US3408843A - Lubricant-coolant emulsion stabilization and reuse - Google Patents

Lubricant-coolant emulsion stabilization and reuse Download PDF

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Publication number
US3408843A
US3408843A US589730A US58973066A US3408843A US 3408843 A US3408843 A US 3408843A US 589730 A US589730 A US 589730A US 58973066 A US58973066 A US 58973066A US 3408843 A US3408843 A US 3408843A
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United States
Prior art keywords
emulsion
oil
filter
hardness
metal
Prior art date
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US589730A
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English (en)
Inventor
Treat Lyle
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Dow Chemical Co
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Dow Chemical Co
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Priority to DE19661594398 priority Critical patent/DE1594398A1/de
Priority to GB13905/66A priority patent/GB1118224A/en
Application filed by Dow Chemical Co filed Critical Dow Chemical Co
Priority to US589730A priority patent/US3408843A/en
Priority to US589520A priority patent/US3409551A/en
Priority to GR670133300A priority patent/GR33300B/el
Priority to ES335836A priority patent/ES335836A1/es
Priority to DE1594412A priority patent/DE1594412C3/de
Priority to GB3061/67A priority patent/GB1154303A/en
Priority to NL6701434A priority patent/NL6701434A/xx
Priority to FR95076A priority patent/FR1514458A/fr
Priority to SE3197/67A priority patent/SE342471B/xx
Priority to NO167488A priority patent/NO122493B/no
Priority to BE705624D priority patent/BE705624A/xx
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Publication of US3408843A publication Critical patent/US3408843A/en
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    • C10M173/00—Lubricating compositions containing more than 10% water
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21B—ROLLING OF METAL
    • B21B45/00—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills
    • B21B45/02—Devices for surface or other treatment of work, specially combined with or arranged in, or specially adapted for use in connection with, metal-rolling mills for lubricating, cooling, or cleaning
    • B21B45/0239—Lubricating
    • B21B45/0242—Lubricants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B21—MECHANICAL METAL-WORKING WITHOUT ESSENTIALLY REMOVING MATERIAL; PUNCHING METAL
    • B21C—MANUFACTURE OF METAL SHEETS, WIRE, RODS, TUBES, PROFILES OR LIKE SEMI-MANUFACTURED PRODUCTS 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
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    • C10M2217/00—Organic macromolecular compounds containing nitrogen as ingredients in lubricant compositions
    • C10M2217/06—Macromolecular compounds obtained by functionalisation op polymers with a nitrogen containing compound
    • 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/042—Sulfate esters
    • 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
    • C10M2219/00—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions
    • C10M2219/04—Organic non-macromolecular compounds containing sulfur, selenium or tellurium as ingredients in lubricant compositions containing sulfur-to-oxygen bonds, i.e. sulfones, sulfoxides
    • C10M2219/044—Sulfonic acids, Derivatives thereof, e.g. neutral salts
    • 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
    • C10M2227/00—Organic non-macromolecular compounds containing atoms of elements not provided for in groups C10M2203/00, C10M2207/00, C10M2211/00, C10M2215/00, C10M2219/00 or C10M2223/00 as ingredients in lubricant compositions
    • C10M2227/09—Complexes with metals
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/06—Groups 3 or 13
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/22—Metal working with essential removal of material, e.g. cutting, grinding or drilling
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/24—Metal working without essential removal of material, e.g. forming, gorging, drawing, pressing, stamping, rolling or extruding; Punching metal
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/241—Manufacturing joint-less pipes
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/242—Hot working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
    • C10N2040/243—Cold working
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2040/00—Specified use or application for which the lubricating composition is intended
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2040/20—Metal working
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    • C10N2040/245—Soft metals, e.g. aluminum
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
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    • C10N2040/00—Specified use or application for which the lubricating composition is intended
    • C10N2040/20—Metal working
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
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    • C10N2040/20—Metal working
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    • C10N2040/247—Stainless steel
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01—Emulsions, colloids, or micelles
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/015—Dispersions of solid lubricants
    • C10N2050/02—Dispersions of solid lubricants dissolved or suspended in a carrier which subsequently evaporates to leave a lubricant coating
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/10—Form in which the lubricant is applied to the material being lubricated semi-solid; greasy
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2070/00—Specific manufacturing methods for lubricant compositions
    • C10N2070/02—Concentrating of additives
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
    • G01N33/26—Oils; Viscous liquids; Paints; Inks
    • G01N33/28—Oils, i.e. hydrocarbon liquids
    • G01N33/2894—Oils, i.e. hydrocarbon liquids for metal working or machining

Definitions

  • a lubricant-coolant oil-in-water emulsion used in the shaping of a metal is stabilized and kept filterable by periodically adding polycarboxylic acid chelating agent, such as a polyacetic acid, or salt thereof, in the requisite amount to adjust and maintain the hardness level of the emulsion below about 400 ppm.
  • polycarboxylic acid chelating agent such as a polyacetic acid, or salt thereof
  • the hardness level is maintained in the range of about 25 to 400 ppm.
  • the emulsion is also filtered to remove solid particles larger than about 0.5 to microns maximum dimension.
  • the invention relates to the hot or cold working, cutting or other shaping of metal in any operation wherein there is used a flowing lubricant-coolant oil-in-water emulsion which is recycled and reused.
  • the invention also relates to the composition of such emulsions as well as a method for improving such emulsions.
