EP0451160B1 - Purification of industrial lubricating agents - Google Patents

Purification of industrial lubricating agents Download PDF

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Publication number
EP0451160B1
EP0451160B1 EP89912680A EP89912680A EP0451160B1 EP 0451160 B1 EP0451160 B1 EP 0451160B1 EP 89912680 A EP89912680 A EP 89912680A EP 89912680 A EP89912680 A EP 89912680A EP 0451160 B1 EP0451160 B1 EP 0451160B1
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EP
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Prior art keywords
phase
polymer
lubricating
cutting
polymeric
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EP89912680A
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German (de)
English (en)
French (fr)
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EP0451160A1 (en
Inventor
Gunnar STRÖM
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Alfa Laval Separation AB
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KEMISK SEPARERING TUMBA AB
KEMISK SEPARERING TUMBA AKTIEB
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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
    • C10M175/00—Working-up used lubricants to recover useful products ; Cleaning
    • C10M175/04—Working-up used lubricants to recover useful products ; Cleaning aqueous emulsion based
    • 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
    • C10M107/00—Lubricating compositions characterised by the base-material being a macromolecular compound
    • C10M107/20—Lubricating compositions characterised by the base-material being a macromolecular compound containing oxygen
    • C10M107/30—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M107/32—Condensation polymers of aldehydes or ketones; Polyesters; Polyethers
    • C10M107/34—Polyoxyalkylenes
    • 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
    • C10M125/24—Compounds containing phosphorus, arsenic or antimony
    • 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
    • C10M173/02—Lubricating compositions containing more than 10% water not containing mineral or fatty oils
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/02—Water
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/081—Inorganic acids or salts thereof containing halogen
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/082—Inorganic acids or salts thereof containing nitrogen
    • 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
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/08—Inorganic acids or salts thereof
    • C10M2201/084—Inorganic acids or salts thereof containing sulfur, selenium or tellurium
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2201/00—Inorganic compounds or elements as ingredients in lubricant compositions
    • C10M2201/085—Phosphorus oxides, acids or 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/1033—Polyethers, i.e. containing di- or higher polyoxyalkylene groups used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C—CHEMISTRY; METALLURGY
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    • C10M—LUBRICATING COMPOSITIONS; USE OF CHEMICAL SUBSTANCES EITHER ALONE OR AS LUBRICATING INGREDIENTS IN A LUBRICATING COMPOSITION
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/104—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only
    • C10M2209/1045—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing two carbon atoms only used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/105—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only
    • C10M2209/1055—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing three carbon atoms only used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/106—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing four carbon atoms only
    • C10M2209/1065—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of alkylene oxides containing four carbon atoms only used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/107—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/107—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106
    • C10M2209/1075—Polyethers, i.e. containing di- or higher polyoxyalkylene groups of two or more specified different alkylene oxides covered by groups C10M2209/104 - C10M2209/106 used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/108—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified
    • C10M2209/1085—Polyethers, i.e. containing di- or higher polyoxyalkylene groups etherified used as base material
    • 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
    • C10M2209/00—Organic macromolecular compounds containing oxygen as ingredients in lubricant compositions
    • C10M2209/10—Macromolecular compoundss obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
    • C10M2209/103—Polyethers, i.e. containing di- or higher polyoxyalkylene groups
    • C10M2209/109—Polyethers, i.e. containing di- or higher polyoxyalkylene groups esterified
    • C10M2209/1095—Polyethers, i.e. containing di- or higher polyoxyalkylene groups esterified used as base material
    • 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
    • C10N2050/00—Form in which the lubricant is applied to the material being lubricated
    • C10N2050/01—Emulsions, colloids, or micelles

