EP0321370A1 - Verfahren zur Veränderung des Kühlvermögens von wässrigen Flüssigkeiten zur Härtung von Metall-Legierungen - Google Patents

Verfahren zur Veränderung des Kühlvermögens von wässrigen Flüssigkeiten zur Härtung von Metall-Legierungen Download PDF

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Publication number
EP0321370A1
EP0321370A1 EP19880420422 EP88420422A EP0321370A1 EP 0321370 A1 EP0321370 A1 EP 0321370A1 EP 19880420422 EP19880420422 EP 19880420422 EP 88420422 A EP88420422 A EP 88420422A EP 0321370 A1 EP0321370 A1 EP 0321370A1
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EP
European Patent Office
Prior art keywords
lcst
chosen
water
soluble
solution
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Granted
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EP19880420422
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English (en)
French (fr)
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EP0321370B1 (de
Inventor
François Moreaux
Gérard Beck
Abderrahim Louai
Jeanne Francois
Gilbert Pollet
Jean-Paul Betend
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Servimetal SA
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Servimetal SA
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Priority to AT88420422T priority Critical patent/ATE76104T1/de
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    • CCHEMISTRY; METALLURGY
    • C21METALLURGY OF IRON
    • C21DMODIFYING THE PHYSICAL STRUCTURE OF FERROUS METALS; GENERAL DEVICES FOR HEAT TREATMENT OF FERROUS OR NON-FERROUS METALS OR ALLOYS; MAKING METAL MALLEABLE, e.g. BY DECARBURISATION OR TEMPERING
    • C21D1/00General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering
    • C21D1/56General methods or devices for heat treatment, e.g. annealing, hardening, quenching or tempering characterised by the quenching agents
    • C21D1/60Aqueous agents