  • aluminum and its alloys containing at least 70 percent by weight of aluminum are hereinafter referred to as aluminum;
  • magnesium and its alloys containing at least 70 percent by weight of magnesium are hereinafter referred to as magnesium;
  • copper and its alloys containing at least 50 percent by weight of copper are hereinafter referred to as copper;
  • iron and its alloys containing at least 75 percent by weight of iron are hereinafter referred to as ferrous metal;
  • the operations of rolling, working, drawing, cutting, milling, scalping, drilling, or grinding and the like of metals are hereinafter referred to variously, as method of shaping a metal, metal shaping, and the like;
  • the phase flowing lubricant-coolant oil-inwater emulsion is intended to encompass such emulsions which are sprayed on the workpiece or tool.
  • the pattern of dis tribution of the emulsion on the work rolls is regulated to control the temperature gradient of the rolls transversely to the work stock and hence the shape of the rolls is controlled.
  • the rate of flow of the emulsion onto the metal being shaped regulates the temperature thereof during the various stages of shaping.
  • the emulsion serves: (1) to control the frictional forces existing between the workpiece and the Work tool; (2) to promote the development of desired tool coatings during the shaping process, e.g., roll-coating during rolling; and (3) to prevent excessive transfer of metal from the workpiece to the tool or from the tool to the workpiece, e.g., between the rolls and the workpiece as in rolling operations.
  • Typical lubricant-coolant oil-in-water emulsions that have been used for metal shaping operations such as rolling or cutting have consisted essentially of from about 0.5 to 20 percent by weight of an oil in water, the oil being a mixture referred to in the trade as neat soluble oil or soluble oil.
  • Such neat soluble oil is widely sold as a concentrate containing, generally, about 70-90 percent by weight of a base oil, such as a light mineral oil, from about 1 to 20 percent by weight, based on said neat soluble oil, of one or more anionic and/or nonionic oil-inwater emulsifying agents and the balance substantially water.
  • the neat soluble oil must also contain from about 0.5 to 15 percent by weight of lubricity additives such as long chain fatty acids and salts or esters thereof, e.g., alkanolamine soaps, or, esters such as butyl stearates which serve as extreme pressure agents.
  • lubricity additives such as long chain fatty acids and salts or esters thereof, e.g., alkanolamine soaps, or, esters such as butyl stearates which serve as extreme pressure agents.
  • emulsions are made up conventionally by admixing one of the commercially available substantially water-free concentrates with water.
  • the commercial concentrates usually contain up to 0.5 percent by weight of a bactericide and from about 0.5 to 5 percent by weight of a coupling agent, i.e., a substance which stabilizes the concentrate during storage prior to use.
  • composition of the neat soluble oil itself forms no part of the present invention.
  • the method and composition of the invention are usable with substantially all of the commonly known and used commercially available neat soluble oils, without modification of the soluble oil per se.
  • Suitable commercial compounded oils i.e., soluble oils
  • soluble oils include, for example, Solvac 1535G, Prosol 44 and Prosol 66 supplied by Socony Mobil Oil Company, Rollex A supplied by the Shell Chemical Company, Majestic #101 supplied by Fiske Brothers Refining Com pany, RolKleen #53 supplied by the D. A. Stuart Oil Company, Ltd., A- supplied by Far Best, W.S. 51821 supplied by the Humble Oil Company and Tandemol C86 and Tandemol K87 supplied by E. F. Houghton and Company.
  • a typical neat soluble oil that is commercially available has the following general composition, by weight:
  • the base oil used in making up a neat soluble oil generally is selected from a light hydrocarbon or light hydrocarbon mixture having a viscosity of about 40 to 200 Saybolt Universal seconds (SUS) at 100 F.
  • SUS Saybolt Universal seconds
  • other lubricious materials such as fatty oils, e.g., palm oil, or synthetic materials, e.g., palm oil substitutes, are also used as a base oil in making up soluble oil.
  • Such other lubricious materials may have viscosities as high as about 850 SUS.
  • base oil is understood to encompass the light hydrocarbon or hydrocarbon mixtures recognized as light mineral oils, in addition to lubricious materials including vegetable oils, such as palm oil, animal fats, such as lard oil, and palm oil substitutes and the equivalents thereof, e.g., polyglycols and ethers and esters ample: (1) alkylaryl sulfonates such as the higher ankylbenzene sulfonates wherein higher alkyl means an alkyl group having at least 8 carbon atoms, e.g., C H C H SO Na; (2) fatty alkyl sulfates such as CH (CH OSO Na; (3) the sulfonated fatty amines such as C11H33 CON (CH )C H SO Na; (4) the alkali metal salts of sulfonated fatty acids; and the like.
  • alkylaryl sulfonates such as the higher ankylbenzene sulfonates wherein higher alkyl means an alkyl group
  • alkanolamine soaps of long chain fatty acids are particularly suitable e.g., the diisopropanolamine, diethanolamine or monoethanolamine salts of oleic acid, palmetic acid or stearic acid, the salts being useful singly or as mixtures.
  • Suitable nonionic oil-in-water emulsifiers include the nonionic ethers such as those derived from alkylphenols and ethylene oxide, e.g., C8HI7C6H4OC2HQ(OC2H4)XOH wherein x has a value of 9 to 14 or more, the primary alcohol-ethylene oxide adducts, and the secondary alcohol-ethylene oxide adducts.
  • the metal surface obtained in metal shaping operations is improved after several days of using the emulsion.
  • the emulsion ordinarily accumulates solid particulate matter including metal fines, metal oxide particles, oxidized oils, soil particles and general air-borne industrial contamination.
  • hydraulic oils and bearing lubricants occasionally enter the emulsion as a result of accidental leakage and are collectively referred to as tramp oil.
