EP1319702B1 - Lubrifiant aqueux pour le travail plastique d'un materiau metallique et procede d'elaboration d'un film lubrifiant - Google Patents

Lubrifiant aqueux pour le travail plastique d'un materiau metallique et procede d'elaboration d'un film lubrifiant Download PDF

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Publication number
EP1319702B1
EP1319702B1 EP01925970.4A EP01925970A EP1319702B1 EP 1319702 B1 EP1319702 B1 EP 1319702B1 EP 01925970 A EP01925970 A EP 01925970A EP 1319702 B1 EP1319702 B1 EP 1319702B1
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EP
European Patent Office
Prior art keywords
lubricative
metallic material
aqueous lubricant
wax
lubricant
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.)
Expired - Lifetime
Application number
EP01925970.4A
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German (de)
English (en)
Other versions
EP1319702A4 (fr
EP1319702A1 (fr
Inventor
Yasuo c/o Nihon Parkerizing Co. Ltd. IMAI
Shuji c/o Nihon Parkerizing Co. Ltd. NAGATA
Masayuki c/o Nihon Parkerizing Co. Ltd. YOSHIDA
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.)
Henkel AG and Co KGaA
Original Assignee
Henkel AG and Co KGaA
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Publication of EP1319702A1 publication Critical patent/EP1319702A1/fr
Publication of EP1319702A4 publication Critical patent/EP1319702A4/fr
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Publication of EP1319702B1 publication Critical patent/EP1319702B1/fr
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M173/00—Lubricating compositions containing more than 10% water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B21C9/005—Cold application of the lubricant
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES OR PROFILES, OTHERWISE THAN BY ROLLING; AUXILIARY OPERATIONS USED IN CONNECTION WITH METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL
    • B21C9/00—Cooling, heating or lubricating drawing material
    • B21C9/02—Selection of compositions therefor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21J—FORGING; HAMMERING; PRESSING METAL; RIVETING; FORGE FURNACES
    • B21J3/00—Lubricating during forging or pressing
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M111/00—Lubrication compositions characterised by the base-material being a mixture of two or more compounds covered by more than one of the main groups C10M101/00 - C10M109/00, each of these compounds being essential
    • C—CHEMISTRY; METALLURGY
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    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/02—Carbon; Graphite
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M125/00—Lubricating compositions characterised by the additive being an inorganic material
    • C10M125/10—Metal oxides, hydroxides, carbonates or bicarbonates
    • C—CHEMISTRY; METALLURGY
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    • C10M125/22—Compounds containing sulfur, selenium or tellurium
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    • C10M125/26—Compounds containing silicon or boron, e.g. silica, sand
    • C—CHEMISTRY; METALLURGY
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    • C10M159/00—Lubricating compositions characterised by the additive being of unknown or incompletely defined constitution
    • C10M159/02—Natural products
    • C10M159/06—Waxes, e.g. ozocerite, ceresine, petrolatum, slack-wax
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    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
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    • C10M2201/0413—Carbon; Graphite; Carbon black used as base material
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    • C10M2201/0663—Molybdenum sulfide used as base material
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    • C10M2201/0873—Boron oxides, acids or salts used as base material
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    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
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    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01—Emulsions, colloids, or micelles
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    • C10N2070/00—Specific manufacturing methods for lubricant compositions

