiently dispersing the magnetic powder as primary particles and the dispersed magnetic powder do not settle over time. , The dispersion force is imparted by the polyoxyalkylene allyl phenyl ether type nonionic surfactant, and the sedimentation of the magnetic powder in the concentrated magnetic powder dispersion in which the magnetic powder is dispersed by the action of the surfactant is different in specific gravity. Is generated due to the cohesive force between the magnetic powder particles and the magnetic powder particles, but by adding an anionic activator, the electrostatic repulsion force is increased and the sedimentation is suppressed, and the particle surface of the magnetic powder is coated with a synthetic resin binder. Therefore, the low cohesive force between the magnetic powder particles also helps to suppress sedimentation.
また、本発明に係る湿式磁粉探傷試験用濃厚磁粉分散液は、計量コップなどを用いてその所定量を秤取し、攪拌下において所定量の水（界面活性剤を含まない）に投入して希釈すれば、前記ペースト状物を投入する手法を採る場合と同等の分散状態の検査液が調製できるから、前記水分散性磁粉配合物（粉末）の秤取作業と比較して秤取作業を格段にスピードアップできる。 In addition, a predetermined amount of the concentrated magnetic particle dispersion for wet magnetic particle flaw detection test according to the present invention is weighed using a measuring cup or the like, and poured into a predetermined amount of water (not including a surfactant) under stirring. When diluted, a test solution in a dispersed state equivalent to the method of introducing the paste-like material can be prepared. Therefore, the weighing operation is compared with the weighing operation of the water-dispersible magnetic powder compound (powder). You can speed up dramatically.
また、本発明に係る湿式磁粉探傷試験用濃厚磁粉分散液は、PRTR法の対象物質を用いていないから、人体や環境に優しいものである。 Further, the concentrated magnetic powder dispersion for wet magnetic particle flaw detection test according to the present invention does not use the target substance of the PRTR method, and is therefore friendly to the human body and the environment.
実施の形態． Embodiment.
本実施の形態に係る湿式磁粉探傷試験用濃厚磁粉分散液は、ポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤を５〜20重量％の範囲内での所要量と陰イオン活性剤を0.5〜５重量％の範囲内での所要量とを分散剤として導磁性粒子粉末の粒子表面が合成樹脂バインダーと蛍光顔料とによって被覆されている湿式磁粉探傷試験用磁粉を10〜20重量％の範囲内で水に分散させてなる分散液であり、当該分散液は液温40℃で90日間静置後に当該磁粉が沈降・沈澱せずに分散しているものである。 The concentrated magnetic particle dispersion for wet magnetic particle flaw detection test according to the present embodiment comprises a polyoxyalkylene allyl phenyl ether type nonionic surfactant within a range of 5 to 20% by weight and an anionic surfactant of 0.5%. A magnetic powder for a wet magnetic particle flaw detection test in which the particle surface of the magnetically conductive particle powder is coated with a synthetic resin binder and a fluorescent pigment using a required amount within a range of ˜5% by weight as a dispersant is within a range of 10 to 20% by weight. In the dispersion, the magnetic powder is dispersed without being settled or precipitated after standing at a liquid temperature of 40 ° C. for 90 days.
ポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤としては、例えば、ポリオキシエチレンポリスチリルフェニルエーテル、ポリオキシエチレンジスチリルフェニルエーテル、ポリオキシエチレンモノスチリルフェニルエーテル、ポリオキシエチレンポリオキシプロピレンポリスチリルフェニルエーテルなどの市販界面活性剤の内からHLB値１０〜１２のものを選定し、その１種又は２種以上を用いることが好ましい。 The polyoxyalkylene allyl phenyl ether-type nonionic surfactants such as polyoxyethylene polystyrylphenyl ether, polyoxyethylene di styryl phenyl ether, polyoxyethylene monostyryl phenyl ether, polyoxyethylene polyoxypropylene polystyryl It is preferable to select one having an HLB value of 10 to 12 from commercially available surfactants such as phenyl ether and using one or more of them.
前記ポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤の配合量は、５〜20重量％の範囲内で選定する必要があり、５重量％未満の場合には充分な分散力が得られないので分散液中の磁粉が沈降・沈澱し、20重量％を越えると粘性が高くなりすぎる。 The blending amount of the polyoxyalkylene allyl phenyl ether type nonionic surfactant needs to be selected within a range of 5 to 20% by weight, and if it is less than 5% by weight, sufficient dispersing power cannot be obtained. Therefore, the magnetic powder in the dispersion settles and precipitates, and if it exceeds 20% by weight, the viscosity becomes too high.
