WO2007107262A1 - Hollow body made of plastic having a barrier layer on its inner surface and a method for manufacturing the same - Google Patents
Hollow body made of plastic having a barrier layer on its inner surface and a method for manufacturing the same Download PDFInfo
- Publication number
- WO2007107262A1 WO2007107262A1 PCT/EP2007/002182 EP2007002182W WO2007107262A1 WO 2007107262 A1 WO2007107262 A1 WO 2007107262A1 EP 2007002182 W EP2007002182 W EP 2007002182W WO 2007107262 A1 WO2007107262 A1 WO 2007107262A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- hollow body
- fluorine
- occupancy
- plastic
- mean
- Prior art date
Links
- 239000004033 plastic Substances 0.000 title claims abstract description 36
- 229920003023 plastic Polymers 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 230000004888 barrier function Effects 0.000 title description 13
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 89
- 239000011737 fluorine Substances 0.000 claims abstract description 89
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 89
- 230000009471 action Effects 0.000 claims abstract description 7
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 150000001875 compounds Chemical class 0.000 claims abstract description 3
- NBVXSUQYWXRMNV-UHFFFAOYSA-N fluoromethane Chemical compound FC NBVXSUQYWXRMNV-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 31
- 238000003682 fluorination reaction Methods 0.000 claims description 23
- 230000008093 supporting effect Effects 0.000 claims description 19
- 238000001816 cooling Methods 0.000 claims description 16
- 238000001125 extrusion Methods 0.000 claims description 15
- 229920001169 thermoplastic Polymers 0.000 claims description 11
- 239000004416 thermosoftening plastic Substances 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 7
- 239000002828 fuel tank Substances 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 238000011049 filling Methods 0.000 claims description 3
- 230000002596 correlated effect Effects 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 4
- 238000006243 chemical reaction Methods 0.000 description 9
- 230000000694 effects Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 6
- 239000011248 coating agent Substances 0.000 description 4
- 238000000576 coating method Methods 0.000 description 4
- 238000012417 linear regression Methods 0.000 description 4
- 238000006467 substitution reaction Methods 0.000 description 4
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000011261 inert gas Substances 0.000 description 3
- 229920000642 polymer Polymers 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 238000007493 shaping process Methods 0.000 description 3
- -1 vapours Substances 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 239000000498 cooling water Substances 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- PKXHXOTZMFCXSH-UHFFFAOYSA-N 3,3-dimethylbut-1-ene Chemical compound CC(C)(C)C=C PKXHXOTZMFCXSH-UHFFFAOYSA-N 0.000 description 1
- YHQXBTXEYZIYOV-UHFFFAOYSA-N 3-methylbut-1-ene Chemical compound CC(C)C=C YHQXBTXEYZIYOV-UHFFFAOYSA-N 0.000 description 1
- WSSSPWUEQFSQQG-UHFFFAOYSA-N 4-methyl-1-pentene Chemical compound CC(C)CC=C WSSSPWUEQFSQQG-UHFFFAOYSA-N 0.000 description 1
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 1
- YPDSOAPSWYHANB-UHFFFAOYSA-N [N].[F] Chemical compound [N].[F] YPDSOAPSWYHANB-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 1
- 229910052794 bromium Inorganic materials 0.000 description 1
- 239000008366 buffered solution Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000011010 flushing procedure Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 150000004812 organic fluorine compounds Chemical class 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000001420 photoelectron spectroscopy Methods 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920002239 polyacrylonitrile Polymers 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004080 punching Methods 0.000 description 1
- 238000007347 radical substitution reaction Methods 0.000 description 1
- 150000003254 radicals Chemical group 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/24—Lining or labelling
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F14/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen
- C08F14/18—Monomers containing fluorine
-
- 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
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/42—Component parts, details or accessories; Auxiliary operations
- B29C49/48—Moulds
- B29C49/4823—Moulds with incorporated heating or cooling means
- B29C2049/4825—Moulds with incorporated heating or cooling means for cooling moulds or mould parts
- B29C2049/483—Moulds with incorporated heating or cooling means for cooling moulds or mould parts in different areas of the mould at different temperatures, e.g. neck, shoulder or bottom
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/02—Combined blow-moulding and manufacture of the preform or the parison
- B29C49/04—Extrusion blow-moulding
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/42—Component parts, details or accessories; Auxiliary operations
- B29C49/4273—Auxiliary operations after the blow-moulding operation not otherwise provided for
- B29C49/42828—Coating or painting the article
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C49/00—Blow-moulding, i.e. blowing a preform or parison to a desired shape within a mould; Apparatus therefor
- B29C49/42—Component parts, details or accessories; Auxiliary operations
- B29C49/48—Moulds
- B29C49/4823—Moulds with incorporated heating or cooling means
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2009/00—Layered products
- B29L2009/005—Layered products coated
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
- B29L2031/00—Other particular articles
- B29L2031/712—Containers; Packaging elements or accessories, Packages
- B29L2031/7172—Fuel tanks, jerry cans
-
- 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
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/13—Hollow or container type article [e.g., tube, vase, etc.]