Definitions

  • This invention relates to an aqueous lubricant used for plastic working of metallic material such as iron and steel, stainless steel, titanium, aluminum and others, wherein the surface of the metallic material has not been given any chemical conversion treatment. Also, it relates to a process of using the lubricant.
  • this invention relates to an aqueous lubricant used for producing a lubricative film suitable for plastic deforming work such as forging, wire drawing, tube drawing and others, on the surface of the metallic materials such as iron and steel, stainless steel, titanium, aluminum and others, wherein the surface of the metallic material has not been subjected to any chemical conversion treatment.
  • lubricative film are generally provided on the surface of the metallic material in order to prevent burning defects and galling defects which are arisen by metallic contact between the metallic material and tool.
  • lubricative film being provided on the metal surface
  • lubricative film in which lubricative agent is made to adhere physically on the metal surface
  • other type of lubricative film in which chemical conversion layer are produced on the metal surface previously by chemical conversion treatment of the metallic material and then lubricative agent are applied on the chemical conversion layer.
  • the lubricative agent being adhered physically on the metal surface are used generally for cold working of slight amount of reduction since adhesive power of these are inferior than the adhesive power of the lubricative agent being applied on the chemical conversion layer.
  • phosphate film or oxalate film are provided on the metal surface, which has a role as a carrier for the lubricative agent being applied on it.
  • the lubricative film of this type are constructed by 2 layers, the carrier layer and the lubricative agent layer, and shows very excellent resistance against burning defect of the metallic material. And are used in a wide range of the cold working such as wire drawing, tube drawing, forging and others. And besides in the field of the cold working of heavy amount of reduction, it is widely used to provide a phosphate film or oxalate film, and a lubricative agent are applied on that.
  • the lubricative agent applied on the chemical conversion layer may be divided into two groups in terms of the usage.
  • the first group includes a lubricative agent to be mechanically adhered onto the chemical conversion layer and the second group includes a lubricative agent which reacts with the chemical conversion layer.
  • the first group of lubricative agent includes those being prepared by using mineral oil, vegetable oil or synthetic oil as base oil and containing an extreme pressure additive in the base oil, also includes other one being prepared by dissolving a solid lubricative agent, such as graphite and molybdenum disulfide, together with a binder component into the water. These are adhered and then dried.
  • a solid lubricative agent such as graphite and molybdenum disulfide
  • These lubricative agent of the first group may have advantages of easy for handling the solution since they may be used simply by means of spray coating or dipping coating. However, as they have just a low lubricative properties, they tend to be used for a case where slight amount of deformation of the metallic material is required.
  • a reactive soap such as sodium stearate is used for a cold working where high lubricative property is required
  • the reactive soap reacts with the chemical conversion layer and provides a layer of high lubricative property.
  • JP52-20967A wherein a lubricant composition containing water soluble polymer or its aqueous emulsion as the base component, a solid lubricant and a film-forming agent has been disclosed.
  • a lubricant composition containing water soluble polymer or its aqueous emulsion as the base component, a solid lubricant and a film-forming agent has been disclosed.
  • no composition which has the same degree of preferable effect as in the conventional process of using a chemical conversion layer has been obtained.
  • JP10-8085A relates to an aqueous lubricant used for plastic working of metallic material in which (A) water soluble inorganic salt, (B) solid lubricative agent, (C) at least one oil selected from a group consisting of mineral oil, animal oil, vegetable oil and synthetic oil, (D) surface active agent and (E) water are well dispersed and emulsified homogeneously.
  • the lubricant according to this prior art is too unstable to use in an industry since it has to keep to emulsify the oil component, and is not showing a stable properties.
  • JP2000-63880A As another prior art, an invention of JP2000-63880A can be cited.
  • This prior art is directed to a lubricant used for plastic working of metallic material comprising (A) synthetic resin, (B) water soluble inorganic salt and water, wherein the ratio of (B)/(A) by weight in solid state is in a range from 0. 25/1 to 9/1 and the synthetic resin is kept dissolved or dispersed in the composition.
  • this composition is also not stable to show a high lubricative properties in cold working of heavy amount of reduction, since its main component is the synthetic resin.
  • WO 99/64544 A1 discloses lubricants for the plastic working of metals constituted of a water soluble inorganic salts selected from tungstate, sulfate or borate, a lubricative agent selected from graphite powder or molybdenum disulfide and a polyethylene wax.