陰イオン活性剤としては、例えば、多環フェニルポリエトキシスルホサクシネート、スルホコハク酸ジオクチルナトリウム、アルキルアリルスルホン酸ナトリウム、パルミチン酸ナトリウム、ラウリルエーテルリン酸などの市販陰イオン活性剤の内から選定して用いることが好ましく、本発明品を用いて調製する検査液の使用時（湿式磁粉探傷試験実施時）における検査液の泡立ちや検査物の濡れ性などの点からして、アルキルスルホサクシネート系のものが最も好ましい。 The anionic activator is selected from commercially available anionic activators such as polycyclic phenylpolyethoxysulfosuccinate, dioctyl sodium sulfosuccinate, sodium alkylallyl sulfonate, sodium palmitate, lauryl ether phosphate and the like. It is preferable to use the alkyl sulfosuccinate type in terms of foaming of the test solution and wettability of the test object when using the test solution prepared using the product of the present invention (during the wet magnetic particle flaw detection test). Is most preferred.
前記陰イオン活性剤の配合量は、0.5〜５重量％の範囲内で選定する必要があり、0.5重量％未満の場合には充分な静電反発力が得られないので分散液中の磁粉が沈降・沈澱し、５重量％を越えても配合量に応じた効果は認められない。 The blending amount of the anionic active agent must be selected within the range of 0.5 to 5% by weight, and if it is less than 0.5% by weight, a sufficient electrostatic repulsion cannot be obtained. Even if the amount exceeds 5% by weight, the effect corresponding to the blending amount is not recognized.
なお、前記各市販陰イオン活性剤の内には、後出実施例に見られるとおり、有効成分75％のものも存在している点に留意する必要がある。 It should be noted that some of the above-mentioned commercially available anionic activators include those having an active ingredient of 75%, as will be seen in Examples below.
導磁性粒子粉末の粒子表面が合成樹脂バインダーと蛍光顔料とによって被覆されている湿式磁粉探傷試験用磁粉としては、噴霧法によって製造された市販の湿式磁粉探傷試験用磁粉を用いればよく、具体的には、湿式磁粉探傷用磁粉スーパーマグナLY-10（商品名：マークテック株式会社製）、同スーパーマグナLY-20（商品名：マークテック株式会社製）及び同スーパーマグナLY-20P（商品名：マークテック株式会社製）が挙げられる。 As the magnetic powder for wet magnetic particle flaw detection test in which the particle surface of the magnetic conductive particle powder is coated with a synthetic resin binder and a fluorescent pigment, a commercially available magnetic powder for wet magnetic particle flaw detection test manufactured by a spray method may be used. Includes magnetic powder super magna LY-10 (product name: manufactured by Mark Tech Co., Ltd.), super magna LY-20 (product name: manufactured by Mark Tech Co., Ltd.) and super magna LY-20P (product name). : Mark Tech Co., Ltd.).
前記湿式磁粉探傷試験用磁粉の配合量については、当該磁粉の配合量が増えるに従って分散液を液温40℃で90日間静置後における該磁粉の分散安定性が低下し、約25重量％を越えると磁粉の沈降・沈澱が生じてしまう。なお、当該磁粉の配合量が減れば、その分散安定性は向上するが、反面、検査液の調製に当たって多量の磁粉分散液が必要となるために秤取作業に手間がかかることになる。 Regarding the blending amount of the magnetic powder for wet magnetic particle flaw detection test, as the blending amount of the magnetic powder increases, the dispersion stability of the magnetic powder after standing for 90 days at a liquid temperature of 40 ° C. decreases, and about 25% by weight. If it exceeds, sedimentation and precipitation of magnetic powder will occur. If the blending amount of the magnetic powder is reduced, the dispersion stability is improved, but on the other hand, a large amount of the magnetic powder dispersion is required for the preparation of the test solution, so that the weighing work is troublesome.
秤取作業、磁粉分散液充填容器の寸法、保管スペース、運送費用などの観点からして、10〜20重量％の範囲内で配合することが好ましい。 From the viewpoints of weighing work, the size of the container filled with the magnetic powder dispersion, storage space, transportation cost, etc., it is preferable to blend within the range of 10 to 20% by weight.