Definitions

  • the present invention relates to the technical field of industrial lubricating and/or cooling agents, especially such agents for use in metal working. More specifically the invention relates to purification of such agents, in the following referred to as "lubricating agents", as regards microbial contaminants by using polymeric two-phase systems.
  • Cutting oils and cutting liquids represent a common type of industrial lubricating agents which are widely used in the engineering industry in connection with cutting, turning, drilling, grinding and similar machining of materials. Their primary function is to increase the useful life of the tools by acting as a cooling and lubricating agent between the tools and the work pieces.
  • Cutting oils - as well as lubricating agents in general - consist of so-called base oils, which may be based on mineral oils or be synthetic or semi-synthetic.
  • base oils which may be based on mineral oils or be synthetic or semi-synthetic.
  • cutting liquids/lubricating liquids we mean aqueous emulsions of cutting oils and lubricating oils respectively.
  • Cutting liquids contain a plurality of components, from bactericidal preparations to anti-foam agents and corrosion inhibitors. Several of these components, together with a micro-flora of bacteria and fungi, are considered to be capable of causing problems, especially eczema and skin irriation, for industrial workers (Wahlberg, J.E. 1976, Skin-influence of oil, Esso Symposium 1976).
  • JP 51079959 discloses an agent for the treatment of contaminated waste water, including used cutting oil, by adsorption of the contaminants.
  • the adsorbent consists of very small complex bodies comprising inorganic particles and an organic polymer.
  • the inorganic particles may consist of active carbon or certain metal hydroxides.
  • Aqueous polymeric two-phase systems as such have been known for a long time and have been used in laboratories for biochemical and microbiological analyses and separations, e.g. for separating macro molecules, cell particles and whole cells (e.g. Albertsson P. ⁇ . 1960, Partition of Cell Particles and Macromolecules, 2nd edition, Almquist & Wiksell, Uppsala; Blomquist G. and Ström G. 1984, The Distribution of Mould Fungi Conidies in Polymeric Two-Phase Systems, Work and Health No. 31, Ström G. 1986, Qualitative and Quantitative Analysis of Microorganisms Particularly Fungal Spores-Methodological Developments, doctor's thesis, University of Ume ⁇ ).
  • polymeric two-phase system have found few technical uses.
  • Polymeric two-phase systems substantially consist of two aqueous solutions of polymers having different molecular weights. When the two polymer solutions are mixed in certain proportions, two immiscible aqueous phases are formed.
  • the top-phase substantially contains the low molecular polymer and the bottom-phase substantially contains the high molecular polymer.
  • the water contents in the systems is high, usually between 80-98% depending on the choice of the phase polymers.
  • a suitable watersoluble salt e.g. phosphate buffer.
  • particles or cells are distributed substantially between the top-phase, the inter-phase (the interface between the phases) and the bottom-phase; soluble macromolecules will be distributed between the top and bottom-phases.
  • top-phase component and “bottom-phase component” respectively when referring to those component/components of the polymeric system, which after mixing and separation of the system substantially are found in the top-phase and the bottom-phase respectively.
  • the present invention aims at reducing or eliminating the above mentioned problems and draw-backs of the prior art systems for using, handling and getting rid of industrial lubricating agents, in particular cutting liquids in the engineering industry.
  • a special object of the invention is to provide lubricating agent/cutting liquid systems having a considerably longer useful life than today's systems.
  • Another special object of the invention is to provide a purification process which makes it possible to purify lubricating liquids microbially while in use, thereby considerably reducing the shut-down time because of change of liquid.
  • a further object of the invention is to provide purification methods and means for lubricating liquids which meet high demands on industrial hygien and working environment.
  • a still further object of the invention is to provide an improved analysis method for determining the contents of microbial contaminants in industrial lubricating agents, especially cutting liquids.
  • a further object of the invention is to provide a lubricating agent which is also capable of serving as the top-phase polymer in a polymeric two-phase system for separating microbial contaminants from a lubricating agent.
  • the invention in its different aspects is founded on the basic concept of utilizing polymeric two-phase systems for separating microbial contaminants from contaminated lubricating agents.
  • the polymeric two-phase system will be designed in such a manner that there is formed, after mixing with a lubricating agent and phase separation, a top-phase containing lubricant and a bottom-phase containing at least part of the microbial contaminants, so that at least a major part of the microbial contaminants can be removed together with the bottom-phase, which can easily be separated from the top-phase. (For the purposes of this description also the inter-phase is included in the bottom-phase.)