  • tramp oil As a result of such contamination and also as a result of general use of the emulsion the emulsion begins to break and the droplets of the oil phase agglomerate into larger droplets some of which coalesce sufficiently to provide a substantial quantity of continuous free oil phase.
  • an emulsion which contains no more than about 0.2 percent by weight of continuous free oil phase is considered to be free of such free oil phase.
  • Typical industrial emulsion systems vary in size from perhaps 5,000 to 10,000 gallons or less for smaller cutting or grinding operations to systems as large as 100,000 to 500,000 gallons for large rolling mills, some of which require the circulation of 1,000 to 10,000 gallons of emulsion per minute to one or more mill stands.
  • Another object of the invention is to provide a method of stabilizing and reusing a lubricant-coolant oil-in-water emulsion in metal shaping operations.
  • Another object of the invention is to provide a method of removing particulate matter and eliminating or reducing continuous free oil phase from lubricant-coolant'oilin-water emulsion, apart from a normal level of about 0.2 percent by weight of such oil phase, which is not detrimental in effect.
  • a further object of the invention is to provide a method of increasing the service life of lubricant-coolant oil-inwater emulsions used in the shaping of metal.
  • Yet another object of the invention is to provide an improved lubricant-coolant oil-in-water emulsion for use in metal shaping operations.
  • a conventional rolling or cutting oil emulsion is improved by the addition thereto of an alkaline alkali metal or ammonium or'amine salt of a polycarboxylic acid ehelating agent in'an amount sufiicient to chelate calcium, magnesium, aluminum, heavy metal or other polyvalent metal ions present or accumulating in such an emulsionwhereby the hardness content, expressed as CaCO is reduced below about 400 p.p.m., and the emulsion pH is brought into the range of about 5 to 11. Where foaming is a problem it is much preferred to bring the hardness content to about 25 to 400 p.p.m.
  • the maintenance of a controlled level of hardness content below about 400 ppm, expressed as CaCO and a pH in the range of about 5 to about 11 is essential.
  • Such management of the emulsion substantially prevents oil separation therefrom and has the following further important effects: (a) the emulsion is stabilized so that it can be filtered through a mechanical filter capable of removing solid particulate matter larger than 10 to 20 microns size, and preferably, larger than .1 micron, such as a filter provided with a siliceous precoating; (b) solid'particulate contam' ination such as dirt, metal fines, and metal oxide particles are readily removed on the filter without premature filter blank off problems; (c) light viscosity tramp oils leaking into the system are substantially emulsified thus minimizing the quantity of free oil phase; and (d) oxidized oils and reaction products thereof are removed on filtration.
  • a mechanical filter capable of removing solid particulate matter larger than 10 to 20 microns size, and preferably, larger than
  • An important aspect of the present invention is the discovery that the particle diameter of the globules of emulsified oil is at least partly a function both of pH and hardness content of the emulsion, the nature and concentration of the emulsifying materials present being also controlling factors.
  • This role of hardness had not been appreciated heretofore.
  • Both calcium and magnesium hardness are generally derived in part from the water used to' make up the emulsion. Large quantities of water are frequently and periodically added in many metal shaping operations to replace losses due to evaporation bringing about the addition of substantial amounts of calcium and magnesium hardness. Calcium, and to some extent magnesium ions, also enter the emulsion from concrete mill pits or sumps and storage tanks in which the emulsion is received or stored.
  • the work piece employed is a substantial source of magnesium and/or calcium and/or aluminum ions. These appear to be the main sources which provide for a build-up of hardness content in the emulsion, particularly calcium and magnesium, as the emulsion is recycled and reused.
  • foaming of the emulsion during pumping and spraying operations tends to be a problem in most operations when the hardness level falls too low.
  • foaming tends to be excessive and undesired
  • a hardness level in the range of 100 to 200 p.p.m. expressed as CaCO is preferred; where foaming is less of a problem, a hardness level in the range of 25 to 100 p.p.m. is preferred.
  • the metals which may be rolled or shaped according to the present invention include aluminum, copper, ferrous metal, such as steel, and magnesium. These metals may be shaped cold, or at temperatures as high as about 1050 F., using the emulsion of the invention.
  • the chelating agents used in the method of this invention are the alkali metal or ammonium or amine salts of polycarboxylic acids, including citric acids, tartaric acid, the alkylene amino polyacetic acids, and mixtures of any of the said salts of such polycarboxylic acids.
  • the alkylene amino polyacetic acids include ethylenediaminetetraacetic acid and its well-known homologs and analogs such as N-hydroxyethylenediaminetriacetic acid, diethylenetriaminepentaacetic acid, nitrilotriacetic acid, N-2-hydroxyethyliminodiacetic acid, cyclohexanediaminetetraacetic acid and their obvious equivalents.
  • the amine salts r a flowing stream of said emulsion comprises:
  • the reused emulsion is further characterized by having a pH in the range of about 5 to about 11, but preferably 7 to 10, by the dispersed oil being in the form of globules having an average globule diameter in the range of about 1 to 25 microns and substantially no globules having a diameter exceeding about 50 microns, by a preselected globule diameter being readily maintainable, by the emulsion being readily filterable through a mechanical filter capable of rem( ling solid particles larger than 10 to 20 microns size but preferably particles larger than 0.5 to 1 micron, and by the emulsion being (1) substantially free of solid particles larger than about 10 to 20 microns but preferably no larger than 0.5 to 1 micron and (2) free of more than about 0.2 percent of a free oil phase.