Definitions

  • the invention relates to a method for modifying the cooling power of aqueous media intended for the quenching of metal alloys, these media being made up of so-called reverse-soluble water-soluble organic polymers, which precipitate by increasing the temperature. It also relates to aqueous quenching fluids, the cooling power of which can be modified by adding water-soluble additives.
  • the "cloud point" of a polymer solution can be considered as a physical constant of this solution and that it can be determined by measuring the absorption coefficient of light as a function of temperature, through a cell containing this solution. At the point of trouble, there is an abrupt discontinuity in the transmission which spans a few tenths of kelvins.
  • the quenching of a metal part in an aqueous cooling fluid generally comprises three phases. If we take the case of a steel part previously brought to a temperature of about 850 ° C: - the first stage is that of calefaction. The part is surrounded by a vapor sheath that isolates it from the liquid and slows down cooling.
  • This stage may however, depending on the conditions of the operation, not exist or be eliminated by various means well known to specialists.
  • the second stage is that of nucleated boiling, that is to say the formation of vapor bubbles on a large number of points of the part.
  • the third stage corresponds to cooling by conduction and convection, by direct contact between the part and the quenching fluid.
  • each quenching medium and at equal initial temperature of the quenched parts, to draw temperature curves as a function of time and of the cooling rate as a function of time or of temperature (derivative curves) which are called often: "drasticity curves".
  • the quenching medium is selected so as to slow or accelerate the cooling in the zones of high temperature or in the zone below approximately 300 ° C. (critical zone of the martensitic transformation) in which deformation or even "quenching nipples" may occur.
  • this requires a whole range of quenching fluids, each corresponding to a type of alloy.
  • the present invention proposes to solve this problem. It relates to a process for modifying the cooling power of at least one organic polymer with reverse solubility, having a lower critical solubility temperature (usually abbreviated as LCST, Low critical solution temperature) this process being characterized in that one adds to the aqueous solution of said polymer a controlled amount of a water-soluble additive which modifies said critical temperature as the case may be, increasing or decreasing.
  • LCST Low critical solubility temperature
  • These additives are chosen: - among certain water-soluble mineral salts if the LCST is to be reduced; however, some organic compounds also have this property - among certain water-soluble organic compounds, but at the same time relatively hydrophobic, if one wants to increase (or in some cases, decrease) the LCST.
  • These additions are made at doses of between 0 and 200 grams per liter of the quenching medium.
  • Another object of the invention is an aqueous medium for the quenching of metal alloys, comprising at least one water-soluble polymer with reverse solubility, with an LCST point, characterized in that it comprises, in addition, at least one additive intended to modify, in a controlled manner, its LCST point, increasing or decreasing, and thus to model the cooling curve.
  • the invention applies in particular, but not limited to, quenching media based on oxyethylene polymers, oxyethylene and oxypropylene copolymers known under the trade name "EMKAROX” (registered trademark of Imperial Chemical Industries ), in which the propylene oxide (OP) / ethylene oxide (OE) ratio can be between 0 and 1, as well as PVME (polyvinyl methyl ethers), PDME (polydimethoxyethylene) polymers, to name only the main ones.
  • the orders of efficiency of cations, anions and salts are as follows (indicated in the order of decreasing efficiency): - At equal molar concentration: K+, Na+, Ca+, Mg++, Zn++, Li+ B4O7 ⁇ , PO4 ⁇ , CO3 ⁇ , SiO3 ⁇ , SO4 ⁇ , F ⁇ , Cl ⁇ , CH3COO ⁇ , Br ⁇ , ClO3 ⁇ , I ⁇ , Na3PO4, Na2B4O7, Na2CO3, Na2SiO3, K2SO4, MgSO4, ZnSO4, Li2SO4, KF, NaCH3CO2, KCl, NaCl, CaCL2, MgCl2, KBr, KClO3, LiCl, KI.
  • additives will be preferred whose efficiency is greatest so as to limit the salt concentration of the quenching medium to the strict minimum for obvious reasons.
  • Figure 1 embodies all that has just been exposed on the effect of the two groups of additives; we note, moreover, that the cloud point is lowered in a substantially linear manner, by addition of increasing amounts of mineral salts: it appears that the disodium carbonate Na2CO3 has, at equal concentration, an efficiency greater than that of sodium metaborate ( Borax).
  • Borax sodium metaborate
  • Propylene glycol and acetamide raise the cloud point more effectively than their respective lower counterparts, ethylene glycol and formamide, while the effect of potassium iodide is insignificant as previously reported. .
  • Table I gives the characteristics of the solutions used for the drasticity measurements.
  • the basic solution is EMKAROX FC31-165000 at 4% by weight.
  • ADDITIVE Na2CO3 KI Propylene glycol conc. % 0 0.76 1.52 3.04 4 5 10 20 viscosity (cp) 1 1.03 1.06 1.13 0.96 1.2 1.4 1.8 viscosity 3.5 3.4 3.27 3.01 3.46 4.14 4.72 5.9 ⁇ cm.
  • FIG. 2 shows the influence of the additions of sodium carbonate according to Table 1 on the shape of the cooling curves, the initial temperature of the quenched steel part being 850 ° C.
  • This influence which is not very marked in the nucleated boiling zone is amplified in the conduction / convection cooling zone, below 300 ° C. where there is a noticeable reduction in the cooling rate.
  • FIG. 4 which corresponds to the same conditions as FIG. 2, the additive being propylene glycol, shows that the modeling effect of the drasticity curve begins at 850 ° C., with a significant decrease in the cooling rate, and reverses below about 300 ° C.
  • FIG. 10 shows the variations in the cooling rate in the range 25-300 ° C. (approximately) as a function of the cloud point for three temperatures: 100, 150 and 200 ° C. and for several concentrations of disodium carbonate, disodium phosphate, ethylene glycol, propylene glycol and potassium iodide.
  • the present invention provides a solution to the problem of the multiplicity of aqueous quenching fluids required by the treatment of parts made of different alloys or requiring different quenching speeds in particular temperature ranges. It is possible to model the cooling curve at the option of the users, from a single solution of water-soluble polymer, to which a cloud point of a predetermined value can be given. It also allows, on a secondary basis, to correct the effect, on the point of cloudiness of auxiliary additives, such as biocides, defoamers, anticorrosives, etc. Finally, it can temporarily restore the LCST point on solutions which begin to be affected by aging due to prolonged use, for example to complete a series of quenches before the complete renewal of the solution.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Preventing Corrosion Or Incrustation Of Metals (AREA)
  • Heat Treatments In General, Especially Conveying And Cooling (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Heat Treatment Of Strip Materials And Filament Materials (AREA)
  • Lubricants (AREA)
  • Eyeglasses (AREA)
EP88420422A 1987-12-17 1988-12-15 Verfahren zur Veränderung des Kühlvermögens von wässrigen Flüssigkeiten zur Härtung von Metall-Legierungen Expired - Lifetime EP0321370B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
AT88420422T ATE76104T1 (de) 1987-12-17 1988-12-15 Verfahren zur veraenderung des kuehlvermoegens von waessrigen fluessigkeiten zur haertung von metalllegierungen.

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
FR8718109A FR2624875B1 (fr) 1987-12-17 1987-12-17 Procede de modification du pouvoir refroidissant de milieux aqueux destines a la trempe d'alliages metalliques
FR8718109 1987-12-17

Publications (2)

Publication Number Publication Date
EP0321370A1 true EP0321370A1 (de) 1989-06-21
EP0321370B1 EP0321370B1 (de) 1992-05-13

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Family Applications (1)

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EP88420422A Expired - Lifetime EP0321370B1 (de) 1987-12-17 1988-12-15 Verfahren zur Veränderung des Kühlvermögens von wässrigen Flüssigkeiten zur Härtung von Metall-Legierungen

Country Status (7)