  • One aspect of the invention comprises a method of purifying microbially contaminated lubricating agents, which is characterized by the steps of mixing the lubricating agent with a polymeric two-phase system, allowing the mixture to separate so as to form a top-phase containg the lubricating liquid and a bottom-phase containing at least a part of the microbial contaminants, and separating at least a major part of the microbially enriched bottom-phase from the top-phase.
  • the enclosed drawing schematically shows a purification plant illustrating how the principle of the cutting liquid cleaning according to the invention may be put into practice.
  • the plant comprises a tank 1 for cutting liquid S containing the top-phase component.
  • the cutting liquid S is continuously being circulated between the tank 1 and work stations (not shown) through inlet conduits 2 and outlet conduits 3 of the tank. Suitable distribution conduits, pumps, etc. are used for transporting cutting liquid to and from the work stations. This is quite conventional technique and will therefore not be described further in this context.
  • the plant comprises a mixing tank 4, in which there is a stirrer 5, and a separator 6.
  • the latter can also be connected to the separator 6 through a conduit 9 having a shut-off valve 10.
  • a supply container 11 for fresh or recovered bottom-phase component and a collection container 12 for used bottom-phase are connected to the mixing tank 4 through a conduit 13, and a conduit 14 interconnects the collection container 12 with the bottom part of the separator 6.
  • Fresh bottom-phase component can be supplied to the supply container 11 from a supply (not shown) through a conduit having a valve 15.
  • An interconnecting conduit 16 makes it possible, if desired, to re-use bottom-phase from the container 12 through a (dash-dotted) conduit 16, which may have a suitable rough filter 17.
  • a return conduit 18 returns purified cutting liquid to the tank 1.
  • the described plant can be used i.a. as follows for purifying microbially contaminated cutting oil circulating through the tank 1. It should in this context especially be noticed that the cleaning can be carried out without any need of interrupting the feeding of cutting liquid to the work stations; this means that the circulation of cutting liquid through the conduits 2 and 3 may continue as usual.
  • Contaminated cutting liquid S is supplied to the mixing tank 4 by opening the valve 8 in the conduit 7.
  • Fresh or reused bottom-phase is supplied to the mixing tank 4 through the conduit 13. The supply valves are then closed and top and bottom-phase components are mixed with the contaminated cutting liquid.
  • valve 10 is opened and the mixture is transferred to the separator 6, wherein it is allowed to separate into a top-phase T and a bottom-phase B. A major or minor part of the microbial contaminants from the top-phase T to the bottom-phase B will then move into the bottom-phase B, but the cutting liquid will remain in the top-phase T.
  • the purified top-phase will be returned to the cutting oil tank 1 through the conduit 18.
  • the bottom-phase B together with its microbial contaminants will be discharged through the bottom conduit 14.
  • the bottom-phase B can either be discarded through a drain 19 or be returned to the tank 11, preferably after rough filtering and/or other purification in the device generally designated 17. Disposal is preferred when the bottom-phase component consists of cheap material, whereas re-use is preferable when it contains expensive material such as fractionated dextran.
  • the re-circulated top-phase will also contain a minor amount of the corresponding salt.
  • Such salts may have an unfavourable effect on the properties of the cutting liquid, and it is then preferable to desalt the top-phase before returning it into the tank 1.
  • the plant shown in the drawing has been provided with a desalting device 20, which may be based on desalting principles which are known per se .
  • Top-phase polymers which are preferred according to the invention are comparatively low molecular hydrophilic polymers, especially polymers which are not solid at room temperature.
  • hydrophilic polymers of higher molecular weight, which are solid at room temperature can also be used within the scope of the invention.
  • the top-phase component of the two-phase system comprises at least one polyalkylene glycol, especially a polyethylene glycol having an average molecular weight of 200-20,000, especially 400-10,000, in particular about 600-4,000.
  • top-phase also other hydrophilic polymers which are liquid at room temperature and/or at the temperature of use and which per se are useful in synthetic cutting oils as the single cutting oil component or together with other cutting oil components in synthetic or semi-synthetic cutting oils.
  • Polyoxyalkylene-polyalcohol ethers such as polyoxyalkyleneglycol ethers, linear polymers of ethylene and/or propylene oxide are a few examples of preferred polymers, which are capable of simultaneously functioning as a cutting liquid and a top-phase component.
  • Such lubricating liquids may, for example, contain at least about 2% by weight, especially at least 4, often at least 6% by weight of the polymer, especially at least 7% by weight.
  • the concentration of the top-phase polymers in the lubricating liquid decreases with increasing molecular weight.
  • the bottom-phase component contains a polymer
  • such polymer preferably has a higher average molecular weight than the top-phase polymer.
  • the bottom-phase polymer preferably has an average molecular weight of at least 40,000, and it is preferably cross-linked.
