EP0697471B1 - Verfahren zur Entfernung von Verunreinigungen von Metalloberflächen - Google Patents

Verfahren zur Entfernung von Verunreinigungen von Metalloberflächen Download PDF

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Publication number
EP0697471B1
EP0697471B1 EP19950304632 EP95304632A EP0697471B1 EP 0697471 B1 EP0697471 B1 EP 0697471B1 EP 19950304632 EP19950304632 EP 19950304632 EP 95304632 A EP95304632 A EP 95304632A EP 0697471 B1 EP0697471 B1 EP 0697471B1
Authority
EP
European Patent Office
Prior art keywords
composition
mixture
volume
active agent
surface active
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
EP19950304632
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English (en)
French (fr)
Other versions
EP0697471A1 (de
Inventor
William G.F. Ford
Tommy R. Gardner
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.)
Halliburton Energy Services Inc
Original Assignee
Halliburton Energy Services Inc
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Filing date
Publication date
Priority claimed from US08/437,709 external-priority patent/US5489394A/en
Application filed by Halliburton Energy Services Inc filed Critical Halliburton Energy Services Inc
Publication of EP0697471A1 publication Critical patent/EP0697471A1/de
Application granted granted Critical
Publication of EP0697471B1 publication Critical patent/EP0697471B1/de
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/16—Organic compounds
    • C11D3/18—Hydrocarbons
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23G—CLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G5/00—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents
    • C23G5/02—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents
    • C23G5/024—Cleaning or de-greasing metallic material by other methods; Apparatus for cleaning or de-greasing metallic material with organic solvents using organic solvents containing hydrocarbons