  • the reused emulsion is a tight emulsion designed for reversing mill work and cutting operation, for example, the reused emulsion is also further characterized by the dispersed base oil being in the form of globules having an average globule diameter in the range of about 1 to 2 microns and substantially no globules having a diameter exceeding about 5 microns.
  • the dispersed oil phase is in the form of globules having an average globule diameter in the range of about 2 to 5 microns with substantially no globules larger than about microns.
  • the dispersed oil phase is often in the form of globules having an average globule diameter in the range of about 5 to microns with substantially no globules larger than about 50 microns diameter.
  • Each of tight, loose and coarse emulsions are readily filterable when treated and maintained according to the invention.
  • An important aspect of the invention is the provision for maintenance and control of globule diameters while avoiding emulsion breakage. Even the normally metastable emulsions are maintainable.
  • Tight emulsions are obtained and maintained upon pumping, mixing or otherwise thoroughly agitating the emulsion and further filtering the emulsion under conditions in which the concentration of unchelated hardness is below about 100 p.p.m.
  • Coarse emulsions tend to arise and be maintained under conditions wherein the amount of unchelated hardness is substantially above 200 parts per million.
  • the basic tendency of the emulsion to exhibit fine or coarse globules is dependent upon the materials used to make up the compounded soluble oil concentrate. It is to be understood that making up and maintaining an emulsion according to the present invention provides an effect that is superimposed upon the basic nature of the preselected emulsion.
  • the emulsion size moves to a dynamically stable size and is controllably maintainable at such dynamically stable size using the composition and method ofthe invention, i.e., upon maintaining the unchelated hardness below about 400 p.p.m. and the pH in the range of 5 to 11, a soluble oil emulsionwill reach a dynamically stable globule size averaging about 1 to microns diameter with substantially no globules larger than 50 microns diameter.
  • an emulsion is made up generally from water and a commercial neat soluble oil of the type described hereinabove. If desired, the emulsion may be made up from the individual components.
  • the alkali metal or ammonium or amine salt of polycarboxylic acid chelating agent used according to the invention is added to the water employed in making up the emulsion or the chelating agent may be added to the diluted emulsion in any convenient form, i.e., as a solution, slurry, or dry particulate solid.
  • the chelating agent usually in the form of a 20 to percent by weight aqueous alkaline solution, is added in the requisite amount to bring the hardness level and the pH into the ranges indicated hereinabove.
  • the water employed or the finished emulsion is analyzed in order to determine the needed quantity of chelating agent solution.
  • the completed emulsion is then placed in service in metal shaping operations.
  • clean emulsion is circulated from clean storage to the workpiece where it is used.
  • the emulsion flowing off the workpiece and off the tool or mill is collected as in a sump where some of the particulate matter present settles out.
  • the emulsion may be allowed to settle further in a system with a large inventory of emulsion, but in general, the emulsion is more or less in constant circulation.
  • a brief quiet period in a dirty" tank is advantageous in the collection and removal of tramp oils before subsequent filtration.
  • the emulsion is sampled for analysis, and hardness level and pH are adjusted by the addition of the indicated requirements of alkaline solution of chelating agent.
  • the emulsion is then pumped to clean storage; if desired, the addition of chelating agent solution may be made to the emulsion in the clean storage vessel.
  • the emulsion after settling in dirty storage is filtered before sampling, adjusting the hardness and pH levels, and pumping to clean storage.
  • Filtering is conveniently and effectively carried out with most any mechanical filter, such as one employing a filter paper or membrane, and especially a filter using a precoat of a siliceous material such as diatomaceous earth.
  • the filter must be capable of removing fine particulate matter, preferably all matter coarser than one micron size.
  • the clean emulsion remains in clean storage until use when the cycle commences again with the pumping of the lubricant-coolant emulsion to the metal shaping operation. Normally, the retention in clean storage is brief, being of the order of 5 to 30 minutes unless a very large inventory of emulsion is used.
  • Lubricantcoolant emulsion so-handled and maintained remains stable and usable throughout many, many cycles completed during the space of from several months to several years and usually during at least 6 months or more of steady use.
  • EXAMPLE 1 This example will best be understood with reference to the accompanying drawing on which there is depicted a schematic flow diagram for an 18,000 gallon emulsion system.
  • the reference numeral 1 refers generally to an 84inch wide 4-high reversing hot mill.
  • 5,000-pound slabs of aluminum ingot (not shown) were rolled from an initial thickness of approximately 14 inches to various gauges down to a final gauge less than about inch thick, the metal at the final pass having the form of either sheet or plate.
  • Product from this mill must be suitable either as a final product, or as re-roll stock to be further processed before use.
  • a flood lubricant-coolant emulsion as described above, was applied to the workrolls through a system of spray-nozzles (not shown).
  • the relative distribution of coolant across the width of the rolls was regulated by adjusting the flow through the various nozzles provided.
  • the emulsion temperature was in the preferred 120-l30 F. range as it is initially on the mill rolls.
  • Sump pumps 4 then carried the lubricant-coolant emulsion to a 12,000 gallon storage tank 5 which is divided into a 4,000 gallon clean compartment 6, and an 8,000 gallon dirty compartment 7. From the sump, the emulsion was directed first to dirty compartment 7. From there it was pumped through a mechanical filter 8 precoated with Celite 545 diatomaceous earth, and returned to the clean compartment 6.
  • the filter has a capacity of 1,500 gallons per trninute, a rate that is faster than the normal milldemand rate. Therefore, while the clean and dirty compartments of the storage tank communicate with each other, normally the flow not needed in the metal shaping operations was directed from the clean compartment 6 to the dirty compartment 7.
