DE3933874A1 - Modifying surface of polyolefin containers - by exposing container to low pressure plasma in fluorine-contg. gas atmos. - Google Patents
Modifying surface of polyolefin containers - by exposing container to low pressure plasma in fluorine-contg. gas atmos.Info
- Publication number
- DE3933874A1 DE3933874A1 DE19893933874 DE3933874A DE3933874A1 DE 3933874 A1 DE3933874 A1 DE 3933874A1 DE 19893933874 DE19893933874 DE 19893933874 DE 3933874 A DE3933874 A DE 3933874A DE 3933874 A1 DE3933874 A1 DE 3933874A1
- Authority
- DE
- Germany
- Prior art keywords
- fluorine
- containers
- contg
- low pressure
- pressure plasma
- 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- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
- C08J7/12—Chemical modification
- C08J7/126—Halogenation
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
Abstract
Description
Behälter aus Polyolefin weisen mitunter den Nachteil auf, daß sie zur Aufbewahrung bestimmter organischer Flüssigkeiten wenig geeignet oder ungeeignet sind, sofern sie diese Flüssigkeiten durchlassen, beispielsweise Kraftstoffe, wie Benzin.Polyolefin containers sometimes have the disadvantage that they are little for the storage of certain organic liquids suitable or unsuitable, provided they contain these liquids let through, for example, fuels, such as gasoline.
Es ist jedoch bereits bekannt, daß die Permeabilität von Behältern aus Polyolefin gegenüber derartigen organischen Flüssigkeiten dadurch verbessert werden kann, daß man sie einer Fluoratmosphäre aussetzt. Auf die starke Umweltbelastung dieses Stands der Technik muß nicht näher eingegangen werden.However, it is already known that the permeability of containers polyolefin over such organic liquids can be improved by giving it one Exposed to fluorine atmosphere. On the strong environmental impact of this State of the art need not be discussed in more detail.
Erfindungsgemäß wird nun ein Verfahren zur Oberflächenmodifizierung von Behältern aus Polyolefin vorgeschlagen, bei dem man ein oder mehrere derartige Behälter einem Niederdruckplasma in einer ein fluorhaltiges Gas aufweisenden Atmosphäre aussetzt. Unter dem Ausdruck "fluorhaltiges Gas" soll Fluor selbst nicht verstanden werden.According to the invention, a method for surface modification is now provided proposed by containers of polyolefin, in which one one or more such containers a low pressure plasma in exposing a fluorine-containing gas atmosphere. Fluorine itself is not meant by the term "fluorine-containing gas" be understood.
Der Fachmann ist mit der Erzeugung eines Niederdruckplasmas hinlänglich vertraut. Zum einschlägigen Stand Technik sei lediglich beispielhaft verwiesen auf Rutscher & Deutsch, Plasmatechnik, Carl-Hanser-Verlag 1984. So kann die Prozeßkammer aus einem beständigen Metall, beispielsweise aus Aluminium oder Edelstahl, bestehen. Für die Erzeugung des Niederdruckplasmas wird im Vakuum unter Hochfrequenzeinwirkung beispielsweise im Frequenzbereich von kHz bis GHz gearbeitet, beispielsweise im Bereich von 30 kHz bis 10 GHz.The skilled person is familiar with the production of a low-pressure plasma sufficiently familiar. To the relevant state technology was by way of example only referred to rides & German, Plasma technology, Carl-Hanser-Verlag 1984. Thus, the process chamber made of a durable metal, such as aluminum or stainless steel. For the generation of low-pressure plasma becomes in the vacuum under Hochfrequenzeinwirkung for example worked in the frequency range from kHz to GHz, for example in the range of 30 kHz to 10 GHz.
Üblicherweise bestehen die Behälter aus Polyethylen oder Polypropylen. Das erfindungsgemäße Verfahren eignet sich besonders zur Oberflächenmodifizierung von Polyolefinbehältern, die zur Aufbewahrung von Kraftstoffen, wie Benzin, vorgesehen sind.Usually, the containers are made of polyethylene or polypropylene. The inventive method is particularly suitable for the surface modification of polyolefin containers used for Storage of fuels such as gasoline are provided.
Beispiele für fluorhaltige Gase sind Tetrafluorkohlenstoff und/oder Schwefelhexafluorid, die man ggf. jeweils im Gemisch mit einem oder mehreren nicht-fluorhaltigen Gasen einsetzen kann, beispielsweise einem oder mehreren Edelgasen, wie Helium, Neon oder Argon, und/oder Sauerstoff.Examples of fluorine-containing gases are carbon tetrafluoride and / or sulfur hexafluoride, which if necessary in each case in a mixture with one or more non-fluorine-containing gases can, for example, one or more noble gases, such as helium, Neon or argon, and / or oxygen.
