EP3404083A1 - Procédé de lavage pour des huiles de rouleau et de dressage - Google Patents

Procédé de lavage pour des huiles de rouleau et de dressage Download PDF

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Publication number
EP3404083A1
EP3404083A1 EP17171441.3A EP17171441A EP3404083A1 EP 3404083 A1 EP3404083 A1 EP 3404083A1 EP 17171441 A EP17171441 A EP 17171441A EP 3404083 A1 EP3404083 A1 EP 3404083A1
Authority
EP
European Patent Office
Prior art keywords
oil
rolling
aluminum
phase
aqueous
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP17171441.3A
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German (de)
English (en)
Inventor
Olaf Güssgen
Thomas Graf
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Speira GmbH
Original Assignee
Hydro Aluminium Rolled Products GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hydro Aluminium Rolled Products GmbH filed Critical Hydro Aluminium Rolled Products GmbH
Priority to EP17171441.3A priority Critical patent/EP3404083A1/fr
Priority to JP2018093076A priority patent/JP6762988B2/ja
Priority to EP18171973.3A priority patent/EP3404084B1/fr
Publication of EP3404083A1 publication Critical patent/EP3404083A1/fr
Withdrawn legal-status Critical Current

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Classifications

    • 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
    • C10M175/005—Working-up used lubricants to recover useful products ; Cleaning using extraction processes; apparatus therefor
    • 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
    • C10M175/02—Working-up used lubricants to recover useful products ; Cleaning mineral-oil 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
    • 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
    • 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
    • C10N—INDEXING SCHEME ASSOCIATED WITH SUBCLASS C10M RELATING TO LUBRICATING COMPOSITIONS
    • C10N2010/00—Metal present as such or in compounds
    • C10N2010/02—Groups 1 or 11
    • 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
    • C10N2040/244—Metal working of specific metals
    • C10N2040/245—Soft metals, e.g. aluminum

