US3923541A - Vapor degreasing system - Google Patents

Vapor degreasing system Download PDF

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Publication number
US3923541A
US3923541A US371836A US37183673A US3923541A US 3923541 A US3923541 A US 3923541A US 371836 A US371836 A US 371836A US 37183673 A US37183673 A US 37183673A US 3923541 A US3923541 A US 3923541A
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US
United States
Prior art keywords
rosin
vapor
solvent
water
phase
Prior art date
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Expired - Lifetime
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US371836A
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English (en)
Inventor
Robert Michael Healy
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Northrop Grumman Guidance and Electronics Co Inc
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Litton Systems Inc
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Publication date
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Priority to US371836A priority Critical patent/US3923541A/en
Priority to CA199,518A priority patent/CA996843A/en
Publication of USB371836I5 publication Critical patent/USB371836I5/en
Application granted granted Critical
Publication of US3923541A publication Critical patent/US3923541A/en
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/10—Cleaning involving contact with liquid with additional treatment of the liquid or of the object being cleaned, e.g. by heat, by electricity or by vibration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B08—CLEANING
    • B08B—CLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00—Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04—Cleaning involving contact with liquid
    • B08B3/08—Cleaning involving contact with liquid the liquid having chemical or dissolving effect
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S134/00—Cleaning and liquid contact with solids
    • Y10S134/902—Semiconductor wafer