Definitions

  • the present invention relates generally to solvent compositions and to a method of removing materials such as pipe dopes and thread lubricants from metal surfaces using the compositions.
  • materials such as pipe dopes, thread lubricants and the like are routinely removed from the surfaces of tubular goods, e.g. strings of threaded tubing and casing disposed in the well bores, prior to performing stimulation treatments, forming gravel packs, etc. If such materials are not removed, they can be carried into producing formations and reduce the production of hydrocarbons therefrom by plugging formation pores and flow channels.
  • DE-A-3316988 discloses a cleaning agent for cleaning machines, especially for the paper, cardboard; carton and pulp industries.
  • the cleaning agent may include D-limonene, dipentene and additional terpenes and an uncharacterised compatible surfactant.
  • the invention provides a method of removing contaminant materials such as pipe dopes and thread lubricants from a metal surface, which method comprises contacting the metal surface with a nonaqueous solvent for the contaminants to dissolve them in the composition, said solvent composition comprising a surface active agent for breaking up and dispersing the contaminants, and D-limonene and a mixture of other terpenes predominantly including dipentene for dissolving said contaminants, wherein the surface active agent is an alkyl naphthalene sulfonate diisopropyl amine salt, sodium di-2-ethylhexyl sulfosuccinate, or a blend of coco-diethanolamide and coco-sulfosuccinate.
  • the environmentally friendly nonaqueous solvent compositions of the present invention are particularly effective in removing materials such as commercial thread lubricants, metal-containing pipe dopes and metal-free pipe dopes. As mentioned, it is essential that such materials be removed from the surfaces of tubing and casing disposed in a well bore prior to performing producing formation stimulation treatments, forming gravel packs in the well or performing any other treatment or procedure whereby the materials may be carried into producing formations. If such materials are not removed, they can be carried into producing formations or gravel packs whereby hydrocarbon flow pores and channels are plugged.
  • the environmentally friendly nonaqueous solvent compositions of the present invention are basically comprised of surface active agent as defined in claim 1 for breaking up and dispersing the materials to be removed by the solvent composition, D-limonene and a mixture of other terpenes predominantly including dipentene for dissolving the materials.
  • Terpenes are unsaturated hydrocarbons having the formula C 10 H 16 which may be either acyclic or cyclic with one or more benzenoid groups. They are highly effective solvents and are not harmful to the environment.
  • a particularly suitable mixture of terpenes for use in accordance with the present invention predominantly includes dipentene and D-limonene.
  • Such a mixture which is presently preferred is comprised of a commercial mixture of dipentene and other terpenes from a paper pulping process and commercial D-limonene.
  • the commercial mixture of dipentene and other terpenes from a paper pulping process is commercially available from the Halliburton Company of Duncan, Oklahoma, under the trade designation "PARAGON 1 E + TM" and has the following composition.
  • the commercial D-limonene is available, for example, from the Florida Chemical Company of Lake Alfred, Florida.
  • the surfactants are selected from the group consisting of an alkyl naphthalene sulfonate diisopropyl amine salt, sodium di-2-ethylhexyl sulfosuccinate and a blend of coco-diethanolamide and coco-sulfosuccinate.
  • the alkyl naphthalene sulfonate diisopropyl amine salt surface active agent is commercially available, for example, from Champion Technologies, Inc. of Houston, Texas.
  • the sodium di-2-ethylhexyl sulfosuccinate surface active agent is commercially available from Witco Chemical Company of Houston, Texas.
  • the blend of coco-diethanolamide and coco-sulfosuccinate surface active agent is commercially available from Mona Chemical Company of Paterson, New Jersey.
  • a preferred nonaqueous solvent composition of the present invention which is a liquid blend is comprised of one of the surface active agents described above present in an amount in the range of from about 5% to about 25% by volume of the composition, D-limonene present in an amount in the range of from about 5% to about 90% by volume of the composition, and a mixture of other terpenes predominantly including dipentene present in an amount in the range of from about 5% to about 90% by volume of the composition.
  • the most preferred liquid blend solvent composition is comprised of an alkyl naphthalene sulfonate diisopropyl amine salt surface active agent present in an amount of about 15% by volume of the composition, D-limonene present in an amount of about 35% by volume of the composition, and a mixture of other terpenes predominantly including dipentene present in an amount of about 50% by volume of the composition.
  • the nonaqueous solvent compositions of this invention preferably include glacial acetic acid to react with metals and other reactive components in the pipe dopes and other materials to be removed and facilitate the dispersal of the materials.
  • glacial acetic acid When glacial acetic acid is included, the solvent composition is preferably formed into an emulsion which prevents the acid from spending too quickly.
  • a preferred composition including acetic acid is comprised of a surface active agent of the type described above present in an amount in the range of from about 5% to about 25% by volume of the composition, D-limonene present in an amount in the range of from about 5% to about 90% by volume of the composition, a mixture of other terpenes predominantly including dipentene present in an amount in the range of from about 5% to about 90% by volume of the composition, and glacial acetic acid present in an amount in the range of from about 5% to about 25% by volume of the composition.