なお、粉砕法によって製造された市販の湿式磁粉探傷試験用磁粉は、その製造法に起因して導磁性粒子粉末の粒子表面に存在する合成樹脂バインダーの量が少ないので磁粉粒子間の凝集力が高いから、その使用は避けるべきである（後出比較例２参照）。
In addition, the commercially available magnetic powder for wet magnetic particle flaw detection test produced by the pulverization method has a small amount of the synthetic resin binder present on the particle surface of the magnetically conductive particle powder due to the production method, so that the cohesive force between the magnetic powder particles is low. Since it is expensive, its use should be avoided (see Comparative Example 2 below).
本実施の形態に係る湿式磁粉探傷試験用濃厚磁粉液の製造は容易である。 Production of the concentrated magnetic powder for wet magnetic particle testing is easy.
すなわち、前記各市販界面活性剤の内から選定したHLB値10〜12のポリオキシアルキレンアリルフェニルエーテル型非イオン系界面活性剤が５〜20重量％の範囲内、前記各市販陰イオン活性剤の内から選定した陰イオン活性剤が0.5〜５重量％の範囲内、前記噴霧法によって製造された各市販湿式磁粉探傷試験用磁粉から選定した導磁性粒子粉末の粒子表面が合成樹脂バインダーと蛍光顔料とによって被覆されている湿式磁粉探傷試験用磁粉が10〜20重量％の範囲内、残部が水となるように、それぞれ秤取し、ステンレス製タンクに、先ず、秤取した当該非イオン系界面活性剤、当該陰イオン活性剤及び当該水を入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、秤取した当該磁粉を加え、さらに60分間攪拌すれば、目的とする湿式磁粉探傷試験用濃厚磁粉分散液が得られる。 That is, the polyoxyalkylene allyl phenyl ether type nonionic surfactant having an HLB value of 10 to 12 selected from the above-mentioned commercially available surfactants is in the range of 5 to 20% by weight. In the range of 0.5 to 5% by weight of the anionic activator selected from the above, the surface of the magnetically conductive particle powder selected from the magnetic powders for each of the commercially available wet magnetic particle flaw detection tests produced by the spray method is a synthetic resin binder and a fluorescent pigment. The nonionic interface was first weighed in a stainless steel tank so that the magnetic powder for wet magnetic particle flaw detection test covered by and in the range of 10 to 20% by weight and the balance was water Add the activator, the anionic activator and the water, stir for 15 minutes at room temperature (about 25 ° C.) using a propeller-type electric mixer, add the weighed magnetic powder while continuing stirring, 60 minutes By stirring for a while, the intended concentrated magnetic powder dispersion for wet magnetic particle testing is obtained.
ここに得られる湿式磁粉探傷試験用濃厚磁粉分散液には、磁粉の分散安定性を阻害しない限り、湿式磁粉探傷試験の実施に当たって常用されている消泡剤、防錆剤、防腐剤、湿潤剤などの所要量を添加することができる。 The concentrated magnetic particle dispersion for wet magnetic particle flaw detection test obtained here has a defoaming agent, rust preventive agent, preservative, and wetting agent that are commonly used in the wet magnetic particle flaw detection test unless the dispersion stability of the magnetic powder is impaired. The required amount such as can be added.
ここに得られる湿式磁粉探傷試験用濃厚磁粉分散液を用いた検査液の調製も容易である。 It is also easy to prepare a test liquid using the dense magnetic powder dispersion liquid for wet magnetic particle flaw detection test obtained here.
所要量の水（界面活性剤を含まない）を入れたタンクに、その水面をスパチュラーなどを用いて攪拌しながら、ここに得られる湿式磁粉探傷試験用濃厚磁粉分散液の所要量（通常、水１ｌ当たり磁粉0.5〜２ｇとなる量）を計量コップなどを用いて秤取して投入すれば、当該濃厚磁粉分散液は瞬時に分散し、磁粉が均一に分散している検査液が調製でき、当該検査液には乳化剤として用いた前記界面活性剤が所要濃度（通常、水１ｌ当たり25〜400ppm）で含まれている。 While stirring the water surface with a spatula or the like in a tank containing the required amount of water (without surfactant), the required amount of the concentrated magnetic powder dispersion for wet magnetic particle testing (usually water) If we measure and put in 0.5 to 2 g of magnetic powder per liter) using a measuring cup or the like, the concentrated magnetic powder dispersion liquid is instantly dispersed, and a test liquid in which the magnetic powder is uniformly dispersed can be prepared. The test solution contains the surfactant used as an emulsifier at a required concentration (usually 25 to 400 ppm per liter of water).