  • a secondary coarse strainer filter 9 was provided in the system to remove particles large enough to clog the spray nozzles used at the mill. From the clean compartment 6 the coolant ordinarily flowed through such secondary filter 9 on its way to the mill.
  • the mechanical filter was a tube-type filter, containing about 750 tubes of woven Monel-wire mesh. Each tube was l-inch in diameter and 3 feet long. The wire diameter was 0.011 inch. The mesh openings have maximum dimensions of 0.006 inch to 0.008 inch while the average openings are 0.004 inch x 0.006 inch.
  • the filter tubes were precoated with Celite 545 diatomaceous earth, a filter aid of which about percent of the particles are finer than about 40 microns.
  • the precoat or filter cake formed on each tube retained solids greater than one micron in diameter.
  • the precoat was introduced into the suction side of the filter pump 10 from a 150 gallon tank 11 in the form of a suspension containing pounds of filter aid and the balance water. One-half of the contents of this tank were used to precoat the filter; thus 50 pounds of filter aid formed the initial cake.
  • the porosity of the filter was controlled during the useful life of the filter cake by periodic controlled additions of filter aid, as well understood in the art.
  • body feed which consisted ofabout 50 pounds of filter aid and the balance being 300 gallons of water. Normally, body feed was metered in during approximately three seconds out of each trninute at a rate sufficient to provide about 50 pounds of filter aid during each 24-hour period. In addition to the original 50 pound precoat, the filter can handle an additional 200 pounds of body feed. Thus, under normal operating conditions, about five days of filter operation were attainable between back-washes. When an unusual condition occurred, such as excessive leakage of tramp oils into the system, or greater dirt load from rolling certain alloys; a faster rate of body feed was employed to avoid excessive pressuredrop build-up across the filter. In this case, the cycle between backwashes was shortened.
  • the back-wash operation requires about 35 minutes.
  • coolant from the filter vessel was discharged into the 1,500 gallon recovery storage tank 13.
  • the entire recovery filter cycle takes about 7 hours. Filtration of the back-wash to retain used filter aid solids for waste disposed was accomplished advantageously by making use of a cloth-type filter or equivalent (not shown).
  • Samples for analytical control were removed after the final filtering just before the lubricant-coolant emulsion was pumped to the mill.
  • the composition of the lubricant-coolant emulsion was maintained in the following manner.
  • the oil phase of the emulsion consisted of 4.5 to 6.0 weight percent of a light oil, having a viscosity, at 100 F., of 100-200 SUS, emulsified in water with one or more anionic and/or non-ionic emulsifiers as described above.
  • the emulsion was made up with water.
  • an aqueous solution of an alkaline chelant was added to the resulting emulsion.
  • the quantity of such alkaline chelating agent used was such as to bring the hardness of the aqueous phase of the emulsion within a range of 100-200 p.p.m., expressed as CaCO and the pH within a range of 9 to 10, to give the emulsion the desired properties of stability and lubricity. When the hardnessof the emulsion approached 200 p.p.m., more chelating agent was added.
  • Percent soluble oz'L-This test gives the concentration of oil in the emulsion. The concentration is determined by breaking a sample of the emulsion with acid, centrifuging the broken emulsion, and measuring the oil layer. Adjustment of the oil concentration to the desired range is accomplished by the addition of neat soluble oil or de-ionized water.
  • Hardness The concentration of polyva'lent metal ions, such as magnesium, calcium, and aluminum ions, was maintained in the range of 100-200 p.p.m., expressed as calcium carbonate. Additions of chelant salt were made to prevent build-up above this range. Addition of hard make-up water was employed to increase hardness on a few occasions when the hardness fell below the desired range.
  • polyva'lent metal ions such as magnesium, calcium, and aluminum ions
  • Filter time This test measures the time for one gallon of warm lubricant-coolant emulsion to pass through a double thickness of Whatman No. 30 filter paper, 7 centimeters in diameter, under suction. Acceptable range is 5-8 minutes, at a 10 pounds per square inchdilferential pressure (absolute)- Higher values may indicate malfunction of the filter leading to excessive dirt build-up, 'or it may indicate low chelant salt and/ or high tramp oil concentration.
  • pH-Lub'ricant-coolant sample is'diluted to 1 percent and tested with a pH meter.
  • the pH is inherently maintained in the range of 9 to 10 by the periodic addition of alkaline chelant salt.
  • Example 3 The procedure of Example 1 was followed for a large number of successive mill passes. Some of each of aluminum plate and coil and magnesium plate and coil were rolled interchangeably on the same mill over a period of 15 months.
  • the hardness of the lubricant emulsion gradually increased periodically to about 250 p.p.m., calculated as CaCO Each time the hardness reachedsuch a level of concentration, about 15 gallons of aqueous 38 percent tetrasodium salt of ethylenediaminetetraacetic acid was added to the emulsion to bring the hardness level down to about to 100 p.p.m., expressed as CaCO In each instance the hardness level was reduced so as to maintain hardness within the range of about 100-200 p.p.m., expressed as CaCO Occasionally a 55-gallon drum of soluble oil concentrate containing emulsifying agent was added to the emulsion to make up for base oil taken out by the filter and especially for accidental spillage or sewerage of the emulsion. Water losses due
  • the emulsion was filtered using the filter and precoat described in Example 1. During periods of active use, the emulsion was filtered steadily during transfer from the dirty compartment 7 to the clean compartment 6. During such times the filter was back-washed and recoated about every 48 hours.
  • the emulsion flooding the rolls and cascading over the sheet metal is collected in an underlying sump, pumped to dirty storage, then filtered through a precoated mechanical filter employing a siliceous material for precoating and capable of removing solid particulate matter larger than 1 micron size.