Definitions

  • the invention relates to a process for the recycling of aluminum-contaminated oil from rolling / tempering processes.
  • Rolled oils and tempering oils are coolants that have a major impact on production efficiency and product quality.
  • the coefficient of friction between the work roll and the rolling stock should neither be too high nor too low.
  • a low coefficient of friction improves the lubrication in the nip, so that energy consumption, frictional heat and roller wear are reduced.
  • the rolling oils are heavily contaminated by metal abrasion.
  • the impurities are essentially metal abrasion and metal soaps from the rolling stock, for example aluminum and magnesium, as well as to metal abrasion from the rollers (for example, iron and chromium).
  • metal abrasion from the rollers for example, iron and chromium.
  • temper rolling comparatively small amounts of rolling oil are used, but after a short time they are heavily contaminated with metal abrasion.
  • the proportion of aluminum in the rolling oil can then be up to 2 wt .-% and more, based on the mass of the oil.
  • the condition of the rolling oil must be continuously monitored during rolling or temper rolling, so that the limit concentrations of aluminum for the respective rolling processes are not exceeded.
  • high amounts of aluminum in the rolling oil during rolling lead to problems with the product quality.
  • Large amounts of metal abrasion in the rolling oil lead to damage to the rolls and to the formation of visually conspicuous surface contamination on the rolling stock, such as rolls, dark stripes and holes.
  • the DE 15 45 299 A1 proposes that waste oils from waste oils from engines and transmissions of motor vehicles be coagulated by mixing with an aqueous alkali hydroxide solution of a concentration of 10 to 50 wt .-% in a ratio of 2 to 15 wt .-%, based on the mass of waste oil and separating the clarified oil from the coagulating liquid and the suspension of the aging products and then further processing them by the processes of the petroleum industry, for example by refining.
  • the particle sizes are so low and the particle size distribution of the metal abrasion is so unfavorable that a satisfactory separation from the oil by filtration is hardly achievable.
  • the invention is therefore an object of the invention to provide a process for the purification and reuse of used rolling oil or casting oil, which avoids the aforementioned disadvantages.
  • This object is achieved by a process for the recycling of aluminum-contaminated oil from rolling or casting processes, in which aluminum-contaminated rolling oil or casting oil is mixed with aqueous alkali metal hydroxide solution, causes a phase separation between the aqueous phase and oil phase, then the aqueous phase of separates the oil phase and the oil phase freed with a drying agent of residual water and possibly existing suspended matter.
  • the inventive method allows the recycling of the purified oil as rolling or casting oil.
  • the product oil of the process according to the invention has a high quality. Impurities due to thermal treatment of the oil are not present at the time of recycling.
  • a high saving of oil in industrial rolling and skin-pass coating plants is made possible.
  • contaminated oils from rolling / coating processes without waste-producing filtrations and / or thermal separation processes such as distillation or rectification can be purified in a discontinuous process and reused as pure oil.
  • wastewater in relatively small quantities.
  • the resulting aluminum hydroxide can be used in the water treatment.
  • Critical waste is avoided.
  • the ecological footprint is significantly lower than in conventional cleaning processes. The same applies to the investment and operating costs.
  • rolling oils and tempering oils are oils and oil-containing liquids intended for rolling and temper rolling.
  • oil in the context of the invention includes fatty alcohols, fatty acids, fatty acid esters and kerosene cuts, mineral oils, vegetable oils and synthetic oils and mixtures thereof.
  • the hydrocarbon chains of these compounds may have, for example, 8 to 20, preferably 10 to 18, carbon atoms.
  • the boiling end of the aforementioned organic chemical compounds should be below the usual in the aluminum industry lowest annealing temperature of about 320 ° C.
  • the kinematic viscosity of the rolling and tempering oils at 40 ° C is usually below 10 mm 2 / s, preferably below 6 mm 2 / s.
  • rolling oils and tempering oils may contain conventional rolling additives.
  • the oils to be purified as starting material in the process according to the invention have been previously used in the coating and rolling of films and wires made of aluminum. These oils are highly contaminated by metallic abrasion compared to their first use.
  • the impurities contained therein are, for example, aluminum abrasion and other metal abrasion.
  • the content of aluminum particles in the contaminated oil may be, for example, 500 to 4,000 mg / l. High levels of metal debris can severely affect product quality in rolling processes, especially when producing very thin tapes.