Bei der Verwendung beispielsweise eines Tetrafluorkohlenstoff/ Argon-Gemischs wird man annehmen können, daß die Polyolefinoberfläche fluoriert wird, während sie bei Einsatz eines Schwefelhexafluorid/Sauerstoff-Gemischs zusätzlich sulfoniert wird. In beiden Fällen erreicht man eine Teilpolarisierung der Oberfläche, durch die sich die Permeabilität der Polyolefinbehälter insbesondere gegenüber Benzin herabsetzen läßt.When using, for example, a tetrafluorocarbon / Argon mixture will be assumed that the Polyolefinoberfläche fluorinated while using a Sulfur hexafluoride / oxygen mixture additionally sulfonated becomes. In both cases one achieves a partial polarization of Surface through which the permeability of the polyolefin container especially lower than gasoline.
Nachstehend wird die Erfindung durch ein Beispiel näher erläutert.The invention will be explained in more detail by an example.
Es wurde folgende Prozeßkammer verwendet:The following process chamber was used:
Kammertür vorne, mit Hebelverschluß, dichtet selbsttätig beim
Schließen, mit Trennstecker (Sicherheitsabschaltung der Hochfrequenz),
Sichtfenster aus Spezialglas, Durchmesser ca. 150 mm.
Kammerflutventil mit Partikelfilter in Kammerrückwand.
Magnetventile und Verrohrung aus Edelstahl.
Elektropneumatische Absperrventil aus Aluminium, NW 40 KF an
Kammerunterseite.
Enddruck in der Kammer:
ca. 2-3 × 10-2 mbar.
Typischer Arbeitsdruck:
0,2-0,5 mbar.
Vakuummessung mittels Kapazitätsmeßdose, MKS Typ Baratron, Gasart-
unabhängig, Meßbereich 10-3-10 mbar.
Alle verwendeten Flanschverbindungen in KF und Pneurop.Chamber door at the front, with lever lock, seals automatically when closing, with isolating plug (safety shutdown of the high frequency), inspection window made of special glass, diameter approx. 150 mm. Chamber flood valve with particle filter in chamber rear wall. Solenoid valves and piping made of stainless steel.
Electropneumatic shut-off valve made of aluminum, NW 40 KF on underside of chamber.
Final pressure in the chamber: approx. 2-3 × 10 -2 mbar.
Typical working pressure: 0.2-0.5 mbar.
Vacuum measurement by means of a capacitance load cell, MKS type Baratron, gas type independent, measuring range 10 -3 -10 mbar.
All flange connections used in KF and Pneurop.
Leybold-Heraeus S 65 BC mit Ölfiltriereinrichtung, Ölabscheider mit Ölrückführung, Pumpe mit Fomblinöl gefüllt, Pumpleistung 65 m³/h.Leybold-Heraeus S 65 BC with oil filter, oil separator with oil return, pump filled with Fomblinöl, pumping capacity 65 m³ / h.
Prozeßkammer: 3067-G
Material: Al
Innenabmessungen (mm): Breite 800, Höhe 840, Tiefe 1080
Gaseinlässe: 12
Absaugung: Kammerboden
Verfügbares Kammervolumen: 787 l
Gasversorgung: 3 Gaskanäle mit Manometer für Vordruckanzeige.
Präzisionsdosierung mittels "Mass-Flow-Controller" (geeicht auf
Sauerstoff, Freon 14 und Luft).
Belüftung: durch Magnetventil in der Kammerrückwand
Prozeßsteuerung: PC-5000
Hochfrequenzgenerator: Magnetron, Arbeitsfrequenz 2450 MHz,
maximale Ausgangsleistung bis 1200 W, stufenlos regelbar vom
Controller PC-5000, Einkoppelung der HF-Kapazität
Vakuum-System: 100 m³/h Sperrschieberpumpe mit Ölfilter und Ölrückführung,
500 m³/h Rootsblower, Fomblinöl
Vakuum-Messung: MKS-Baratron, Kapazitätsmeßröhre
Vakuumanschluß: Pneurop NW 100 LF am Kammerboden
Anschlußwerte: 220/380 V Drehstrom 3phasig mit Null- und
Schutzleiter 3×32 A
Prozeßgase und Belüftung: 1/4′′ Swagelok-Verbindung Edelstahl,
Eingangsdruck 2 bar
Preßluft: 1/4′′ Swagelok-Verbindung Messung, Eingangsdruck 4-5
bar
Belüftung 1′′Process chamber: 3067-G
Material: Al
Inside dimensions (mm): width 800, height 840, depth 1080
Gas inlets: 12
Extraction: chamber floor
Available chamber volume: 787 l
Gas supply: 3 gas ducts with pressure gauge for pre-pressure indication.
Precision dosing by means of "mass flow controller" (calibrated for oxygen, freon 14 and air).