本発明を実施例及び比較例によって詳しく説明すれば、次のとおりである。 The present invention will be described in detail with reference to examples and comparative examples.
実施例１：ステンレス製タンクに、水道水570ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）200ｇ及びスルホコハク酸ジオクチルナトリウム（有効成分75％・日本乳化剤株式会社製）30ｇ及び消泡剤KS-537（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-10（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して湿式磁粉探傷試験用濃厚磁粉分散液1000ｇを得た。 Example 1: In a stainless steel tank, 570 g of tap water, 200 g of polyoxyethylene polystyryl phenyl ether (HLB11) and 30 g of dioctyl sodium sulfosuccinate (active ingredient 75%, manufactured by Nippon Emulsifier Co., Ltd.) and an antifoaming agent KS-537 ( 50 g of product name (manufactured by Shin-Etsu Chemical Co., Ltd.) was added and stirred at room temperature (about 25 ° C) for 15 minutes using a propeller-type electric mixer. -10 (trade name / manufacturing history: spray method, manufactured by Marktec Co., Ltd.) 150 g was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a concentrated magnetic powder dispersion for wet magnetic particle testing.
実施例２：ステンレス製タンクに、水道水600ｇ、ポリオキシエチレンモノスチリルフェニルエーテル（HLB10.5）50ｇ、多環フェニルポリエトキシスルホサクシネート（エアロールT-1500：商品名・有効成分75％・東邦化学工業株式会社製）30ｇ、防錆剤（亜硝酸ナトリウム）20ｇ及び消泡剤KM-75（商品名・信越化学工業株式会社製）100ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-20P（商品名・製造履歴：噴霧法・マークテック株式会社製）200ｇを加え、さらに60分間攪拌して湿式磁粉探傷試験用濃厚磁粉分散液1000ｇを得た。 Example 2: In a stainless steel tank, tap water 600g, polyoxyethylene monostyryl phenyl ether (HLB10.5) 50g, polycyclic phenyl polyethoxysulfosuccinate (Air Roll T-1500: trade name, active ingredient 75%, Toho 30 g of chemical industry), 20 g of rust inhibitor (sodium nitrite) and 100 g of antifoaming agent KM-75 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), and at room temperature (about 25 ° C), propeller type After stirring for 15 minutes using an electric mixer, add 200 g of magnetic powder Super Magna LY-20P (trade name / manufacturing history: spray method, manufactured by Marktec Co., Ltd.) for wet magnetic particle testing for 60 minutes while continuing stirring. By stirring, 1000 g of a concentrated magnetic powder dispersion for wet magnetic particle testing was obtained.
実施例３：ステンレス製タンクに、水道水650ｇ、ポリオキシエチレンジスチリルフェニルエーテル（HLB10）50ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）50ｇ及びアルキルアリルスルホン酸ナトリウム50ｇ及び消泡剤KS-537（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-10（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して湿式磁粉探傷試験用濃厚磁粉分散液1000ｇを得た。 Example 3: In a stainless steel tank, tap water 650 g, polyoxyethylene distyryl phenyl ether (HLB10) 50 g, polyoxyethylene polystyryl phenyl ether (HLB11) 50 g, sodium alkylallyl sulfonate 50 g and antifoam KS-537 (Product name: Shin-Etsu Chemical Co., Ltd.) 50 g was added and stirred at room temperature (about 25 ° C) for 15 minutes using a propeller-type electric mixer. LY-10 (trade name / manufacturing history: spray method, manufactured by Marktec Co., Ltd.) (150 g) was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a concentrated magnetic powder dispersion for wet magnetic particle testing.
実施例４：ステンレス製タンクに、水道水580ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）200ｇ、パルミチン酸ナトリウム20ｇ及び消泡剤KM-75（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-20（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して湿式磁粉探傷試験用濃厚磁粉分散液1000ｇを得た。 Example 4: In a stainless steel tank, 580 g of tap water, 200 g of polyoxyethylene polystyryl phenyl ether (HLB11), 20 g of sodium palmitate and 50 g of antifoaming agent KM-75 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.) After stirring for 15 minutes using a propeller-type electric mixer at room temperature (about 25 ° C), magnetic powder super magna LY-20 for wet magnetic particle flaw detection test (trade name / manufacturing history: spraying method / mark) 150 g of Tech Co., Ltd.) was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a concentrated magnetic powder dispersion for wet magnetic particle testing.