  • the degree of soiling of the oil with metal abrasion is visually detectable during the rolling or skin-pass treatment and can also be determined gravimetrically by determining the turbidity or by examination with particle counters and particle size analyzers.
  • the contaminated oil described above is mixed with a dilute aqueous alkali metal hydroxide solution with stirring in accordance with the present invention.
  • the contaminated oil is introduced into the aqueous alkali metal hydroxide solution.
  • Alkalimetallhydroxidnaps in the context of the invention means a solution of alkaline earth metal hydroxide and / or alkali metal hydroxide.
  • Particularly suitable alkali metal hydroxides according to the invention are sodium hydroxide and potassium hydroxide.
  • the concentration of the alkali metal hydroxide in the aqueous solution is preferably so high that the aluminum present in the oil is completely dissolved.
  • the amount of alkali metal hydroxide preferably present is sized to provide an excess of alkali metal hydroxide as compared to the aluminum particles and other metal particles present in the oil.
  • the alkali metal hydroxide solution may contain alkali metal in a concentration of preferably 1 to 9% by weight, more preferably 2 to 7% by weight, based on the weight of the solution.
  • the alkali metal hydroxide solution initially introduced can, for example, have a concentration of from 2 to 5% by weight of alkali metal hydroxide, based on the mass of the alkali metal hydroxide solution.
  • the volumetric proportion of the aqueous alkali metal hydroxide solution may preferably be more than 40% v / v, based on the volume of rolling oil and aqueous alkali metal hydroxide solution.
  • the aqueous alkali metal hydroxide solution and the contaminated oil are thoroughly mixed.
  • the aluminum is washed out of the oil phase.
  • Aluminum is thereby converted to aluminum hydroxide and further to aluminate, which are soluble in the alkaline aqueous phase.
  • soaps may also form.
  • the aluminate remains in solution in the alkaline aqueous phase. If present, other metals also go into solution as hydroxides.
  • a water-soluble polyalkylene glycol may be added.
  • the addition of a polyalkylene glycol for phase separation is particularly useful when the rolling oil contains additives such as acids. These acids can be fatty acids having 12 to 16 carbon atoms.
  • the polyalkylene glycol is preferably one of viscosity class 140.
  • the kinematic viscosity of the polyalkylene glycol may be 140 mm 2 / s to 160 mm 2 / s, preferably about 150 mm 2 / s. The kinematic viscosity was determined with a rotational viscometer according to ASTM D-7042.
  • the polyalkylene glycol contains ethylene and propylene units. It can be used in an amount of 1 to 10 wt .-%, preferably 3 to 6 wt .-%, based on the mass of alkali metal hydroxide solution and polyalkylene glycol.
  • the mixing of contaminated oil and aqueous alkali metal hydroxide solution may preferably be carried out in a stirrer equipped reactor at room temperature (about 20 ° C).
  • the reactor may preferably be a conical conical reactor.
  • the stirrer used can be conventional stirrers.
  • an axial stirrer (propeller stirrer) is particularly suitable in the reactor for intensive mixing of aluminum-containing oil phase and aqueous alkali metal hydroxide phase to enable.
  • a tangential stirrer anchor stirrer
  • the reactor is vented. By venting the reactor, an increase in the concentration of hydrogen gas during the leaching of the aluminum should be avoided.
  • the mixing of the oil with the aqueous alkali metal hydroxide solution is preferably carried out until the oil phase is free of metallic aluminum. However, it is not mandatory that the oil phase is completely free of metallic aluminum.
  • the intensive mixing of the two phases can take, for example, 30 to 120 minutes, depending on the reactor size and stirring intensity. A visual visual inspection is sufficient. Before cleaning, the oil is dark and not transparent, clear and transparent after cleaning. The oil has a clear to yellowish color after cleaning.
  • a phase separation into an aqueous phase and an oil phase is done.
  • a time of 30 to 120 minutes may be required.
  • the higher density aqueous phase is deposited in the lower part of the reactor.
  • the liberated from aluminum oil with lower density floats on the aqueous phase.
  • the extent of the phase separation or the progress of the separation of the two phases can be monitored during the separation process by measuring the electrical conductivity of the liquid in the reactor or visually.
  • the aqueous phase is separated after phase separation. This is done, for example, by allowing the aqueous aluminate / aluminum hydroxide-containing phase, which optionally contains further metal hydroxides, to flow out of the lower part of the reactor.
  • water or an aqueous liquid may preferably be fed to the lower part of the reactor so as to drain the purified rolling oil by the rise of the liquid level in the upper part of the reactor.
  • the oil phase is washed once or twice with demineralized water. Even during washing, an intensive mixing of the oil with the water used for washing takes place. Subsequently, a phase separation of oil phase and wash water phase is allowed again. Thereafter, the washing water is separated as before the aqueous alkaline aluminate-containing phase.