Definitions

  • the solvent system comprises an aqueous solution B 37 l 3 of a base of sufficient strength to saponify the organic acid on the items to be cleaned. and an organic sol- U-S. Cl. ent the aqueous solution The so].
  • 134/105; 134/108; 252/369 vent is boiled and forms a vapor phase consisting of Int. Clthe vapors of the rganic olvents and water vapor of Search 35, 40, 3O, 1O, vapor phase contacts the enclosed item
  • organic solvent dissolves the rosin and. by condensal l References Cited tion, the solution of rosin in organic solvent drips back UNITED STATES PATENTS into the turbulating liquid phase where it is contacted 2,1 l3,l29 4/l938 Dinley l34/l1 by the base- The base sapohifies the rosin; the result- 2 2g5 333 9 3 Humphmy 252 3 9 X ing soap is the waste of the process. The soap dissolves 3,070,463 12/1962 Barday 134/11 in the water, and the organic solvent is available again 3.0859 8 4/1963 Sh i t al- 134/30 in the cleaning system.
  • VAPOR DEGREASING SYSTEM FIELD OF THE INvENTIoN This invention relates to an improved two-phase vapor degreasing system and, more peularly,,-to an improved vapor degreasing system in which the major part of the resulting waste products is biodegradable.
  • a vapor degreaser or vapor degreasing -system includes a covered vat or other closed chamber, sometimes technically referred to as a refluxing chamber, containing a liquid solvent.
  • the items to be cleaned are placed in the upper portion of said chamber and the solvent is heated to-form a solvent vapor within the upper part of the chamber above the turbulating liquid.
  • the vapor dissolves the residues on the item and effectively washes such residues from the confined items; the condensate drips down into the liquid phase.
  • the cleaned items are thereupon removed from the chamber.
  • Various means are known for automatically inserting and removing items and for automatically heating the liquid solvents. The reader may make reference to the literature for the details of their.
  • a degreasing system in which the part to be cleaned is treated in a two-phase liquid system containingessentially a chlorinated hydrocarbon, for example trichloroethylene, perchloroethylene, methylene chloride or I l l -tricholoroethane containing a small amount of cationic surface active agent and a proportion of water. That process also leaves a waste in the organic phase which is not biodegradable.
  • a chlorinated hydrocarbon for example trichloroethylene, perchloroethylene, methylene chloride or I l l -tricholoroethane containing a small amount of cationic surface active agent and a proportion of water.
  • aqueous cleaners or solvents do appear on the market which convert resinous acids to watersoluble biodegradable soaps.
  • the disadvantage of these solvents is that they cannot be used in a vapor degreaser to vapor clean.
  • the parts to be cleaned must be in contact 2. with the. liquid phase of the'solvent.
  • a solvent is used in a washing machine" type of operation in which the item to becleaned is immersed in turbulent solution whic-hwashes and dissolves the residue.
  • the vapor degreaser solvent system of may invention exists in two phases in the liquid state: an aqueous phase, comprising water and a base of-low volatility of sufficient strength to saponify the organic acid to be removed from the object to be cleaned; and an organic solvent liquid immis proficient with water, which may be a halogenated hydrocarbon or mixture thereof. Minor amounts of anti-foam agents and volatile wetting agents, such as alcohol, may be included. Additionally, aliphatic hydrocarbons may be included in the organic solvent to alter the boiling temperature of the solvent system.
  • the solvent system is placed in a refluxing chamber and the system is heated and turbulated to form a vapor phase comprising the organic compounds and some water'vapor, but not the base, which is of low volatility and does not vaporize.
  • the vapor wets the contaminated parts, installed in the upper part of the refluxing chamber and the organic solvent thereby dissolves the rosin or other organic compounds and the water dissolves any salts or inorganic acids; the condensate drips back into the-turbulating liquid.
  • any acid present comes in contact with the base and thence chemically combines with the base to form a salt or soap-The soap, soluble in water, dissolves in the water contained within the two-phase liquid system.
  • the soapy water may be drawn off and disposed ofin the utility sewer system.
  • a closed chamber I sometimes termed a refluxing chamber, is illustrated symbolically in the FIGURE.
  • the chamber is closed with a cover 2 and a tray 3 is suspended by wires 4 from the cover.
  • the chamber is filled to a predetermined depth with the liquid cleaning solvent system 7, which is in two phases, 7a and 7b, as becomes more apparent, so as to leave unfilled the upper portion of the chamber.
  • a source of heat represented symbolically by a heating rod, which is a conventional electric heating device 9, is provided.
  • a condensing coil 6 is conventional structure is included in the upper part of the chamber.
  • the condensing coil is typically hollow metal tubing and a source -of coolant, not illustrated, pumps coolant through the tubing to enhance condensationv This device removes heat from the vapor, thus permitting a high condensation rate.
  • a reservoir for replenishing solvent is shown symbolically as 8.
  • the reservoir is connected by piping, illustrated by lines through a valve 11, to chamber 1.
  • a settling vessel 12 a slight modification to a conventional degreaser, is connected by a pipe 13 and valve 14 to one part of the chamber containing phase 7a and is connected by pipe 15 and valve 16 to a lower part of the chamber, containing phase 7b.
  • An outlet pipe 17 is located in the upper part of settling tank and a valve 18 closes the pipe.
  • Liquid solvent 7 is a two-phase liquid solvent in that it comprises at least two liquids which are immiscible in one another and whichin the quiescent state separates into two phases or layers, 70 and 7b.
  • liquid layer 7b is an organic cleaning solvent substantially immiscible in water.
  • This phase contains halogenated hydrocarbons, which are insoluble in water, and, by way of example, commercially available dichoromethane, tetrachloroethylene, trichloromonofluoromethane, trichlorotrifluorethanes, and tetrachlorodifluoroethanes.