実施例５：ステンレス製タンクに、水道水700ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）100ｇ及びラウリルエーテルリン酸10ｇ、防錆剤（亜硝酸ナトリウム）20ｇ及び消泡剤KS-538（商品名・信越化学工業株式会社製）20ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-10（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して湿式磁粉探傷試験用濃厚磁粉分散液1000ｇを得た。 Example 5: In a stainless steel tank, 700 g of tap water, 100 g of polyoxyethylene polystyryl phenyl ether (HLB11) and 10 g of lauryl ether phosphoric acid, 20 g of a rust preventive (sodium nitrite) and an antifoaming agent KS-538 (trade name)・ Add 20 g of Shin-Etsu Chemical Co., Ltd.) and stir for 15 minutes at room temperature (about 25 ° C) using a propeller-type electric mixer. (Product name / manufacturing history: spray method / manufactured by Marktec Co., Ltd.) 150 g was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a concentrated magnetic powder dispersion for wet magnetic particle testing.
比較例１：ステンレス製タンクに、水道水600ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）200ｇ及び消泡剤KS-537（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-10（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して比較用濃厚磁粉分散液1000ｇを得た。 Comparative Example 1: In a stainless steel tank, 600 g of tap water, 200 g of polyoxyethylene polystyryl phenyl ether (HLB11) and 50 g of an antifoaming agent KS-537 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.) are placed at room temperature (about 25 ℃ -10), using a propeller-type electric mixer for 15 minutes, and then continuing the stirring, magnetic powder super magna LY-10 for wet magnetic particle flaw detection test (trade name / manufacturing history: spray method, manufactured by Marktec Co., Ltd.) 150 g was added and further stirred for 60 minutes to obtain 1000 g of a comparative concentrated magnetic powder dispersion.
比較例２：ステンレス製タンクに、水道水570ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）200ｇ及びスルホコハク酸ジオクチルナトリウム（有効成分75％・日本乳化剤株式会社製）30ｇ及び消泡剤KS-537（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-1500（商品名・製造履歴：粉砕法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して比較用濃厚磁粉分散液1000ｇを得た。 Comparative Example 2: In a stainless steel tank, 570 g of tap water, 200 g of polyoxyethylene polystyryl phenyl ether (HLB11) and 30 g of dioctyl sodium sulfosuccinate (active ingredient 75%, manufactured by Nippon Emulsifier Co., Ltd.) and an antifoaming agent KS-537 ( 50 g of product name (manufactured by Shin-Etsu Chemical Co., Ltd.) was added and stirred at room temperature (about 25 ° C) for 15 minutes using a propeller-type electric mixer. -1500 (trade name / manufacturing history: pulverization method, manufactured by Marktec Co., Ltd.) 150 g was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a comparative concentrated magnetic powder dispersion.
比較例３：ステンレス製タンクに、水道水595ｇ、ポリオキシエチレンイソデシルエーテル（HLB11）200ｇ、スルホコハク酸ジオクチルナトリウム（有効成分75％・日本乳化剤株式会社製）５ｇ及び消泡剤KM-75（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-20（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して比較用濃厚磁粉分散液1000ｇを得た。 Comparative Example 3: In a stainless steel tank, tap water 595 g, polyoxyethylene isodecyl ether (HLB11) 200 g, dioctyl sodium sulfosuccinate (active ingredient 75%, manufactured by Nippon Emulsifier Co., Ltd.) and antifoam KM-75 (product) (Made by Shin-Etsu Chemical Co., Ltd.) 50g, stirred for 15 minutes at room temperature (about 25 ° C) using a propeller-type electric mixer, and then continued stirring, magnetic powder super magna LY- for wet magnetic particle testing 150 g of 20 (trade name / manufacturing history: spraying method / manufactured by Marktec Co., Ltd.) was added and stirred for 60 minutes to obtain 1000 g of a comparative concentrated magnetic powder dispersion.