  • a particularly preferred emulsified nonaqueous solvent composition containing glacial acetic acid of this invention is comprised of a blend of coco-diethanolamide and cocosulfosuccinate present in an amount of about 20% by volume of the composition, D-limonene present in an amount of about 10% by volume of the composition, a mixture of other terpenes predominantly including dipentene present in an amount of about 60% by volume of the composition, and glacial acetic acid present in an amount of about 10% by volume of the compositions.
  • the solvent composition can be circulated down the tubing and up the annulus between the tubing and the casing for a time period sufficient to remove the materials from the tubing and casing surfaces.
  • small quantities of formation fluids, including water may become admixed with the solvent, however such compositions remain substantially nonaqueous during the time period over which it removes the lubricants or pipe dopes.
  • Other techniques can also be utilized such as pumping the nonaqueous solvent composition into the tubing and annulus, and after the required time period, displacing the solvent composition containing dissolved materials to the surface with produced fluids.
  • the nonaqueous solvent compositions of this invention are caused to contact surfaces containing the materials to be removed for time periods in the range of from about 5 minutes to about 20 minutes so that substantially all of the materials are dissolved in the solvent compositions.
  • a liquid blend nonaqueous solvent composition which does not contain acetic acid is utilized or a stable emulsified nonaqueous solvent composition containing acetic acid is utilized.
  • the emulsified composition with acetic acid is utilized where the materials to be removed contain acid reactive materials such as metal particles and the like.
  • Pipe dopes described in Table III below were obtained for testing. As shown, the pipe dopes included two metal containing pipe dopes, two conventionally used proprietary mixture pipe dopes, and two metal free, environmentally safe pipe dopes. TABLE III Pipe Dopes Tested Pipe Dope No. Pipe Dope Description Trade Designation And Commercial Source PD-1 Proprietary Mixture "LIQUID-O-RING 300TM” Oil Center Research, Inc. of Lafayette, LA. PD-2 Mixture of grease, oil, lead, zinc, copper, graphite, talc and lime API MODIFIED Pipe Dope RSR Corporation of Dallas, TX. PD-3 Proprietary Mixture "LUBON 404TM” Oil Center Research, Inc. of Lafayette, LA.
  • a volume of 200 milliliters of the solvent composition to be tested was placed in a 300 milliliter beaker.
  • a magnetic stirring bar was inserted, and the beaker was placed on a magnetic stirrer.
  • Coupons cut from N-80 steel having dimensions of 15.2 cm (6") (length) x 5.1 cm (2") (width) x 0.318 cm (1/8") (thickness) were utilized in the tests.
  • a coupon was first weighed, and then a small amount of the pipe dope to be removed was smeared on the coupon on one side and at one end thereof. The coupon was reweighed to determine the exact weight of the pipe dope. Approximately 3 grams of pipe dope were used in each test.
  • the coupon was then suspended in the solvent composition in the 300 milliliter beaker with the end containing the pipe dope submerged in the solvent composition.
  • the solvent composition was agitated by the magnetic stirrer for 5 minutes at ambient conditions.
  • the coupon was then removed from the beaker and gently rinsed with distilled water. Excess water was blotted with a paper towel, and the coupon was dried in an oven at 93.3°C (200°F) for 15 minutes. After removing the coupon from the oven, it was allowed to cool to ambient temperature. A final weight was then determined and the percentage of pipe dope removed was calculated. If less than 100% of the pipe dope was removed, the test was repeated up to a maximum of 20 minutes in 5 minute intervals using the same coupon and the remaining pipe dope until the 20 minutes had expired or 100% of the pipe dope had been removed. The results of the tests are set forth in Tables IV through IX below.
  • reagent grade xylene, solvent composition S1 was effective in removing at least 90% of the API MODIFIED pipe dope in 5 minutes.
  • Commercially available D-Limonene, S4 was effective in removing at least 90% of the pipe dope in 10 minutes.
  • Solvent compositions S12, S29, S30 and S31 all removed at least 90% of the API MODIFIED Pipe Dope within 10 minutes.
  • reagent grade xylene, S1, and commercial D-Limonene, S4 were effective in removing at least 90% of "LUBON 404TM” thread lubricant in 15 minutes.
  • Solvent composition S31 was effective in removing at least 90% of the "LUBON 404TM” after 15 minutes and solvent composition S29 removed at least 90% of the lubricant after 20 minutes.
  • solvent composition S24 was effective in removing at least 90% of the "KOPR-KOTETM" Pipe Dope after 10 minutes.
  • Solvent compositions S23, S25, S29, S30 and S31 were all effective in removing at least 90% of the pipe dope after 15 minutes.
  • Solvent compositions S18 and S28 were effective in removing at least 90% after 20 minutes.
  • the most consistent solvent compositions in removing the metal containing pipe dopes, i.e., API MODIFIED Pipe Dope (Table V) and "KOPR-KOTETM" Pipe Dope (Table VII) were solvent compositions S24 and S31.
  • Reagent Grade Xylene, S1 was effective in removing at least 90% of the environmentally safe, metal free "LOS-MODIFIEDTM" Pipe Dope after 10 minutes.
  • Commercially available D-Limonene, S4 was effective in removing at least 90% of the pipe dope after 15 minutes.
  • Solvent composition S25 was effective in removing at least 90% of the pipe dope after 15 minutes while blends S24, S29 and S30 were effective in removing at least 90% after 20 minutes.
  • emulsions S23, S24 and S25 and liquid blends S29, S30 and S31 were subjected to thermal stability tests at 93.3°C (200°F) in a hot water bath for 6 hours. There was no separation or layering out of the various components during this time period and no change in appearance was observed.
  • Samples 1-4 each visibly separated within less than four hours. Sample 5 prepared in accordance with the present invention showed no visible signs of separation. Thus it is apparent that Samples 1-4 did not comprise a stable emulsion.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Metallurgy (AREA)
  • Mechanical Engineering (AREA)
  • Materials Engineering (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Detergent Compositions (AREA)
  • Lubricants (AREA)