  • Liquid layer 7a is largely water and a strong organic or inorganic base of low volatility, such as an alkali metal or alkaline earth metal hydroxide, diethanol amine, or an alkali metal silicate or carbonate.
  • a strong organic or inorganic base of low volatility such as an alkali metal or alkaline earth metal hydroxide, diethanol amine, or an alkali metal silicate or carbonate.
  • liquid phase 7a may contain additionally additives which reduce foaming and for other purposes.
  • the item to be cleaned of contaminants such as rosin or resin
  • the tray 3 is inserted on the tray 3 and is therein suspended above the liquid solvent 7.
  • the container is covered so as to prevent the escape of vapors.
  • heater 9 is operated to heat the contents of the chamber 1 and the liquid solvent 7 is brought to a boil.
  • the liquid 7 is thus turbulated so as to intermix the two phases, 7a and 7b, and a portion of the cleaning liquid 7 is vaporized.
  • the vapor consists primarily of the organic solvent from phase 7b and some parts of water. Inasmuch as the base is of low volatility it remains in the turbulating liquid solution and does not vaporize.
  • the organic solvent vapors condense upon item 5 and dissolve any rosin residues thereon.
  • the water vapor or vapor of any other polar compound, such as alcohol, as may be present aids in dissolving any salts present as a contaminant in the rosin.
  • the condensed solvent containing the dissolved impurity drips back into the turbulating liquid phases 7 and thence comes into contact with the base.
  • the contaminant to be an organic acid, such as resin or rosin referred to above
  • the base chemically reacts with and saponifies the rosin, forming an organic salt, commonly termed a soap.
  • the soap is soluble in water and accordingly this in turn is dissolved in the aqueous phase of the turbulating liquid.
  • the solvents 7 may be allowed to cool and separate again into two layers, 7a and 7b in the settling chamber.
  • the aqueous phase may be drawn off via the settling chamber 12 as necessary to remove the soap and dissolved salts.
  • the valves 14 and 16 are opened to allow the liquid phases to fill the settling tank 12 and the valves are again closed.
  • valve 18 is opened to allow a part of the liquid phase 7a to run out outlet 17.
  • the major part of drawn-off solution is of low toxicity, is biodegradable, and is miscible with ordinary water. Accordingly it may be deposited in the utility sewer system.
  • the organic solvent remains in the vapor degreaser. Additional aqueous phase may be added when necessary to replenish the portions drawn off. And, occasionally, the small losses of the organic phase due to drag out and vapor loss may be replenished.
  • the two-phase liquid solvent used in my invention is further illustrated by the following examples.
  • the rosin is inserted as a contaminant residue directly into the liquid for ease of experiment. The action of the rosin is thus speeded up.
  • those examples serve as a valid demonstration of the solvent as applied in a vapor degreaser.
  • the contaminant 15 grams WW grade gum rosin
  • the flask was covered and the mixture was refluxed for a period of approximately 8 hours. Thereafter the mix ture was cooled and allowed to settle whereupon the liquids separated into two phases or layers of liquid.
  • the upper layer was clear brown in color.
  • the lower layer was water white.
  • the pH factor of the upper lay was Ca. 12.8.
  • the contaminant 6.7 grams WW rosin
  • the contents were heated, brought to a boil and allowed to reflux for a period of approximately 8 hours.
  • the boiling point of the mixture was 76 Centigrade.
  • the solution was allowed to cool and settle and the liquid thereupon separated into two layers or phases.
  • the upper phase was colored clear brown.
  • the lower phase was colored water white.
  • the pH factor of the upper layer was 12.6. This also demonstrates that the rosin placed into the mixture was dissolved and had been quantitatively saponifled and transferred to the aqueous phase.
  • the contents were mixed in a round bottom glass flask and covered.
  • the flask was placed upon a heater, the contents were brought to a boil and were refluxed for a period of approximately 6 hours. Thereupon the flask was removed from the heater and the contents allowed to cool and settle. Thereafter the contents separated into two distinct layers.
  • the upper layer was a clear brown color and had a pH factor of 12.8.
  • the bottom layer was water white in color.
  • the system may also contain anti-foam agents, well known to those versed in the art, and as such commercially available.
  • volatile wetting agents such as alcohols
  • volatile wetting agents such as alcohols
  • organic phase may contain aliphatic hydrocarbons such as hexane, heptane, etc. These are useful to alter the boiling temperature of the system, and the melting point of organic solvent. They are also, in general, less costly than the halocarbons and should be used in proportions small enough so that the system does not become flammable.
  • the aqueous phase, water included amounts of foam-reducing additives and wetting agents such as n-propanol.
  • the organic layer had various examples of solvents which may generically be termed halogenated hydrocarbons and suitable hydrocarbon additives.
  • the base which was mixed with the water, is of low volatility. Essentially the base employed must be strong with respect to the organic salt, the soap, which is to be formed upon a combination of the base with the organic acid, such as rosin.
  • said vapor degreaser having a two-phase liquid solvent located in the sump thereof, said two-phase liquid solvent comprising a first liquid containing an organic solvent and a second liquid containing water and an inorganic base of low volatility, said inorganic base being sufficiently strong to neutralize said organic acid materials, and said first and second liquids being immiscible in one another; heating said mixture to boil said two-phase liquid solvent wherein said solvent is in a state of turbulance and a vapor of water and organic solvent is created in said vapor section and refluxing said mixture,