Country Link
EP (1) EP0321370B1 (de)
JP (1) JPH0637665B2 (de)
AT (1) ATE76104T1 (de)
DE (1) DE3871106D1 (de)
ES (1) ES2037267T3 (de)
FR (1) FR2624875B1 (de)
GR (1) GR3005214T3 (de)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994026939A1 (en) * 1993-05-18 1994-11-24 Aluminum Company Of America A method of heat treating metal with liquid coolant containing dissolved gas
EP0897995A1 (de) * 1997-07-31 1999-02-24 Mazda Motor Corporation Gussstück aus Leichtmetal, Wärmbehandlungsverfahren
EP0967292A1 (de) * 1998-06-24 1999-12-29 Durferrit SARL Verfahren und Vorrichtung zur Überwachung des Kühlvermögens eines Flüssigkeits
WO2002008137A3 (de) * 2000-07-24 2002-05-30 Henkel Kgaa Teilchenförmiges kompositmaterial zur gesteuerten freisetzung eines wirkstoffs
CN104136634A (zh) * 2012-03-02 2014-11-05 出光兴产株式会社 水系冷却剂
US10633611B2 (en) 2013-03-26 2020-04-28 Sumitomo Seika Chemicals Co., Ltd. Water-soluble metal working oil agent
WO2020178112A1 (de) * 2019-03-01 2020-09-10 Thyssenkrupp Steel Europe Ag Verfahren zur beschleunigten abkühlung von stahlflachprodukten

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP6227248B2 (ja) * 2012-12-27 2017-11-08 出光興産株式会社 水系冷却剤
JP7357535B2 (ja) * 2019-12-17 2023-10-06 三井化学株式会社 アルキレンオキシド重合体の製造方法
JP7422530B2 (ja) * 2019-12-17 2024-01-26 三井化学株式会社 アルキレンオキシド重合体の曇点測定用溶媒

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3022205A (en) * 1958-05-14 1962-02-20 Gen Motors Corp Method of quenching and quenching liquid
US3475232A (en) * 1966-11-23 1969-10-28 Houghton & Co E F Method of quenching
DE3345253A1 (de) * 1982-12-16 1984-07-12 PCUK Produits Chimiques Ugine Kuhlmann, Paris Verfahren zum abschrecken von eisenlegierungen in waesserigem medium
EP0206347A1 (de) * 1985-06-28 1986-12-30 Union Carbide Corporation Abschreckverfahren

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3022205A (en) * 1958-05-14 1962-02-20 Gen Motors Corp Method of quenching and quenching liquid
US3475232A (en) * 1966-11-23 1969-10-28 Houghton & Co E F Method of quenching
DE3345253A1 (de) * 1982-12-16 1984-07-12 PCUK Produits Chimiques Ugine Kuhlmann, Paris Verfahren zum abschrecken von eisenlegierungen in waesserigem medium
EP0206347A1 (de) * 1985-06-28 1986-12-30 Union Carbide Corporation Abschreckverfahren

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
JOURNAL OF POLYMER SCIENCE, vol. 14, no. 10, octobre 1976, pages 2241-2251, John Wiley & Sons, Inc.; E.A. BOUCHER et al.: "Effects of inorganic salts on the properties of aqueous poly(ethylene oxide) solutions" *

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1994026939A1 (en) * 1993-05-18 1994-11-24 Aluminum Company Of America A method of heat treating metal with liquid coolant containing dissolved gas
US5681407A (en) * 1993-05-18 1997-10-28 Aluminum Company Of America Method of heat treating metal with liquid coolant containing dissolved gas
US5820705A (en) * 1993-05-18 1998-10-13 Aluminum Company Of America Spray quenching of metal with liquid coolant containing dissolved gas
US6214136B1 (en) 1997-07-31 2001-04-10 Mazda Motor Corporation Light-alloy casting heat treatment method
EP0897995A1 (de) * 1997-07-31 1999-02-24 Mazda Motor Corporation Gussstück aus Leichtmetal, Wärmbehandlungsverfahren
EP0967292A1 (de) * 1998-06-24 1999-12-29 Durferrit SARL Verfahren und Vorrichtung zur Überwachung des Kühlvermögens eines Flüssigkeits
FR2780508A1 (fr) * 1998-06-24 1999-12-31 Durferrit Sarl Procede et dispositif pour le controle du pouvoir refroidissant d'un fluide
WO2002008137A3 (de) * 2000-07-24 2002-05-30 Henkel Kgaa Teilchenförmiges kompositmaterial zur gesteuerten freisetzung eines wirkstoffs
CN104136634A (zh) * 2012-03-02 2014-11-05 出光兴产株式会社 水系冷却剂
US20150000710A1 (en) * 2012-03-02 2015-01-01 Idemitsu Kosan Co., Ltd. Water-based coolant
EP2821510A4 (de) * 2012-03-02 2015-11-11 Idemitsu Kosan Co Wässriges kühlmittel
US10633611B2 (en) 2013-03-26 2020-04-28 Sumitomo Seika Chemicals Co., Ltd. Water-soluble metal working oil agent
WO2020178112A1 (de) * 2019-03-01 2020-09-10 Thyssenkrupp Steel Europe Ag Verfahren zur beschleunigten abkühlung von stahlflachprodukten

Also Published As

Publication number Publication date
JPH0637665B2 (ja) 1994-05-18
FR2624875B1 (fr) 1992-06-26
ATE76104T1 (de) 1992-05-15
FR2624875A1 (fr) 1989-06-23
ES2037267T3 (es) 1993-06-16
DE3871106D1 (de) 1992-06-17
EP0321370B1 (de) 1992-05-13
JPH01259119A (ja) 1989-10-16
GR3005214T3 (de) 1993-05-24

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