  • the filtered emulsion is collected in clean storage and is again promptly reused in the mill.
  • the emulsion being pumped to the filter is sampled, analyzed, and the requisite additions of the sodium salt of nitrilotriacetic acid are made to maintain the pH of the emulsion in the range of 8.5 to 9.5 andthe hardness content of the emulsion in the range of 100 to 200 p.p.m., expressed as CaCO
  • additions of water and of neat soluble oil are made to compensate for losses by evaporation and drag-out.
  • Periodic tests show that the oil globule sizes in the emulsion remain stable at an average size of about 15 microns diameter with substantially no globules larger than 40 microns diameter.
  • the emulsion remains stable and substantially free of continuous free oil phase, the oil globule sizes remain stable at about 15 microns diameter, the sheet steel is satisfactorily reduced in thickness in the rolls and the surface of the rolled metal is 12 p smooth and bright and substantially free of surface im perfections.
  • EXAMPLE 5 Cold rolling of brass is carried out on each of a 2-high reversing breakdown mill, a 2-high rundown mill, and a 4-stand tandem finish mill. In typical operations, continuous cast 26 inch wide fiat brass bars each weighing about 3,000 pounds are cold rolled from 3.25 inch thickness to 0.540 inch gauge flat plate on the breakdown mill. Nine passes and two intermediate anneals are required to accomplish the reduction in thickness. The rolls and workpieces are lubricated by a flow and spray application of 800 gallons per minute of a recirculating, filtered, lubricant-cooled oil-in-water emulsion from a system containing 16,000 gallons of emulsion.
  • the emulsion has a neat soluble oil concentration of about 12 percent by weight, average oil globule diameters of about 1 to 2 microns, a hardness content of to 200 p.p.m., expressed as CaCO and a pH of about 7.8 to 8.5. Hardness and pH are maintained by periodic additions of the trisodium salt of nitrolotriacetic acid to the emulsion. Overhauling (scalping) removes any stain that develops on the rolled plate.
  • brass strip is rolled from 0.500 to 0.102 inch thick without annealing.
  • strip is rolled from 0.102 inch thickness to 0.012 inch gauge with intermediate annenals as necessary.
  • the workpieces and the rolls of each mill are cooled and lubricated with 650 gallons per minute of a recirculating, filtered lubricant-coolant oil-in-water emulsion from a common system holding 20,000 gallons of emulsion.
  • the emulsion has a neat soluble oil concentration of about 7 percent, an average oil globule diameter in the range of about 5 microns, a hardness content maintained in the range of 25 to 75 p.p.m., expressedas CaCO and a pH of about 7.3 to 7.8.
  • the emulsion is made up from the soluble oil Prosol 66, supplied by Socony Mobil Vacuum Company, Prosol 66 soluble oil is low in sulfur compounds and is non-staining of copper and copper alloys. Hardness and pH are maintained by periodic additions to the system of the tetramonium salt of ethylenediaminetetraacetic acid. Routine losses of emulsion are made up adding new emulsion to the system.
  • the sodium, potassium, ammonium, and amine salts of each of ethylenediaminetetraacetic acid, N-hydroxyethylethylenediaminetriacetic acid, N 2 hydroxyethyliminodiacetic acid, diethylenetriaminepentaacetic acid, nitrilotriacetic acid and cyclohexanediaminetetraacetic acid are useful in controlling and maintaining oil-in-water lubricant-coolant emulsions employed in metal shaping operations including rolling, working, drawing, cutting, milling, scalping, drilling, machining and grinding of magnesium, aluminum, copper and ferrous metal.
  • the emulsions managed and reused according to the invention, including fine filtering are further characterized by surprisingly low ion concentrations of metals such as aluminum, iron and silicon, the ion concentrations, respectively, remaining generally below about 1 to 30 ppm.
  • metals such as aluminum, iron and silicon
  • metal surfaces in continuous or repeated contact with the present treated emulsions seem to become passivated toward the emulsions so that there is little metal ion uptake.
  • the chelating agents employed tie up substantial proportions of metal ions in the emulsions which would otherwise react with metal surfaces to provide molecular hydrogen.
  • Molecular hydrogen which has a powerful catalytic effect on the growth of anaerobic bacteria, is largely avoided.
  • initial bacterial growth is largely filtered out so that colonies are not readily established. Removal of metal fines by filtration also removes metal fines which would otherwise contribute to the electrochemical action which provides the undesired molecular hydrogen.
  • a chelant selected from the group consisting of alkali metal salts, ammonium salts and amine salts of a polycarboxylic acid chelating agent
  • the method as in claim 1 which includes the further steps of periodically sampling and. analyzing the emulsion for hardness and pH, and adding chelant in the requisite amount to maintain each of the hardness level of the aqueous phase and the pH value within the said ranges.
  • the shaping method is rolling and the emulsion comprises (1) from about 2 to about 15 percent by weight of neat soluble oil, (2) spent chelant, the chelant being combined with polyvalent metal ions, (3) from about 25 to 400 p.p.m. of unchelated hardness, expressed as CaCO and (4) the balance substantially water, and the further steps which comprise:

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US589730A 1965-03-29 1966-10-26 Lubricant-coolant emulsion stabilization and reuse Expired - Lifetime US3408843A (en)

Priority Applications (13)

Application Number Priority Date Filing Date Title
DE19661594398 DE1594398A1 (de) 1965-03-29 1966-01-26 Gleitmittelstabilisierung zur Rueckgewinnung beim Walzen von Aluminium und dessen Legierungen
GB13905/66A GB1118224A (en) 1965-03-29 1966-03-29 Lubricant stabilization of recovery in the rolling of aluminum and its alloys
US589730A US3408843A (en) 1965-03-29 1966-10-26 Lubricant-coolant emulsion stabilization and reuse
US589520A US3409551A (en) 1965-03-29 1966-10-26 Lubricant-coolant emulsion
GR670133300A GR33300B (el) 1966-10-26 1967-01-13 Γαλακτωμα λιπανσεως - ψυξεως.