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Detergent Compositions (AREA)
  • Cleaning By Liquid Or Steam (AREA)
US371836A 1973-06-20 1973-06-20 Vapor degreasing system Expired - Lifetime US3923541A (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
US371836A US3923541A (en) 1973-06-20 1973-06-20 Vapor degreasing system
CA199,518A CA996843A (en) 1973-06-20 1974-05-10 Vapor degreasing method and system

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US371836A US3923541A (en) 1973-06-20 1973-06-20 Vapor degreasing system

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USB371836I5 USB371836I5 (enrdf_load_stackoverflow) 1975-01-28
US3923541A true US3923541A (en) 1975-12-02

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Cited By (20)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4478364A (en) * 1980-11-07 1984-10-23 Re-Al, Inc. Method of mounting and cleaning electrical slide switch of flush through design
US4788043A (en) * 1985-04-17 1988-11-29 Tokuyama Soda Kabushiki Kaisha Process for washing semiconductor substrate with organic solvent
US4935066A (en) * 1988-02-19 1990-06-19 Wright C E Process for decomposing baked-on grease or oil
US5055138A (en) * 1988-07-08 1991-10-08 Isc Chemicals Limited Cleaning and drying of electronic assemblies
US5056174A (en) * 1986-07-17 1991-10-15 Mitsubishi Jukogyo K.K. Dry cleaning method and apparatus
US5156173A (en) * 1991-05-14 1992-10-20 Envirosolv High-efficiency, low-emissions cleaning method and apparatus
US5183067A (en) * 1988-07-08 1993-02-02 Isc Chemicals Limited Cleaning and drying of electronic assemblies
US5402806A (en) * 1993-10-19 1995-04-04 Northrop Grumman Corporation Cleaning apparatus having a partitioned boil sump
JPH0771661B2 (ja) 1991-11-22 1995-08-02 ジャパン・フィールド株式会社 油分が付着した被洗浄物の洗浄方法
US5482563A (en) * 1993-04-06 1996-01-09 Motorola, Inc. Method for electrical assembly cleaning using a non-azeotropic solvent composition
US5534078A (en) * 1994-01-27 1996-07-09 Breunsbach; Rex Method for cleaning electronic assemblies
USRE35975E (en) * 1988-07-08 1998-12-01 Rhone-Poulenc Chimie Cleaning and drying of electronic assemblies
US5894851A (en) * 1997-05-12 1999-04-20 Hartman; Albert V. Refrigerated vapor degreasing method
US6303500B1 (en) 1999-02-24 2001-10-16 Micron Technology, Inc. Method and apparatus for electroless plating a contact pad
US6412501B1 (en) * 1999-06-29 2002-07-02 Kimmon Quartz Co., Ltd. Drying apparatus and drying method
US6616769B2 (en) * 2001-09-28 2003-09-09 Air Products And Chemicals, Inc. Systems and methods for conditioning ultra high purity gas bulk containers
FR2878423A1 (fr) * 2004-11-30 2006-06-02 Jacques Puech Degraisse broches
US20070077769A1 (en) * 1997-02-14 2007-04-05 Interuniversitair Micro-Elektronica Centrum Vzw Method of removing organic contaminants from a semiconductor surface
TWI495519B (zh) * 2012-06-08 2015-08-11 Japan Field Kk 被清洗物之蒸汽清洗方法及其裝置
CN104923520A (zh) * 2015-06-24 2015-09-23 西安航空动力股份有限公司 经磨粒流加工后的涡轮叶片残留磨料的清洗方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2113129A (en) * 1934-05-15 1938-04-05 Solvent Machine Company Treatment of work with solvents
US2285333A (en) * 1940-12-31 1942-06-02 Hercules Powder Co Ltd Rosin-containing soaps
US3070463A (en) * 1961-06-08 1962-12-25 Donald J Barday Solvent recovering and purifying method and apparatus
US3085918A (en) * 1959-05-22 1963-04-16 Ici Ltd Cleaning process
US3094469A (en) * 1958-07-12 1963-06-18 Dehydag Gmbh Process for cleaning metal objects
US3733218A (en) * 1971-11-15 1973-05-15 Diamond Shamrock Corp Removal of solder flux with azeotropic solvent mixtures

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2113129A (en) * 1934-05-15 1938-04-05 Solvent Machine Company Treatment of work with solvents
US2285333A (en) * 1940-12-31 1942-06-02 Hercules Powder Co Ltd Rosin-containing soaps
US3094469A (en) * 1958-07-12 1963-06-18 Dehydag Gmbh Process for cleaning metal objects
US3085918A (en) * 1959-05-22 1963-04-16 Ici Ltd Cleaning process
US3070463A (en) * 1961-06-08 1962-12-25 Donald J Barday Solvent recovering and purifying method and apparatus
US3733218A (en) * 1971-11-15 1973-05-15 Diamond Shamrock Corp Removal of solder flux with azeotropic solvent mixtures