Ventilation: by solenoid valve in the back of the chamber
Process control: PC-5000
High frequency generator: Magnetron, operating frequency 2450 MHz, maximum output power up to 1200 W, infinitely adjustable from the controller PC-5000, coupling of the HF-capacity
Vacuum system: 100 m³ / h gate valve pump with oil filter and oil return, 500 m³ / h Rootsblower, Fomblinöl
Vacuum measurement: MKS Baratron, capacitance measuring tube
Vacuum connection: Pneurop NW 100 LF at the bottom of the chamber
Connection values: 220/380 V 3-phase three-phase with neutral and protective conductor 3 × 32 A.
Process gases and aeration: 1/4 '' Swagelok stainless steel connection, inlet pressure 2 bar
Compressed air: 1/4 '' Swagelok connection measurement, inlet pressure 4-5 bar
Ventilation 1 ''
Es wurde ein 80-l-Benzintank aus Polyethylen in der Prozeßkammer bei einem Druck von 50 Pascal und einer Hochfrequenz von 2,45 GHz in Gegenwart eines Gemischs aus 10% Tetrafluorkohlenstoff und 90% Argon (Volumenbasis) 5 min lang einem Plasma ausgesetzt. Durch die genannte Behandlung wurde die Permeabilität des Tanks für Super (Aral) um 85% herabgesetzt.There was an 80 liter polyethylene tank in the process chamber at a pressure of 50 pascals and a high frequency of 2.45 GHz in the presence of a mixture of 10% carbon tetrafluoride and 90% argon (volume basis) for 5 minutes in a plasma exposed. By the mentioned treatment became the permeability of the tank for Super (Aral) reduced by 85%.
Claims (3)
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19893933874 DE3933874A1 (en) | 1989-10-11 | 1989-10-11 | Modifying surface of polyolefin containers - by exposing container to low pressure plasma in fluorine-contg. gas atmos. |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE19893933874 DE3933874A1 (en) | 1989-10-11 | 1989-10-11 | Modifying surface of polyolefin containers - by exposing container to low pressure plasma in fluorine-contg. gas atmos. |
Publications (1)
Publication Number | Publication Date |
---|---|
DE3933874A1 true DE3933874A1 (en) | 1991-04-18 |
Family
ID=6391231
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
DE19893933874 Withdrawn DE3933874A1 (en) | 1989-10-11 | 1989-10-11 | Modifying surface of polyolefin containers - by exposing container to low pressure plasma in fluorine-contg. gas atmos. |
Country Status (1)
Country | Link |
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DE (1) | DE3933874A1 (en) |
Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5521351A (en) * | 1994-08-30 | 1996-05-28 | Wisconsin Alumni Research Foundation | Method and apparatus for plasma surface treatment of the interior of hollow forms |
US5560963A (en) * | 1991-10-07 | 1996-10-01 | Ford Motor Company | Low pressure plasma treatment of an article surface |
US5660639A (en) * | 1995-10-17 | 1997-08-26 | Ford Motor Company | Method and apparatus for plasma treating an article |
US6896838B2 (en) | 2001-11-21 | 2005-05-24 | Closure Medical Corporation | Halogenated polymeric containers for 1, 1-disubstituted monomer compositions |
EP1595913A1 (en) * | 2004-05-14 | 2005-11-16 | Inergy Automotive Systems Research (SA) | Method for preparing a hollow element of a fuel system |
WO2009074132A1 (en) * | 2007-12-13 | 2009-06-18 | Christof-Herbert Diener | Surface treatment process |
-
1989
- 1989-10-11 DE DE19893933874 patent/DE3933874A1/en not_active Withdrawn
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5560963A (en) * | 1991-10-07 | 1996-10-01 | Ford Motor Company | Low pressure plasma treatment of an article surface |
US5521351A (en) * | 1994-08-30 | 1996-05-28 | Wisconsin Alumni Research Foundation | Method and apparatus for plasma surface treatment of the interior of hollow forms |
US5660639A (en) * | 1995-10-17 | 1997-08-26 | Ford Motor Company | Method and apparatus for plasma treating an article |
US6896838B2 (en) | 2001-11-21 | 2005-05-24 | Closure Medical Corporation | Halogenated polymeric containers for 1, 1-disubstituted monomer compositions |
EP1595913A1 (en) * | 2004-05-14 | 2005-11-16 | Inergy Automotive Systems Research (SA) | Method for preparing a hollow element of a fuel system |
WO2005113654A2 (en) * | 2004-05-14 | 2005-12-01 | Inergy Automotive Systems Research (Société Anonyme) | Method for preparing a hollow element of a fuel system |
WO2005113654A3 (en) * | 2004-05-14 | 2006-03-30 | Inergy Automotive Systems Res | Method for preparing a hollow element of a fuel system |
WO2009074132A1 (en) * | 2007-12-13 | 2009-06-18 | Christof-Herbert Diener | Surface treatment process |
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