比較例４：ステンレス製タンクに、水道水500ｇ、ポリオキシエチレンジスチリルフェニルエーテル（HLB10）150ｇ、ポリオキシエチレンポリスチリルフェニルエーテル（HLB11）100ｇ、アルキルアリルスルホン酸ナトリウム50ｇ及び消泡剤KS-537（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-10（商品名・製造履歴：噴霧法・マークテック株式会社製）150ｇを加え、さらに60分間攪拌して比較用濃厚磁粉分散液（ゲル状物）1000ｇを得た。 Comparative Example 4: In a stainless steel tank, tap water 500 g, polyoxyethylene distyryl phenyl ether (HLB10) 150 g, polyoxyethylene polystyryl phenyl ether (HLB11) 100 g, sodium alkylallylsulfonate 50 g and antifoam KS-537 (Product name: Shin-Etsu Chemical Co., Ltd.) 50 g was added and stirred at room temperature (about 25 ° C) for 15 minutes using a propeller-type electric mixer. 150 g of LY-10 (trade name / manufacturing history: spraying method / manufactured by Marktec Co., Ltd.) was added, and the mixture was further stirred for 60 minutes to obtain 1000 g of a comparative concentrated magnetic powder dispersion (gel-like product).
比較例５：ステンレス製タンクに、水道水696ｇ、ポリオキシエチレンモノスチリルフェニルエーテル（HLB10.5）４ｇ、多環フェニルポリエトキシスルホサクシネート（エアロールT-1500：商品名・有効成分75％・東邦化学工業株式会社製）30ｇ、防錆剤（亜硝酸ナトリウム）20ｇ及び消泡剤KM-75（商品名・信越化学工業株式会社製）50ｇを入れ、室温（約25℃）にて、プロペラ式電動ミキサーを用いて15分間攪拌した後、攪拌を続けながら、湿式磁粉探傷試験用磁粉スーパーマグナLY-20P（商品名・製造履歴：噴霧法・マークテック株式会社製）200ｇを加え、さらに60分間攪拌して比較用濃厚磁粉分散液1000ｇを得た。 Comparative Example 5: In a stainless steel tank, tap water 696 g, polyoxyethylene monostyryl phenyl ether (HLB10.5) 4 g, polycyclic phenyl polyethoxysulfosuccinate (Air Roll T-1500: trade name, active ingredient 75%, Toho 30 g of chemical industry), 20 g of rust inhibitor (sodium nitrite) and 50 g of antifoaming agent KM-75 (trade name, manufactured by Shin-Etsu Chemical Co., Ltd.), and propeller type at room temperature (about 25 ° C) After stirring for 15 minutes using an electric mixer, add 200 g of magnetic powder Super Magna LY-20P (trade name / manufacturing history: spray method, manufactured by Marktec Co., Ltd.) for wet magnetic particle testing for 60 minutes while continuing stirring. By stirring, 1000 g of a comparative concentrated magnetic powder dispersion was obtained.
実施例１〜５及び比較例１〜５に係る評価を、次のとおりの濃厚磁粉液分散安定性試験及び湿式磁粉探傷試験によって行った。 The evaluation which concerns on Examples 1-5 and Comparative Examples 1-5 was performed by the following concentrated magnetic powder liquid dispersion stability tests and wet magnetic particle flaw detection tests.
濃厚磁粉液分散安定性試験：実施例１〜５で得た各濃厚磁粉分散液及び比較例１〜５で得た比較用濃厚磁粉分散液（但し、比較例４はゲル状物）を、それぞれ各透明ガラス製ビーカーに200ｇ宛とり、各ビーカーを小穴を開けたアルミホイルによって蓋をした状態で、冷蔵槽内においてビーカー内の液温５℃に保って90日間静置した後の各磁粉分散液の状態と恒温槽内においてビーカー内の液温40℃に保って90日間静置した後の各分散液の状態とを、それぞれ目視にて観察し、上澄み及び沈澱がないものを「○」、10％（体積）以下の上澄みが発生したが沈澱がないものを「△」、沈澱したものを「×」と評価した。 Dense magnetic powder dispersion stability test: Each of the concentrated magnetic powder dispersions obtained in Examples 1 to 5 and the comparative concentrated magnetic powder dispersion obtained in Comparative Examples 1 to 5 (however, Comparative Example 4 is a gel), respectively. Dispersion of each magnetic powder after being left for 90 days in a refrigerated tank with the liquid temperature in the beaker kept at 5 ° C. with 200 g each transparent glass beaker covered with aluminum foil with small holes. The state of the liquid and the state of each dispersion after standing for 90 days with the liquid temperature in the beaker kept at 40 ° C. in the thermostat are visually observed, and “○” indicates that there is no supernatant and no precipitation. A sample having a supernatant of 10% (volume) or less but having no precipitation was evaluated as “Δ”, and a precipitate was evaluated as “x”.