Cited By (28)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4478364A (en) * 1980-11-07 1984-10-23 Re-Al, Inc. Method of mounting and cleaning electrical slide switch of flush through design
US4788043A (en) * 1985-04-17 1988-11-29 Tokuyama Soda Kabushiki Kaisha Process for washing semiconductor substrate with organic solvent
US5056174A (en) * 1986-07-17 1991-10-15 Mitsubishi Jukogyo K.K. Dry cleaning method and apparatus
US4935066A (en) * 1988-02-19 1990-06-19 Wright C E Process for decomposing baked-on grease or oil
US5183067A (en) * 1988-07-08 1993-02-02 Isc Chemicals Limited Cleaning and drying of electronic assemblies
US5055138A (en) * 1988-07-08 1991-10-08 Isc Chemicals Limited Cleaning and drying of electronic assemblies
USRE35975E (en) * 1988-07-08 1998-12-01 Rhone-Poulenc Chimie Cleaning and drying of electronic assemblies
US5156173A (en) * 1991-05-14 1992-10-20 Envirosolv High-efficiency, low-emissions cleaning method and apparatus
JPH0771661B2 (ja) 1991-11-22 1995-08-02 ジャパン・フィールド株式会社 油分が付着した被洗浄物の洗浄方法
US5482563A (en) * 1993-04-06 1996-01-09 Motorola, Inc. Method for electrical assembly cleaning using a non-azeotropic solvent composition
US5402806A (en) * 1993-10-19 1995-04-04 Northrop Grumman Corporation Cleaning apparatus having a partitioned boil sump
US5534078A (en) * 1994-01-27 1996-07-09 Breunsbach; Rex Method for cleaning electronic assemblies
US20070077769A1 (en) * 1997-02-14 2007-04-05 Interuniversitair Micro-Elektronica Centrum Vzw Method of removing organic contaminants from a semiconductor surface
US5894851A (en) * 1997-05-12 1999-04-20 Hartman; Albert V. Refrigerated vapor degreasing method
US6346151B1 (en) * 1999-02-24 2002-02-12 Micron Technology, Inc. Method and apparatus for electroless plating a contact pad
US20060017163A1 (en) * 1999-02-24 2006-01-26 Tongbi Jiang Device having contact pad with a conductive layer and a conductive passivation layer
US6451116B2 (en) 1999-02-24 2002-09-17 Micron Technology, Inc. Apparatus for electroless plating a contact pad
US20080142983A1 (en) * 1999-02-24 2008-06-19 Tongbi Jiang Device having contact pad with a conductive layer and a conductive passivation layer
US6630400B2 (en) 1999-02-24 2003-10-07 Micron Technology, Inc. Method for electroless plating a contact pad
US20040087142A1 (en) * 1999-02-24 2004-05-06 Tongbi Jiang Method for electroless plating a contact pad
US6967164B2 (en) 1999-02-24 2005-11-22 Micron Technology, Inc. Method for electroless plating a contact pad
US7358185B2 (en) 1999-02-24 2008-04-15 Micron Technology, Inc. Device having contact pad with a conductive layer and a conductive passivation layer
US6303500B1 (en) 1999-02-24 2001-10-16 Micron Technology, Inc. Method and apparatus for electroless plating a contact pad
US6412501B1 (en) * 1999-06-29 2002-07-02 Kimmon Quartz Co., Ltd. Drying apparatus and drying method
US6616769B2 (en) * 2001-09-28 2003-09-09 Air Products And Chemicals, Inc. Systems and methods for conditioning ultra high purity gas bulk containers
FR2878423A1 (fr) * 2004-11-30 2006-06-02 Jacques Puech Degraisse broches
TWI495519B (zh) * 2012-06-08 2015-08-11 Japan Field Kk 被清洗物之蒸汽清洗方法及其裝置
CN104923520A (zh) * 2015-06-24 2015-09-23 西安航空动力股份有限公司 经磨粒流加工后的涡轮叶片残留磨料的清洗方法

Also Published As

Publication number Publication date
CA996843A (en) 1976-09-14
USB371836I5 (enrdf_load_stackoverflow) 1975-01-28

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