  • the inventors have investigated for solving the problems described above and have found that the excellent lubricative properties can be obtained by the aqueous solution containing water soluble inorganic salt, lubricative agent being selected from molybdenum disulphide and graphite, and wax at the specific ratio. Further, they have found out a method of lubricative film processing on the metal surface in saving the treating energy and in saving the treating space.
  • the present invention is an aqueous lubricant used for working the metallic material which contains (A) water soluble inorganic salt, being selected from a group of sulfate, silicate, borate, molybdate and tungstate, (B) lubricative agent being selected from molybdenum disulphid and graphite, and (C) wax, and these components are dissolved or dispersed in water and weight ratio in solid state of (B)/(A) is in the range of 1.0 ⁇ 5.0 and a weight ratio in solid state of (C)/(A) is in the range of 0.1 ⁇ 1.0.
  • A water soluble inorganic salt, being selected from a group of sulfate, silicate, borate, molybdate and tungstate
  • B lubricative agent being selected from molybdenum disulphid and graphite
  • C wax
  • wax as above is water dispersed natural wax or synthetic wax having melting point between 70 ⁇ 150°C.
  • the present invention is a method of processing of the lubrication film of 0.5 ⁇ 40g/m 2 as adherent weight on the surface of the metallic material wherein the aqueous lubricant of above is applied to the cleaned surface of the metallic material and is then dried. It is preferable that the surface of the metallic material is previously cleaned by one or more process selected from a group of shot blasting, sand blasting, alkaline degreasing and acid cleaning, and also preferable that the aqueous lubricant is applied on the surface of the metallic material after the metallic material is heated to 60 ⁇ 100°C.
  • the water soluble inorganic salt (A) used in the aqueous lubricant of the invention is contained in order to give hardness and strength to the coating film. For this purpose, it is required to have a property to be uniformly dissolved in the aqueous solution and to form a strong lubricative film after drying.
  • the inorganic salt giving such property it is preferable to use at least one selected from a group consisting of sulfate, silicate, borate, molybdate and tungstate.
  • sulfate, silicate, borate, molybdate and tungstate As the examples for the inorganic salt described above, sodium sulfate, potassium sulfate, potassium silicate, sodium borate (sodium tetraborate), potassium borate (potassium tetraborate), ammonium borate (ammonium tetraborate), ammonium molybdate, sodium molybdate and sodium tungstate may be given. Any of these salts may be used either alone or in combination of 2 or more salts.
  • one or more than one of the lubricative agent (B) being selected from molybdenum disulphide and graphite are used in order to enhance the lubricative properties. They are contained in a form of being dispersed, and the known surfactant may be used when necessary.
  • the (B)/(A), namely the weight ratio in solid state of the water soluble inorganic salt (A) and the lubricative agent (B), is in a range of 1.0 ⁇ 5.0. And is preferable to be 2.0 ⁇ 4.0.
  • the ratio is less than 1.0, sliding properties of the lubricative film are decreased.
  • the ratio exceeds 5.0, the aqueous lubricant become unstable.
  • wax (C) it is preferable to use a natural wax or a synthetic wax, though there is no specific limitation in its chemical structure and the type.
  • the wax may melt by a heat generated during the plastic deformation of the metallic material thereby improve the lubricative property of the coating layer. For this reason, it is preferable to use those having a melting point in a range of 70 ⁇ 150°C and being stable in aqueous lubricant and those not to weaken the strength of the lubricative film so as to perform the preferable lubrication from the early stage of the plastic working.
  • the practical examples for the wax may include paraffin wax, micro crystalline wax, petrolatum wax, fisher ⁇ tropsch wax, polyethylene wax, polypropylene wax, carnauba wax, montane wax and the like. These waxes are preferably combined with another component and contained in a form of water dispersion or water emulsion in the aqueous lubricant of the invention.
  • the (C)/(A), namely the weight ratio in solid state of water soluble inorganic salt (A) and the wax (C) is in a range of 0.1 ⁇ 1.0, and more preferably in a range of 0. 2 ⁇ 0. 8.
  • the ratio is less than 0. 1, sliding property of the lubricative film may be insufficient, while the adhesive performance of the coating layer may be insufficient when the ratio is more than 1. 0.
  • any surface active agent of nonionic, anionic, amphoteric and cationic type may be used.
  • the nonionic surface active agent may include polyoxyethylene alkyl ether, polyoxyalkylene(ethylene and/or propylene) alkyl phenyl ether, polyoxyethylene alkyl ester comprising polyethylene glycol (or ethylene oxide) and higher fatty acid (C12 ⁇ C18, for example), polyoxyethylene sorbitan alkyl ester comprising sorbitan, polyethylene glycol and higher fatty acid (C12 ⁇ C18, for example).
  • the anionic surface active agent may include fatty acid salts, sulfuric acid ester salt, sulfonate salt, phosphoric acid ester salt, and dithiophosphoric acid ester salt.
  • the amphoteric surface active agent may include carboxylates either in amino acid configuration or in betaine configuration, sulfuric acid ester salt, sulfonate salt, phosphoric acid ester salt.