  • suitable bottom-phase polymers are polysaccharides, in raw or refined form, especially cross-linked polysaccharides, in particular cross-linked dextran, starch, cellulose, polyglucose or cross-linked mono-, di- or oligosaccharides.
  • suitable bottom-phase polymers are polyvinyl alcohols of different average molecular weights. Polyvinyl alcohols can be recovered from the bottom-phase by e.g. precipitation.
  • the bottom-phase component may also advantageously comprise a small amount of a suitable agent distributing into the bottom-phase and promoting the transfer of the microbial contaminants from the top-phase to the bottom-phase.
  • a suitable agent preferably carry positive electric charges which attract the negative charges on the cell surfaces of the bacteria.
  • the system is preferably kept at a pH from neutral to slightly basic so as to expose the charges on the cell surfaces of the bacteria.
  • charge-exposing agents are hydrophilic polymers containing positively charged groups,. e.g. DEAE-groups.
  • Such positively charged agents may be present in very low concentrations (the order of magnitude of 10 -2 % - 10 -3 %) and still have a strong effect.
  • these salts may e.g. consist of common buffer salts such as alkali metal phosphates and sulphates and mixtures thereof.
  • the amounts of such salts may vary within comparatively broad limits, the amount i.a. depending on the particular salts and the particular top-phase polymer being used. For example, good results are obtained when using a two-phase system comprising phosphate buffer in combination with low molecular polyetheylene glycol, about 10-20% of each component.
  • the lubricating liquids preferably comprise 1-16% by weight of lubricating oil, especially about 2-10% by weight of lubricating oil, at least about 2% by weight of top-phase component, especially at least about 4% by weight of top-phase component, and when the top-phase component comprises a low molecular polymer which is not solid at room temperature, preferably at least about 8% by weight of the top-phase component, the remainder essentially consisting of water.
  • the upper limit for the amount of top-phase component is not particularly critical and will therefore primarily be chosen with regard to practical/economical considerations.
  • polymeric two-phase systems for separating microbial contaminants from contaminated lubricating liquids can also preferably be used for analysing the separated phase with regard to microbial contaminants.
  • Such an analysis which preferably will be performed substantially quantitatively or semi-quantitatively, gives a very rapid and reliable basis for judging the quality of the lubricating liquid and as a guide for determining what measures may be necessary to take, for example addition of biocides, exchange of lubricating liquid, etc.
  • analyses are performed by cultivation on suitable nutritions substrates, usually having the form of "sticks" to be dipped into the lubricating liquid. The cultivation requires several days to be completed and the error margins are considerable.
  • the bottom-phase which is separated in the purification method for cutting oils according to the invention can be used for the analysis, but it is preferred to take a special sample for the analysis.
  • the bottom-phase it is preferred to use salts of the above indicated type instead of high molecular polymers.
  • the starting point for the use of a two-phase technique for continuous purification of cutting liquids is that addition of cutting oil/emulsion concentrates to a two-phase system provides a top-phase in the nature of e.g. a cutting liquid/polymer phase which is well separated from a bottom-phase which collects microbial contaminants.
  • a top-phase in the nature of e.g. a cutting liquid/polymer phase which is well separated from a bottom-phase which collects microbial contaminants.
  • factors which may influence the distribution of a microbial particle between the top, inter and bottom-phases are, for example, the choice of polymers - charged/uncharged polymers - the polymer concentration, the choice of pH and the ionic strength.
  • the machining test was performed using production machining data on heat treatment steel (SS 2541-03) and a stable machine tool.
  • Equipment Work piece material SIS 2541-03 (260 HB) Tool material: High speed steel, SIS 2724, ⁇ 6 mm Numerically-controlled bed cutter: SAJO VBF 450 Machining Data Cutting speed 17-35 m/min Feed: 0.17 mm/r Depth of bores: 24 mm (4 x d) Warn-out test: total destruction
  • the work pieces are taken from one charge and are rolled in sequence. They are cut to a size of 200 x 30 x 375 mm (about 400 bores/plate) and spot faced.
  • the tools are normalized with narrow geometric tolerances and hardness variations.
  • the work pieces (2) are clamped into the machine and the test program is designed so as to distribute the machining on both plates for each tool, the purpose being to avoid local unevenness in the material.
  • the cutting speed is varied for different drills in order to obtain a relation between cutting speed and warn-out time (vT-curve).
  • Destruction of the tool is seen as vibrations and changing cuttings (the tip melts). This occurs within a few seconds.
  • the test results show that the addition, according to the invention, of a top-phase polymer to a mineral oil based fine emulsion results in a plurality of positive effects as regards the properties of the cutting liquid.