DE1594412A DE1594412C3 (de) 1965-03-29 1967-01-19 Öl-in-Wasser-Emulsion
ES335836A ES335836A1 (es) 1965-03-29 1967-01-19 Un metodo para preparar una emulsion lubricante y refrige- rante de aceite en agua.
GB3061/67A GB1154303A (en) 1965-03-29 1967-01-20 Lubricant-Coolant Emulsion
NL6701434A NL6701434A (enrdf_load_stackoverflow) 1965-03-29 1967-01-30
FR95076A FR1514458A (fr) 1965-03-29 1967-02-15 Emulsions lubrifiant-réfrigérant utilisées dans le laminage ou d'autres procédés de mise en forme des métaux
SE3197/67A SE342471B (enrdf_load_stackoverflow) 1965-03-29 1967-03-08
NO167488A NO122493B (enrdf_load_stackoverflow) 1965-03-29 1967-03-29
BE705624D BE705624A (enrdf_load_stackoverflow) 1965-03-29 1967-10-25

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US589730A US3408843A (en) 1965-03-29 1966-10-26 Lubricant-coolant emulsion stabilization and reuse
US589520A US3409551A (en) 1965-03-29 1966-10-26 Lubricant-coolant emulsion

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BE (1) BE705624A (enrdf_load_stackoverflow)
DE (2) DE1594398A1 (enrdf_load_stackoverflow)
ES (1) ES335836A1 (enrdf_load_stackoverflow)
FR (1) FR1514458A (enrdf_load_stackoverflow)
GB (2) GB1118224A (enrdf_load_stackoverflow)
NL (1) NL6701434A (enrdf_load_stackoverflow)
NO (1) NO122493B (enrdf_load_stackoverflow)
SE (1) SE342471B (enrdf_load_stackoverflow)

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US3568834A (en) * 1969-11-05 1971-03-09 Dow Chemical Co Filtering alkaline metal cleaner
US3756052A (en) * 1971-12-27 1973-09-04 Dow Corning Metal working lubricant
FR2219800A1 (enrdf_load_stackoverflow) * 1973-03-02 1974-09-27 Ici Ltd
US3846319A (en) * 1973-03-27 1974-11-05 Chevron Res Dioxan-containing aluminum lubricant
US4027512A (en) * 1976-05-04 1977-06-07 The Dow Chemical Company Lubricant-coolant emulsion additive for metal working operations
DE2732142A1 (de) * 1977-07-15 1979-01-18 Dow Chemical Co Zusatzstoff fuer eine schmiermittel- kuehlmittel-emulsion
US4199381A (en) * 1977-08-16 1980-04-22 Oxy Metal Industries Corporation Preparation of metals for cold forming
US4202193A (en) * 1978-10-03 1980-05-13 National Steel Corporation Apparatus for controlling the concentration and stability of an emulsion
EP0019670A1 (en) * 1979-05-23 1980-12-10 Glyco Chemicals, Inc. Antimicrobial compositions, method of inhibiting the growth of microorganisms and metal working fluid compositions containing these antimicrobial compositions
US4377487A (en) * 1978-10-31 1983-03-22 Occidental Chemical Corporation Metal coating process and compositions
EP0113863A3 (en) * 1982-12-22 1986-02-12 Merck Patent Gesellschaft Mit Beschrankter Haftung Cutting oil for non-ferro metal working without removal of chips
US4784795A (en) * 1984-12-24 1988-11-15 Dow Corning Gmbh Lubricant composition for water fittings
EP0332788A1 (fr) * 1988-03-17 1989-09-20 Societe Des Ceramiques Techniques Procédé de traitement des émulsions ou des microémulsions d'huile dans l'eau poluées
FR2628749A1 (fr) * 1988-03-17 1989-09-22 Alsthom Cgee Procede de traitement des emulsions ou des microemulsions d'huile dans l'eau polluees
US20040204326A1 (en) * 2003-04-08 2004-10-14 Crompton Corporation Anti-oxidants in soluble oil base for metal working fluids
US20070048343A1 (en) * 2005-08-26 2007-03-01 Honeywell International Inc. Biocidal premixtures
US9570880B2 (en) 1998-11-25 2017-02-14 Imra America, Inc. Multi-mode fiber amplifier
US20230311221A1 (en) * 2020-09-16 2023-10-05 Illinois Tool Works Inc. Standpipe recirculation systems for material removal machines
US12403539B2 (en) * 2020-09-16 2025-09-02 Illinois Tool Works Inc. Standpipe recirculation systems for material removal machines

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GB1325851A (en) * 1971-01-13 1973-08-08 Alcan Res & Dev Process for control of lubricants in an aluminium rolling mill
US3750847A (en) * 1972-05-03 1973-08-07 Master Chemical Corp Method of supplying an aqueous cutting fluid to machine tools
US4098929A (en) 1973-11-12 1978-07-04 Chrysler Corporation Method for improved parting from hot surfaces
BE857770A (fr) * 1976-09-01 1978-02-13 Nat Res Lab Composition stabilisee de fluide pour le travail des metaux et son obtention
JPS5841083B2 (ja) * 1978-10-05 1983-09-09 日産自動車株式会社 水溶性切削剤の再生方法