  • the cationic surface active agent may include amine salt of fatty acid, quaternary ammonium salt and the like.
  • Each of these surface active agent may be used either alone or in combination of two or more of them.
  • Aqueous lubricant of the present invention may further be applied as a lubricant for cold working (wire drawing, tube drawing, forging, etc) when the metallic materials of iron and steel, stainless steel, copper or copper alloy, aluminum or aluminum alloy, titanium or titanium alloy are already coated by known process of forming the phosphate layer (zinc phosphate, manganese phosphate, iron phosphate, tin phosphate, etc), oxalte layer (iron oxalate, etc), cryolite and calcium aluminate layer.
  • Shape of the metallic material is not especially limited, and not only bar and block but also shaped product being produced by hot forging (gear, shaft, etc) may be used.
  • a purified surface of the metallic material is made to contact with the aforementioned aqueous lubricant and then dried, and produce the lubricative film of 0.5 ⁇ 40g/m 2 on the surface of the metallic material.
  • the processing of the lubricative film of the invention is non-reactive type.
  • the amount of the lubricative film produced on the surface of the metal may be adjusted according to the degree of deformation of the plastic cold working. And it is more preferable to be in a range of 2 ⁇ 20g/m 2 .
  • the lubricity becomes insufficient.
  • dregs may appear in the working and the cavity provided on the surface of the tool may be crammed by arisen dregs.
  • the amount of the lubricative film may be calculated from the surface area of the metallic material and the weight difference before and after the treatment.
  • treatment solution may be obtained by diluting the concentrated aqueous lubricant by water.
  • the type of the water used for this dilution is not limited, but deionized water or distilled water are preferable.
  • surface cleaning of the metallic material is preferable to be carried out by one or more cleaning step being selected from shot blasting, sand blasting, alkali decreasing and acid cleaning.
  • the main purpose of these cleaning is to remove a oxide scale being grown in the annealing or to remove a contamination of oil or others.
  • waste water may be possible to decrease to zero, for example, by shot blasting for cleaning the surface and by producing the lubricative film using the aqueous lubricant of the invention.
  • aqueous lubricant of the invention there are no specific limitation in the method of applying the aqueous lubricant of the invention to the surface of the metallic material. And dipping method, flow coat method, spray method and other method can be used. The application is sufficient when the surface is sufficiently covered by the aqueous lubricant, and there is no restriction in applying time.
  • the aqueous lubricant is to be dried. Drying may be done by keeping it under the ordinary temperature, and it may also be preferable by keeping it at 60 ⁇ 150°C for 10 ⁇ 60 minutes.
  • the aqueous lubricant is applied after heating the metallic material to 60 ⁇ 100°C in order to increase the drying efficiency. Also, it is preferable to apply the aqueous lubricant after being heated to 50 ⁇ 90°C.
  • drying efficiency may be much improved and the loss of heat energy may be much decreased.
  • Die (1) has an inner surface of the funnel like shape.
  • Rod sample (2) are set on the top of the die (1) as in Fig. 2 (A) , then being pressed and the bottom of the sample (2) are forced to move into the funnel hole of the die (1) as shown in Fig. 2 (B) .
  • spike having the shape corresponding to the funnel are produced.
  • the height of the formed spike are shown as spike height in Table 1. The lubricating is excellent when the spike has a large spike height.
  • Aqueous lubricant 1 as below (containing 1 wt % of nonionic surfactant for dispersion) was used and treated in Process A above.
  • Aqueous lubricant 1 Aqueous lubricant 1
  • Aqueous lubricant 2 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in Process B above.
  • Aqueous lubricant 3 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in Process A above.
  • Aqueous lubricant 4 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in Process A above.
  • Aqueous lubricant 5 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in Process B above.
  • Aqueous lubricant 6 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in Process A above.
  • Aqueous lubricant 7 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in treating process B above.
  • Aqueous lubricant 8 as below was used in treating process A above.
  • Aqueous lubricant 9 as below (containing 1 wt % of nonionic surfactant for dispersion) was used in treating process A above
  • Comparative example 1 where lubricative agent is not contained and comparative example 2 where wax is not contained are inferior in their lubricative properties.
  • comparative example 3 where treatment was carried out in a conventional process of using the chemical conversion layer of phosphate and reactive soap the lubricative property is as excellent as in the present invention.
  • much waste matter may appear from the reaction of chemical conversion, and special complicated equipments become necessary in disposal of waste water and for controlling the aqueous lubricant, and the burden for keeping the environment become increase.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Inorganic Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Lubricants (AREA)