  • the metal-cutting test which is an indirect measure of the cooling and lubricating properties of the liquid, showed reduced wear of the machine tool when using a cutting liquid containing a polymer.
  • a useful tool life expressed as the number of holes/drill, of about 28 was recorded for the normal cutting liquid, and a value of 130 for the corresponding polymer/cutting liquid mixture (see vT-curve in Fig. 2).
  • An important property for the useful life of a cutting liquid is the capability of efficiently separating contaminating leak oil from i.a. hydraulic systems.
  • the comparative tests with and without admixture of polymer showed a lower tendency of leak oil emulgation into the cutting liquid according to the invention, which means that it is easy to remove leak oil from the system.
  • the cutting liquid had an evident anti-corrosive effect on cast-iron whereas the effect of the reference liquid was unacceptable for engineering products. Both products showed an increased effect on steel.
  • Amine derivatives are often used as corrosion inhibitors in cutting liquids. These amines often cause working environmental problems. Furthermore, carbon/nitrogen compounds of the amine type can readily be used as a substrate by microorganism, thereby promoting the microbial growth. The evident corrosion inhibiting effect when adding a top-phase polymer according to the invention can make it possible to completely exclude amine compounds from these products.
  • Hard crystalline evaporation residues from a cutting liquid may have a negative effect on movable machine parts and precision tools.
  • the evaporation tests with the mineral oil based fine emulsion with addition of polymer according to the invention showed that the product could not be evaporated, probably because a formed surface layer prevented water from escaping.
  • Other evaporation tests using both mineral oil based and semi-synthetic emulsion concentrates containing polymer according to the invention and water showed that no hard crystalline evaporation residue was formed.
  • the mineral oil based concentrate two-phases were obtained, one consisting of concentrate and the other of the added top-phase polymer.
  • a polymer mixture consisting of diethylaminoethyl dextran (DEAE-dextran) and below listed polymers was added to each of the systems for the separation test:
  • the final concentration in the system was 0.001% for DEAE-dextran and 1% for the other polymers (w/w).
  • the quantification of the number of fungi elements was performed by cultivation on a substrate composed of 2% (w/w) of malt extract (Oxoid, L 39), 1.5% Agar (Oxoid, L 28) and 30 mg/l of streptomycin sulphate (Sigma Chemical Co.). Incubation was carried out at room temperature (22°C) during 4 days, after which the number of colony forming units could be determined.
  • the concentration of bacteria was determined by the cultivation on a substrate composed of 2.4% (w/w) Tryptone Glucose Extract Agar (CM 127, Oxoid), 0.2% Casein Hydrolysate (Acid) (L 41, Oxoid) and 50 mg/l Actidione (Sigma).
  • the number of colony forming units was determined after incubation for six days at room temperature.
  • Tables 1 and 2 The results of separation tests performed with different dextran fractions or soluble starch as the bottom-phase polymer and with the above described composition of the top-phase are presented in Tables 1 and 2.
  • Table 1 Separation of bacterial cells of Bacillus subtilis using different bottom-phase polymers. The amount of bacterial cells before the separation was 1.6 x 10 8 /ml in Systems 1 and 3 and 1.5 x 10 8 in System 2. The final concentration of the bottom-phase polymers was 1%. A semi-synthetic fine emulsion (5-Star-40) was used as the emulsion concentrate.
  • Bottom-phase-polymer a) Bact. conc. after sep.
  • a semi-synthetic fine emulsion was used together with the top-phase polymers (Table 1), and in the other case a mineral oil based rough emulsion (Table 2). Together with the bottom-phase polymers also diethylamino-ethyl-dextran (DEAE-dextran) was added to a final concentration of 0.001%.
  • DEAE-dextran diethylamino-ethyl-dextran
  • top-phase polymers according to the invention with excellent results can be included in cutting liquids and at the same time function as the top-phase in a two-phase system for microbial cleaning of the cutting liquid.
  • dextran As regards dextran, a broad range of fractions, from finely fractioned Dextran 500 (molecular weight 500,000) to more unfractionated (and consequently cheaper) raw dextran have been tested and found to be very useful. When using high molecular dextran it has been found to be especially advantageous with a top-phase concentration of about 19% (w/w) of Polyethylene glycol 600 or, alternatively, about 12.5% Polyethylene glycol 600 + 2.5% Polyethylene glycol 8000. In the latter case it is suitable to use a semi-synthetic cutting liquid concentrate.
  • the amount of dextran may be about 1%, resulting in a bottom-phase volume making up about 3-5% of the total system.
  • dextran may be replaced by other high molecular polymers, e.g. soluble starch, glucogen or synthetic polyglucose, as the bottom-phase polymer.
  • High molecular polyethylene glycols which are crystalline at room temperature, are not soluble in a concentrate based on mineral oi only, but is highly soluble in synthetic emulsion concentrates. Evaporation tests using a mixture of 2.5% (weight/weight) of Polyetheylene glycol 8000 (Carbovax 6000), 5% (w/w) of semi-synthetic emulsion concentrate (fine emulsion), and 12.5% (w/w) of Polyethylene glycol 600 did not produce any crystalline residue.