湿式磁粉探傷試験：実施例１〜５で得た各濃厚磁粉分散液及び比較例１〜５で得た各比較用濃厚磁粉分散液（但し、比較例４はゲル状物）と前記濃厚磁粉分散安定性試験（40℃）実施後の実施例１〜５で得た各濃厚磁粉分散液及び比較例１〜５で得た各比較用濃厚磁粉分散液（但し、比較例４はゲル状物）とを用い、それぞれを磁粉濃度１g／ｌとなるようにメスシリンダーを用いて秤取し、秤取した各磁粉分散液を、それぞれ水道水を入れた各タンクに攪拌下において投入して各検査液を調製した。 Wet magnetic particle testing: each concentrated magnetic powder dispersion obtained in Examples 1 to 5 and each comparative concentrated magnetic powder dispersion obtained in Comparative Examples 1 to 5 (however, Comparative Example 4 is a gel) and the concentrated magnetic powder dispersion Each concentrated magnetic powder dispersion obtained in Examples 1 to 5 after the stability test (40 ° C.) and each comparative concentrated magnetic powder dispersion obtained in Comparative Examples 1 to 5 (however, Comparative Example 4 is a gel) And weighed each using a graduated cylinder so that the magnetic powder concentration becomes 1 g / l, and put each weighed magnetic powder dispersion into each tank containing tap water under stirring, for each inspection. A liquid was prepared.
前記各検査液ごとに、JIS-Z-2320-2に規定されている『対比試験片タイプ１』を浸潰してゆっくりと引き上げ、暗室において紫外線灯を照射して当該試験表面に形成された欠陥指示模様を目視にて観察し、前記濃厚磁粉液分散安定性試験実施前の濃厚磁粉分散液（含、比較用濃厚磁粉分散液）を用いた検査液による欠陥指示模様と前記濃厚磁粉液分散安定性試験（40℃）実施後の濃厚磁粉分散液（含、比較用濃厚磁粉分散液）を用いた検査液による欠陥指示模様とに変化が認められないものを「○」、変化が認められるものを「×」と評価した。 For each of the above test solutions, the "contrast specimen type 1" specified in JIS-Z-2320-2 is soaked and slowly pulled up, and a defect formed on the test surface by irradiating with an ultraviolet lamp in a dark room The indication pattern is visually observed, and the defect indication pattern by the test solution using the concentrated magnetic powder dispersion (including the comparative concentrated magnetic powder dispersion) before the concentrated magnetic powder dispersion stability test is conducted and the concentrated magnetic powder dispersion stability That there is no change in the defect indication pattern by the inspection liquid using the concentrated magnetic powder dispersion (including comparative magnetic powder dispersion for comparison) after the performance test (40 ° C) is performed. Was evaluated as “×”.
前記各試験における各評価結果を表１に示す。 Table 1 shows each evaluation result in each test.
本発明によれば、湿式磁粉探傷試験に用いられる検査液の調製作業を格段にスピードアップできると共に、人や環境に優しく、しかも、夏期などの高温（30°〜38℃）環境下における長期保存や容器の開閉によっても磁粉の沈降・沈澱が生じない湿式磁粉探傷試験用濃厚磁粉分散液が提供できるので、大量の検査液の調製を必要としている自動車メーカーや鉄鋼メーカーの各製造ラインにおける湿式磁粉探傷試験従事者の要請に応じることができるから、本発明の産業利用性は大きいといえる。 According to the present invention, the preparation of a test solution used in a wet magnetic particle flaw detection test can be significantly speeded up, and it is friendly to people and the environment, and is also stored for a long time in a high temperature (30 ° to 38 ° C.) environment such as summer. We can provide a concentrated magnetic powder dispersion for wet magnetic particle flaw detection tests that does not cause sedimentation or precipitation of magnetic particles even when the container is opened or closed, so that wet magnetic particles in each production line of automobile manufacturers and steel manufacturers that need to prepare a large amount of inspection liquid It can be said that the industrial applicability of the present invention is great because it can meet the demands of flaw detection test workers.
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| JPS6035252A (en) * | 1983-08-08 | 1985-02-23 | Tokushu Toryo Kk | Dispersant for magnetic powder liquid used in wet type magnetic flaw detector |
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