  • the duration of the mixing of oil and wash water and the duration of the phase separation can be chosen as well as when washing with and separating from metal hydroxide solution.
  • the purified oil is removed from the reactor.
  • the oil will usually be saturated or almost saturated after washing out the aluminum with water.
  • the amount of water in the oil may be about 100 ppm.
  • the oil is passed through a filter.
  • This filtration device is used to dry the oil. It also serves to remove any suspended in the oil suspended matter.
  • the filtration device may contain one or more substances for the chemical or physical binding of water. Such substances or drying agents include, for example, silica gels, molecular sieves, sodium sulfate and magnesium sulfate. Sodium sulfate is particularly preferred.
  • the filtration device can be designed as a so-called candle filter, which is filled with the substance for the chemical or physical binding of water (drying agent). By drying the oil both water and suspended matter, if any are still present in the oil, separated from the oil. The resulting oil is essentially anhydrous. This means that the water saturation in the oil is between 20 to 70% of the highest possible water saturation, preferably by 50% or less.
  • the water saturation in the oil can be determined with a capacitive water sensor or determined by Karl Fischer titration.
  • the product oil of the process according to the invention is virtually free of metal abrasion.
  • the oil purity can be determined by measuring the turbidity.
  • the oil thus obtained can be reused as a pure oil in skin-pass or rolling processes.
  • the aqueous aluminate-containing phase can be neutralized.
  • the neutralization can be carried out, for example, by adding sulfuric acid.
  • the precipitation of aluminum hydroxide suspended solids and residual oil are trapped, precipitated and separated from the water. After separation of water and solid phase, the water thus obtained can often be discharged without further treatment but in accordance with the requirements for direct dischargers into the sewer.
  • the washing out of the aluminum from the oil can also take place in two reactors connected in parallel in the so-called pendulum batch operation, or different process stages of the process according to the invention are carried out in parallel in both reactors.
  • the process according to the invention can be carried out at ambient temperature. There is no need to supply energy in the form of heat.
  • the process can be carried out batchwise or continuously.
  • the aluminum foil is tempered in a temper rolling mill 1 with the addition of a tempering oil as a cooling lubricant (8 to 10 l / min).
  • a tempering oil as a cooling lubricant (8 to 10 l / min).
  • the skin-oil is conveyed from a clean oil tank 1 to the temper rolling mill 1.
  • the used enriched with aluminum casting oil is transferred to the storage container 4 for contaminated Dressieröl.
  • the contaminated oil is passed into the reactor 7.
  • Reactor 7 is equipped with a propeller 8 and a pressure aerator 9. By the pressure aerator 9, the enrichment of hydrogen gas in the reactor 7 should be avoided.
  • dilute alkali metal hydroxide solution in the reactor 7 in about 10 times the stoichiometric excess, based on aluminum was presented as 2 to 3% sodium hydroxide solution, before passing through line 5 contaminated oil is fed into the reactor to wash out the aluminum particles.
  • the dilute alkali metal hydroxide solution can be passed into the reactor 7.
  • Alkali metal hydroxide can be stored as a higher concentration solution in a storage tank 10.
  • liquid alkali metal hydroxide solution is transferred from the storage tank 10 via line 11 into a mixer where it is brought to the desired concentration with the addition of water from source 14 via line 13.
  • the conical downwardly formed reactor 7 is an intensive mixing of contaminated with aluminum and used rolling oil with the alkali metal hydroxide with the help of Propellerlickers 8.
  • a phase separation of aqueous alkaline phase and oil phase is brought about in the reactor 7. The extent of phase separation is determined by measuring the electrical conductivity. If the phase separation in the reactor is largely completed, the aqueous alkaline phase is discharged at the bottom of the reactor and passed via line 19 for further treatment 20 such as neutralization. Subsequently, the oil phase is discharged from the reactor 7 and passed via line 15 to a candle filter 16.
  • the drying of the oil takes place. Furthermore, suspended solids are retained in the filter material as it flows through the filter 16.
  • the effluent from the filter oil is passed via line 17 into the clean oil tank 1. From there it can be fed back to the skin pass mill 2 for use in a skin pass.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Lubricants (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
EP17171441.3A 2017-05-17 2017-05-17 Procédé de lavage pour des huiles de rouleau et de dressage Withdrawn EP3404083A1 (fr)