  • the bottom-phase polymer may consist of unfractionated or substantially unfractionated raw dextran.
  • raw dextran preferably has a molecular weight of 5-40 millions, and it is preferably used in mixture with a small amount of positively charged polymer such as DEAE-dextran.
  • Raw dextran is the presently preferred material for the bottom-phase polymer since it is both cheap and efficient. It is especially preferred to use raw dextran which has been substituted with a small amount of positively charged groups, e.g. DEAE groups, in which case it is not necessary to add any separate charged polymer when there is a need thereof.
  • raw fractions of other polysaccharides can be used in corresponding manner.
  • the polymer contents can be as low as about 0.01%.
  • a synthetic cutting liquid was prepared by mixing the following components in water to the indicating concentrations.
  • Emkarox VG 680W (a polyoxyalkylene glycol ether from ICI) 6 % Synperonic T/701 (a foam inhibitor from ICI) 0.1 % Phosphate buffer to pH about 7 Water q.s.
  • Bacterial cells and fungal spores were added (in the above described manner) to the above cutting liquid to simulate a microbially contaminated cutting liquid.
  • Raw dextran molecular weight 5-40 millions, final concentration 0.1%) with added DEAE-dextran (final concentration 0.01%) was used as the bottom-phase polymer.
  • the top and bottom-phases were mixed and allowed to separate; 97-99% of the bacteria and about 99% of the fungi were transferred into the bottom-phase and separated.
  • a presently preferred embodiment of the analysis method according to the invention for quantification of the microbial contamination of cutting liquids will now be described as an illustrative but non-limiting example.
  • the results of the analysis can e.g. be used for judging the quality of the used cutting liquid.
  • a pre-determined amount of a polymeric two-phase system according to the invention was added to a test bottle having a sealable, preferably "pipette shaped" stopper.
  • a bottle holding a total of about 50 ml can e.g. be charged with 20 ml of the system in advance, sealed and delivered to the user.
  • an aliquote (20 ml) of a cutting liquid sample is "pipetted” into the bottle, which is then shaken so as to mix the phases and then allowed to separate with the bottle turned upside down.
  • the bottle may preferably be compressible and have a suitable visible volume scale. The separation is normally very good already after 10 to 20 seconds, but it is preferred to allow the separation to proceed for a few minutes.
  • the bottom-phase which substantially consists of salt solution, e.g. phosphate buffer pH about 6.8 and comparison with a standard curve for a corresponding system, prepared in a manner known per se . It is, however, preferable to make a further separation step in which the bottom-phase from the first step (e.g. 10 ml of bottom-phase), which is rich in biomass, is mixed with a suitable polymer for a second phase system (e.g. 4 g of polypropylene glycol having a molecular weight of about 425).
  • a suitable polymer for a second phase system e.g. 4 g of polypropylene glycol having a molecular weight of about 425.
  • the bottom-phase from the first separation is located closest to the opening of the bottle, which preferably is "pipette shaped", the transfer and metering to the second system can be done very conveniently.
  • this second separation can be carried out in a pre-prepared bottle designed similarly as the first bottle. The second bottle is shaken so as to mix the phases well, then allowed to rest until the phases have separated (normally the same separation times as for the first separation are preferred), and a predetermined amount of the biomass-enriched bottom-phase is taken out for turbidimetric analysis and comparison with a standard curve (which expression also includes a specific mathematical relation or any other relation for quantification of the measured value which has been determined in advance).
  • the sample may optionally be diluted with e.g. particle-free water (in the given specific example e.g. 2 ml sample plus 2 ml of particle-free water).
  • particle-free water in the given specific example e.g. 2 ml sample plus 2 ml of particle-free water.
  • the amount of live biomass can be determined in the above indicated manner, e.g. by using fluorescinediacetate (FDA) as a marker.
  • FDA fluorescinediacetate
  • the separation method according to the invention can also advantageously be used for making used cutting liquids or other lubricating liquids such as waste oil disposable.
  • used cutting liquids or other lubricating liquids such as waste oil disposable.
  • the disposal of e.g. synthetic or semi-synthetic cutting liquids is a very costly process because it is very difficult to concentrate diluted polymer mixtures (and the polymer cannot be disposed of just anywhere).
  • the disposal costs can often be as high as the purchase price. According to the invention this problem can be easily remedied by strongly concentrating the polymer, e.g. in the following way.
  • a used-up cutting liquid containing about 7 % by weight of Emkarox (see above) as the top-phase polymer is mixed with about 60% phosphate buffer (bottom-phase) to a final concentration of 25% and allowed to separate (from a minute to an hour or so).
  • a very concentrated and easily separable polymer top-phase is formed (e.g. 35-50%, total volume about 5% of the cutting liquid volume), which can be destructed, whereas the aqueous phase usually can be disposed of directly.