US5415490A (en) * 1993-07-13 1995-05-16 Flory; John F. Rope termination with constant-cross-section, divided-cavity potted socket
US5795400A (en) * 1994-05-16 1998-08-18 Berger; Mitchell H. Method for recycling coolant for a cutting machine
JP4746300B2 (ja) * 2004-10-01 2011-08-10 株式会社ニクニ 濾過方法および濾過装置
WO2011117892A2 (en) 2010-03-25 2011-09-29 Indian Oil Corporation Ltd. Composition of oil for high speed thin and thick gauge steel sheet rolling in tandem mills
DE102011090098A1 (de) * 2011-12-29 2013-07-04 Sms Siemag Ag Verfahren und Vorrichtung zum Walzen von Walzgut sowie Verwendung eines Kühlschmierstoffes
CN109201757A (zh) * 2018-09-30 2019-01-15 泰安市国士环保科技有限公司 一种轧钢废油的处理方法
CN110257154B (zh) * 2019-05-30 2022-08-02 山西太钢不锈钢股份有限公司 轧制润滑液基础油的制备方法
CN118616695B (zh) * 2024-08-12 2024-10-11 贵州贵铝新材料股份有限公司 一种铝合金加工用循环冷却水自动控制系统

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US2264103A (en) * 1936-06-06 1941-11-25 Procter & Gamble Process and product for softening hard water
US2432784A (en) * 1945-12-07 1947-12-16 Harold F Miller Lubricating and cooling compound for cold reducing mills
US2631978A (en) * 1949-05-13 1953-03-17 Frederick C Bersworth Metalworking lubricant solution
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Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3568834A (en) * 1969-11-05 1971-03-09 Dow Chemical Co Filtering alkaline metal cleaner
US3756052A (en) * 1971-12-27 1973-09-04 Dow Corning Metal working lubricant
FR2219800A1 (enrdf_load_stackoverflow) * 1973-03-02 1974-09-27 Ici Ltd
US3846319A (en) * 1973-03-27 1974-11-05 Chevron Res Dioxan-containing aluminum lubricant
US4027512A (en) * 1976-05-04 1977-06-07 The Dow Chemical Company Lubricant-coolant emulsion additive for metal working operations
DE2732142A1 (de) * 1977-07-15 1979-01-18 Dow Chemical Co Zusatzstoff fuer eine schmiermittel- kuehlmittel-emulsion
US4199381A (en) * 1977-08-16 1980-04-22 Oxy Metal Industries Corporation Preparation of metals for cold forming
US4202193A (en) * 1978-10-03 1980-05-13 National Steel Corporation Apparatus for controlling the concentration and stability of an emulsion
US4377487A (en) * 1978-10-31 1983-03-22 Occidental Chemical Corporation Metal coating process and compositions
EP0019670A1 (en) * 1979-05-23 1980-12-10 Glyco Chemicals, Inc. Antimicrobial compositions, method of inhibiting the growth of microorganisms and metal working fluid compositions containing these antimicrobial compositions
EP0113863A3 (en) * 1982-12-22 1986-02-12 Merck Patent Gesellschaft Mit Beschrankter Haftung Cutting oil for non-ferro metal working without removal of chips
US4784795A (en) * 1984-12-24 1988-11-15 Dow Corning Gmbh Lubricant composition for water fittings
EP0332788A1 (fr) * 1988-03-17 1989-09-20 Societe Des Ceramiques Techniques Procédé de traitement des émulsions ou des microémulsions d'huile dans l'eau poluées
FR2628749A1 (fr) * 1988-03-17 1989-09-22 Alsthom Cgee Procede de traitement des emulsions ou des microemulsions d'huile dans l'eau polluees
US9570880B2 (en) 1998-11-25 2017-02-14 Imra America, Inc. Multi-mode fiber amplifier
US9595802B2 (en) 1998-11-25 2017-03-14 Imra America, Inc. Multi-mode fiber amplifier
US20040204326A1 (en) * 2003-04-08 2004-10-14 Crompton Corporation Anti-oxidants in soluble oil base for metal working fluids
US7569526B2 (en) 2003-04-08 2009-08-04 Crompton Corporation Anti-oxidants in soluble oil base for metal working fluids
US20070048343A1 (en) * 2005-08-26 2007-03-01 Honeywell International Inc. Biocidal premixtures
WO2007025272A3 (en) * 2005-08-26 2007-08-30 Honeywell Int Inc Biocidal premixtures
US20230311221A1 (en) * 2020-09-16 2023-10-05 Illinois Tool Works Inc. Standpipe recirculation systems for material removal machines
US12403539B2 (en) * 2020-09-16 2025-09-02 Illinois Tool Works Inc. Standpipe recirculation systems for material removal machines

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US3409551A (en) 1968-11-05
GB1154303A (en) 1969-06-04
DE1594412B2 (de) 1973-06-20
NO122493B (enrdf_load_stackoverflow) 1971-07-05
BE705624A (enrdf_load_stackoverflow) 1968-04-25
FR1514458A (fr) 1968-02-23
NL6701434A (enrdf_load_stackoverflow) 1968-04-29
SE342471B (enrdf_load_stackoverflow) 1972-02-07
ES335836A1 (es) 1968-03-16
DE1594412A1 (de) 1970-11-05
GB1118224A (en) 1968-06-26
DE1594412C3 (de) 1979-05-10
DE1594398A1 (de) 1970-08-06

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