Priority Applications (3)

Application Number Priority Date Filing Date Title
EP17171441.3A EP3404083A1 (fr) 2017-05-17 2017-05-17 Procédé de lavage pour des huiles de rouleau et de dressage
JP2018093076A JP6762988B2 (ja) 2017-05-17 2018-05-14 圧延オイルおよび表面仕上げオイルの洗浄方法
EP18171973.3A EP3404084B1 (fr) 2017-05-17 2018-05-14 Procédé de lavage pour des huiles de rouleau et de dressage

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
EP17171441.3A EP3404083A1 (fr) 2017-05-17 2017-05-17 Procédé de lavage pour des huiles de rouleau et de dressage

Publications (1)

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EP3404083A1 true EP3404083A1 (fr) 2018-11-21

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EP17171441.3A Withdrawn EP3404083A1 (fr) 2017-05-17 2017-05-17 Procédé de lavage pour des huiles de rouleau et de dressage
EP18171973.3A Active EP3404084B1 (fr) 2017-05-17 2018-05-14 Procédé de lavage pour des huiles de rouleau et de dressage

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EP18171973.3A Active EP3404084B1 (fr) 2017-05-17 2018-05-14 Procédé de lavage pour des huiles de rouleau et de dressage

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JP (1) JP6762988B2 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114522992A (zh) * 2022-03-08 2022-05-24 金龙电缆科技有限公司 一种铝拉丝润滑液循环利用的方法

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2902439A (en) * 1958-07-03 1959-09-01 Aluminum Co Of America Reclamation of aluminum fabricating lubricants
DE1545299A1 (de) 1965-11-15 1969-06-26 Focsaneanu Dr Ing Otto A Verfahren zur Entfernung wesensfremder und wesenseigener Alterungsprodukte aus legierten und unlegierten Altoelen,wie Motoren- und Getriebeablassoelen,bzw. stark verschmutzter Kohlenwasserstoff-Loesemittel
EP0030805A1 (fr) * 1979-11-29 1981-06-24 AMSTED Industries Incorporated Procédé pour la séparation de matériau contaminant d'une huile contaminée
DE2613878C2 (de) 1975-04-10 1986-04-03 Schweizerische Aluminium Ag, Chippis Verfahren zum Reinigen von Walzölen
WO2016166499A1 (fr) * 2015-04-13 2016-10-20 3D Eco Oil Limited Lubrifiant

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2902439A (en) * 1958-07-03 1959-09-01 Aluminum Co Of America Reclamation of aluminum fabricating lubricants
DE1545299A1 (de) 1965-11-15 1969-06-26 Focsaneanu Dr Ing Otto A Verfahren zur Entfernung wesensfremder und wesenseigener Alterungsprodukte aus legierten und unlegierten Altoelen,wie Motoren- und Getriebeablassoelen,bzw. stark verschmutzter Kohlenwasserstoff-Loesemittel
DE2613878C2 (de) 1975-04-10 1986-04-03 Schweizerische Aluminium Ag, Chippis Verfahren zum Reinigen von Walzölen
EP0030805A1 (fr) * 1979-11-29 1981-06-24 AMSTED Industries Incorporated Procédé pour la séparation de matériau contaminant d'une huile contaminée
WO2016166499A1 (fr) * 2015-04-13 2016-10-20 3D Eco Oil Limited Lubrifiant

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RONALDO GONALVES DOS SANTOS ET AL: "Physico-chemical properties of heavy crude oil-in-water emulsions stabilized by mixtures of ionic and non-ionic ethoxylated nonylphenol surfactants and medium chain alcohols", CHEMICAL ENGINEERING RESEARCH AND DESIGN, ELSEVIER, AMSTERDAM, NL, vol. 89, no. 7, 29 November 2010 (2010-11-29), pages 957 - 967, XP028220468, ISSN: 0263-8762, [retrieved on 20101209], DOI: 10.1016/J.CHERD.2010.11.020 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114522992A (zh) * 2022-03-08 2022-05-24 金龙电缆科技有限公司 一种铝拉丝润滑液循环利用的方法
CN114522992B (zh) * 2022-03-08 2024-01-02 金龙电缆科技有限公司 一种铝拉丝润滑液循环利用的方法

Also Published As

Publication number Publication date
JP2019022906A (ja) 2019-02-14
EP3404084A1 (fr) 2018-11-21
EP3404084C0 (fr) 2023-08-09
EP3404084B1 (fr) 2023-08-09
JP6762988B2 (ja) 2020-09-30

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