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  • Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Combustion & Propulsion (AREA)
  • Inorganic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Emergency Medicine (AREA)
  • Lubricants (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)
  • Forging (AREA)
  • Physical Or Chemical Processes And Apparatus (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Separation Of Suspended Particles By Flocculating Agents (AREA)
EP89912680A 1988-11-21 1989-11-21 Purification of industrial lubricating agents Expired - Lifetime EP0451160B1 (en)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
SE8804206 1988-11-21
SE8804206A SE462393B (sv) 1988-11-21 1988-11-21 Anvaendning av vattenhaltiga polymera tvaafassystem foer rening av skaervaetskor, foerfarande och anlaeggning foer reningen samt skaeroljekoncentrat innehaallande polymer ingaaende i tvaafassystemet och skaervaetska utgoerande vattenemulsion av skaeroljekoncentratet
PCT/SE1989/000677 WO1990005768A1 (en) 1988-11-21 1989-11-21 Purification of industrial lubricating agents

Publications (2)

Publication Number Publication Date
EP0451160A1 EP0451160A1 (en) 1991-10-16
EP0451160B1 true EP0451160B1 (en) 1996-09-11

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EP89912680A Expired - Lifetime EP0451160B1 (en) 1988-11-21 1989-11-21 Purification of industrial lubricating agents

Country Status (11)

Country Link
EP (1) EP0451160B1 (da)
JP (1) JP2983235B2 (da)
AT (1) ATE142685T1 (da)
AU (1) AU645004B2 (da)
DE (1) DE68927180T2 (da)
DK (1) DK95591A (da)
ES (1) ES2091767T3 (da)
FI (1) FI105273B (da)
NO (1) NO301080B1 (da)
SE (1) SE462393B (da)
WO (1) WO1990005768A1 (da)

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE69405873T2 (de) * 1993-07-30 1998-04-09 Du Pont Vorrichtung zur gegenstromtrennung einer mehrphasigen flüssigkeit
SE9303437D0 (sv) * 1993-10-18 1993-10-18 Pegasus Separation Ab Reningsförfarande
SE512750C2 (sv) * 1993-11-29 2000-05-08 Alfa Laval Separation Ab Metod för gravimetrisk separation av olja som förorenats med partiklar och eller vatten
EP0760865A1 (en) * 1994-05-23 1997-03-12 E.I. Du Pont De Nemours And Company Method for the rapid separation and identification of microbial contaminants from a complex matrix

Also Published As

Publication number Publication date
AU4519789A (en) 1990-06-12
DE68927180T2 (de) 1997-02-20
SE8804206D0 (sv) 1988-11-21
DK95591A (da) 1991-07-09
FI912351A0 (fi) 1991-05-15
DK95591D0 (da) 1991-05-21
JP2983235B2 (ja) 1999-11-29
DE68927180D1 (de) 1996-10-17
AU645004B2 (en) 1994-01-06
JPH04501731A (ja) 1992-03-26
WO1990005768A1 (en) 1990-05-31
ATE142685T1 (de) 1996-09-15
FI105273B (fi) 2000-07-14
NO301080B1 (no) 1997-09-08
NO911912L (no) 1991-05-16
ES2091767T3 (es) 1996-11-16
EP0451160A1 (en) 1991-10-16
SE462393B (sv) 1990-06-18
NO911912D0 (no) 1991-05-16

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