Claims (7)

  1. Methode zur Entfernung von Schmutzstoffen von einer Metalloberfläche, welche Methode folgendes umfaßt: in Berührung bringen der Metalloberfläche mit einem nichtwässrigen Lösungsmittel, damit die Schmutzstoffe in der Zusammensetzung gelöst werden, wobei die Lösungsmittelzusammensetzung ein oberflächenaktives Mittel zum Auflösen und Dispergieren der Schmutzstoffe und D-Limonen und eine Mischung anderer Terpene enthält, wobei letztere hauptsächlich Dipenten zum Auflösen der Schmutzstoffe enthält, wobei das oberflächenaktive Mittel aus einem Alkylnaphthalinsulfonatdiisopropylaminsalz,Natriumdi-2-ethylhexylsulfosuccinatoder einer Mischung von Kokosdiethanolamid und Kokossulfosuccinat besteht.
  2. Methode nach Anspruch 1, bei der die Mischung anderer Terpene folgende umfaßt, wobei jedes auf das Volumen der Mischung bezogen ist: 25% Dipenten, 17% α-Pinen, 16% 1,4-Cineol, 11% 1,8-Cineol, 10% Terpinolen, 8% Camphen, 7% α-Terpinen, 5% γ-Terpinen and 1% para-Cymol.
  3. Methode nach Anspruch 1 oder 2, bei der die Zusammensetzung des weiteren folgendes, auf das Volumen der Zusammensetzung bezogen, enthält: 5% bis 25% des oberflächenaktiven Mittels, 5% bis 90% D-Limonen und 5% bis 90% der Mischung anderer Terpene, einschließlich Dipenten.
  4. Methode nach einem der vorhergehenden Ansprüche, bei der die nichtwässrige Lösungsmittelzusammensetzung des weiteren Eisessig zur Reaktion mit den Stoffen enthält und die Zusammensetzung durch Vermischen des D-Limonens und der Mischung von Terpenen mit dem oberflächenaktiven Mittel vor dem in Berührung bringen mit dem Eisessig in eine Emulsion überführt wird.
  5. Methode nach Anspruch 4 bei der der Eisessig in einer Menge von 5 bis 25 Vol.-% der Zusammensetzung vorliegt.
  6. Methode nach Anspruch 4 oder 5, bei der die Bestandteile in einer auf das Volumen der Zusammensetzung bezogenen Menge wie folgt vorliegen: 20% oberflächenaktives Mittel, wobei das oberflächenaktive Mittel eine Mischung von Kokosdiethanolamid und Kokossulfosuccinat ist, 10% D-Limonen, 60% der Mischung anderer Terpene, einschließlich Dipenten, und 10% Eisessig.
  7. Methode nach Anspruch 1, 2 oder 3, bei der das oberflächenaktive Mittel ein Alkylnaphthalinsulfonatdiisopropylaminsalz ist, das in einer Menge von 15 Vol-% der Zusammensetzung vorliegt, wobei das D-Limonen in einer Menge von 35 Vol.-% der Zusammensetzung vorliegt und die Mischung anderer Terpene, einschließlich des Dipentens, in einer Menge von 50 Vol.-% der Zusammensetzung vorliegt.
EP19950304632 1994-07-18 1995-07-03 Verfahren zur Entfernung von Verunreinigungen von Metalloberflächen Expired - Lifetime EP0697471B1 (de)

Applications Claiming Priority (4)

Application Number Priority Date Filing Date Title
US27614594A 1994-07-18 1994-07-18
US276145 1994-07-18
US08/437,709 US5489394A (en) 1994-07-18 1995-05-09 Solvent compositions and methods
US437709 2003-05-14

Publications (2)

Publication Number Publication Date
EP0697471A1 EP0697471A1 (de) 1996-02-21
EP0697471B1 true EP0697471B1 (de) 1997-11-12

Family

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Family Applications (1)

Application Number Title Priority Date Filing Date
EP19950304632 Expired - Lifetime EP0697471B1 (de) 1994-07-18 1995-07-03 Verfahren zur Entfernung von Verunreinigungen von Metalloberflächen

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EP (1) EP0697471B1 (de)
DE (1) DE69501023D1 (de)
NO (1) NO315478B1 (de)

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6564869B2 (en) * 2001-07-16 2003-05-20 M-I, L.L.C. Method and composition for cleaning and inhibiting solid, bitumin tar, and viscous fluid accretion in and on well equipment
GB2405639A (en) * 2003-09-08 2005-03-09 R Mc Power Recovery Ltd Metal cleaning compositions
EP3696239A1 (de) * 2019-02-18 2020-08-19 Sabine Berteina-Raboin Verwendung von eukalyptol und zusammensetzungen damit

Family Cites Families (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3437146A (en) * 1968-01-11 1969-04-08 Midwest Chem & Processing Co I Method of removing paraffin from a well with heated solvent
DE3316988C2 (de) * 1983-05-10 1986-07-17 Jürgen 6926 Kirchardt Rohrmoser Verfahren zum Reinigen von Vorrichtungen und Maschinen der Papier-, Pappe- und Zellstoff-Industrie
US4640719A (en) * 1985-07-01 1987-02-03 Petroleum Fermentations N.V. Method for printed circuit board and/or printed wiring board cleaning
US4983224A (en) * 1988-10-28 1991-01-08 Rd Chemical Company Cleaning compositions and methods for removing soldering flux
US5031648A (en) * 1989-05-16 1991-07-16 Skyline Products Ltd. Cleaning of mill gears
JPH036300A (ja) * 1989-05-31 1991-01-11 Shokichiro Urayama 油溶性洗浄剤
DE69004521T2 (de) * 1989-08-07 1994-05-05 Du Pont Reinigungsmittel auf der Basis eines dibasischen Esters und eines Kohlenwasserstofflösungsmittels und Reinigungsverfahren.
JPH03212500A (ja) * 1990-01-18 1991-09-18 Nippon Alpha Metals Kk 金属表面用洗浄組成物
CA2097936A1 (en) * 1990-12-07 1992-06-08 C. Richard Hamilton Method for finishing metal surfaces with terpene

Also Published As

Publication number Publication date
NO315478B1 (no) 2003-09-08
DE69501023D1 (de) 1997-12-18
NO952766D0 (no) 1995-07-12
EP0697471A1 (de) 1996-02-21
NO952766L (no) 1996-01-19

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