- Y10T428/1352—Polymer or resin containing [i.e., natural or synthetic]
Definitions
- Hollow body made of plastic having a barrier layer on its inner surface and a method for manufacturing the same
- the invention relates to a hollow body made of plastic, the inner surface of which has a coating with a locally selective barrier effect, and a method for its produc ⁇ tion.
- plastics for the production of containers for industrial gases and liquids is limited, inter alia, by the permeation of gases, vapours, and solvents through the container wall.
- One possibility of reducing the permeation through the container wall made of plastic is the coating of the inner surface of the container with a permeation-inhibiting barrier layer.
- permeation-inhibiting barrier layers made of plastics, such as, for example, fluorination, coating, coextrusion and the treatment of the surface with barrier layer resins.
- the polymer surface is subjected to attack by elemental fluorine.
- gas-phase fluorination in which a fluorine- containing treatment gas acts briefly on the inner surface of the hollow body has proved particularly useful.
- a fluorine-containing treatment gas acts briefly on the inner surface of the hollow body.
- a stepwise free radical substitution of the CH bonds by CF bonds occurs.
- the fluorination of the surfaces of the plastics not only influences the permeation behaviour to a high degree, but the abrasion resistance, the chemical, thermal and mechanical stability, the adhesion behaviour and the wettability are also influenced. For this reason, the invention is not limited to the fluorination of the inner surface of hollow bodies made of plastic.
- DE 35 11 743 Al describes a method for the manufacture of a hollow body having a fluorinated inner surface, in which a parison comprising a thermoplastic is ex- truded through an annular extruder die and then blown to give a hollow body inside a closed supporting mould using a fluorine-containing treatment gas in such a way that the hollow body fills the inner contours of the supporting mould.
- a cer ⁇ tain duration during which ithe fluorine-containing treatment gas remains in the hollow body and acts on the inner surface thereof is specified here. After expiry of the specified action time, the hollow body is flushed with an inert gas and the supporting mould is removed. This method is referred to as inline fluorination since the fluorination and the manufacture of the hollow body take place simultaneously.
- DE 24 01 948 Al and DE 26 44 508 Al teach methods for so-called offline fluorination in which a gas-phase fluorination is carried out on finished shaped or hollow bodies made of plastic.
- those regions of a container which are subjected to a high load have an improved barrier effect.
- a typical example of this is the runback region of a fuel tank, through which large amounts of fuel flow in normal operation, hi order to ensure the required barrier effect in regions subjected to high load, the process parameters, such as fluorine content, duration of action and temperature of the fluorine-containing treatment gas are regulated in the gas-phase fluorination so that the mean fluorine occupancy in the entire fuel tank reaches or exceeds the value required in regions subjected to high load.
- Those regions of the fuel tank which are subjected to a lower load are provided with a fluorine occupancy which in part considerably exceeds the required degree.