Claims (5)

  1. Lubrifiant aqueux utilisé pour le travail plastique d'une matière métallique qui contient (A) un sel minéral hydrosoluble choisi dans le groupe comportant des sulfate, silicate, borate, molybdate et tungstate, (B) un ou plus d'un agent lubrifiant choisi parmi le disulfure de molybdène et le graphite, et (C) de la cire, ces composants étant dissous ou dispersés dans de l'eau et le rapport en poids (B)/(A) sous forme de matières solides étant dans la gamme de 1,0 à 5,0 et le rapport en poids (C)/(A) sous forme de matières solides étant dans la gamme de 0,1 à 1,0.
  2. Lubrifiant aqueux utilisé pour le travail plastique d'une matière métallique selon la revendication (1), dans lequel la cire est de la cire naturelle ou synthétique dispersée dans l'eau dont le point de fusion va de 70 à 150°C.
  3. Procédé de traitement par film lubrifiant, dans lequel le lubrifiant aqueux selon l'une des revendications (1) à (2) est appliqué sur la surface nettoyée de la matière métallique et séché, et dans lequel le film lubrifiant de 0,5 à 40 g/m2est produit sur la surface de la matière métallique.
  4. Procédé de traitement par film lubrifiant selon la revendication (3), dans lequel la surface nettoyée est obtenue par une ou plus d'une étape de nettoyage choisie dans le groupe comportant le grenaillage, le sablage, le dégraissage alcalin et le nettoyage à l'acide.
  5. Procédé de traitement par film lubrifiant selon l'une quelconque des revendications (3) à (4), dans lequel le lubrifiant aqueux selon l'une quelconque des revendications (1) à (2) est appliqué sur la matière métallique après avoir chauffé la matière métallique à une température de 60 à 100°C.
EP01925970.4A 2000-08-07 2001-04-26 Lubrifiant aqueux pour le travail plastique d'un materiau metallique et procede d'elaboration d'un film lubrifiant Expired - Lifetime EP1319702B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP2000237968 2000-08-07
JP2000237968 2000-08-07
PCT/JP2001/003639 WO2002012419A1 (fr) 2000-08-07 2001-04-26 Lubrifiant aqueux pour le travail au plastique d'un materiau metallique et procede d'elaboration d'un film lubrifiant

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EP1319702A1 EP1319702A1 (fr) 2003-06-18
EP1319702A4 EP1319702A4 (fr) 2004-08-11
EP1319702B1 true EP1319702B1 (fr) 2016-11-09

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US (1) US20030130137A1 (fr)
EP (1) EP1319702B1 (fr)
JP (1) JP3984158B2 (fr)
KR (1) KR100621693B1 (fr)
CN (1) CN1214095C (fr)
CA (1) CA2418942C (fr)
MX (1) MXPA03000789A (fr)
WO (1) WO2002012419A1 (fr)

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CN102092987B (zh) * 2010-12-02 2012-10-10 二重集团（德阳）重型装备股份有限公司 锻件模锻用保温粘接剂及其制备方法
JP5745035B2 (ja) 2011-03-28 2015-07-08 日本パーカライジング株式会社 高潤滑性固体潤滑剤
CN102784983A (zh) * 2011-05-20 2012-11-21 昆山市瑞捷精密模具有限公司 快走丝电火花线切割加工工作液
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JP6694769B2 (ja) 2015-09-30 2020-05-20 株式会社神戸製鋼所 耐食性及び加工後の外観に優れた鋼線材
KR102006129B1 (ko) * 2017-09-21 2019-08-01 재단법인 포항산업과학연구원 스테인레스강 인발 공정 전처리 피막제 및 그 제조 방법
CN108219912B (zh) * 2017-12-30 2023-02-03 常州市奥普泰科光电有限公司 一种水基金属切削液及其制备方法
KR102004352B1 (ko) * 2018-05-30 2019-10-17 김영량 온간 및 열간 단조용 수분산성 윤활제 조성물
CN109609250A (zh) * 2019-01-03 2019-04-12 上海润莱博化工有限公司 一种水溶性金属成型加工工艺润滑剂及其制备方法
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CN112195055B (zh) * 2020-09-30 2022-08-19 郑州机械研究所有限公司 一种药芯铜基钎料丝用拉拔润滑剂、拉拔润滑方法、药芯铜基钎料丝及其应用
CN113210448B (zh) * 2021-05-17 2022-06-03 西北有色金属研究院 一种带润滑涂层的tb9钛合金盘圆丝材冷拉拔制备方法
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EP1319702A4 (fr) 2004-08-11
WO2002012419A1 (fr) 2002-02-14
CA2418942C (fr) 2010-09-14
EP1319702A1 (fr) 2003-06-18
CN1214095C (zh) 2005-08-10
US20030130137A1 (en) 2003-07-10
MXPA03000789A (es) 2004-11-01
CN1468294A (zh) 2004-01-14
KR100621693B1 (ko) 2006-09-08
CA2418942A1 (fr) 2003-02-07
KR20030027002A (ko) 2003-04-03
JP3984158B2 (ja) 2007-10-03

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