- the hollow bodies made of plastic having a fluorinated inner surface which are known in the prior art have the disadvantage that the mean fluorine occupancy has a high value and that the local fluorine occupancy varies in an uncontrolled manner.
- the associated production processes have the disadvantages of increased use of fluorine and/or longer process duration.
- a hollow body made of plastic having a fluorinated inner surface, in which, in one or more defined regions of the inner surface, the fluorine occupancy deviates from the mean fluorine occupancy by at least ⁇ 10%.
- a further object of the invention is to provide a hollow body made of plastic which has an inner surface with a substantially constant barrier effect. This object is achieved by a hollow body made of plastic having a fluorinated inner surface, in which the local fluorine occupancy deviates from the mean fluorine occupancy by less than ⁇ 30 ⁇ g/cm 2 .
- Fig. 1 a shows a schematic view of a defined region
- Fig. 2 shows a graph with measured values of the working examples 1 to 4.
- Fig. 1 a schematically shows a wall section 1 of a hollow body having a fluorinated inner surface 2 and a defined region 3, the defined region 3 being surrounded by an edge zone 4 of a width 5.
- the width 5 of the edge zone 4 may vary along the cir- cumference of the defined region 3.
- Fig. Ib schematically shows the curve of the fluorine occupancy 6 in the edge zone 4, the numeral 7 designating the decrease/increase in the fluorine occupancy 6 over the width 5 of the edge zone 4.
- the hollow body made of plastic has a fluorinated inner surface 2, the fluorine occupancy deviating from the mean fluorine occupancy by at least ⁇ 10% in one or more defined regions 3 of the inner surface 2.
- the fluorine occupancy in the defined regions deviates from the mean value by at least ⁇ 30% in particular by at least ⁇ 50%.
- the defined regions 3 are surrounded by an edge zone 4 in which the fluorine occupancy 6 shows a continuous monotonic increase or decrease.
- the width 5 of the edge zone is from 1 to 15 mm and may vary along the circumference of the defined region 3.
- the quotient of increase/decrease of the fluorine occupancy 7 and width 5 of the edge zone 4 is designated as edge gradient of the fluorine occupancy.
- the mean fluorine occupancy and the wall thickness of the hollow body according to the invention are from 5 to 120 ⁇ g/cm 2 and from 0.5 to 20 mm, respectively.
- the hollow body preferably consists of a thermoplastic.
- Thermoplastics are mouldable at their specific softening temperature; they consist of polymers and copolymers of polystyrene, polyacrylonitrile, polyvinyl chloride and polyolefins.
- Preferably used thermoplastic blends are polyolefin polymers or copolymers of the following monomers: ethylene, propylene, 1-butene, 1-pentene, 4-methyl-l- pentene, 3 -methyl- 1-butene and 3, 3 -dimethyl- 1-butene.
- blends may optionally also contain constituents such as pigments, fillers, dulling agents, plasticizers, flame retardants, anti-static agents and other known materials for influencing the chemical and physical properties of the finished thermoplastic product.
- These blends may also contain other plastics mixed with a polyolefin.
- the hollow body according to the invention is in the form of a fuel tank.
- a further embodiment of the invention relates to a hollow body made of plastic having a fluorinated inner surface, the local fluorine occupancy deviating from the mean fluorine occupancy by less than ⁇ 30 ⁇ g/cm 2 , in particular by less than ⁇ 20 * ⁇ g/cm 2 and particularly preferably by less than ⁇ 10 ⁇ g/cm .
- the methods according to the invention for the production of a hollow body made of plastic, the inner surface of which has a coating having a locally selective barrier effect, are based on gas-phase fluorination in the inline and offline mode.
- the hollow body is filled with a treatment gas having a fluorine content of 0.1 to 25% by volume once or several times for a certain action time - in the range of a few seconds to one hour.
- the temperature of the treatment gas is adjusted between - 120°C and 35 0 C, depending on the fluorine content, the action time, wall temperature of the hollow body and the desired mean fluorine occupancy on the inner sur- face.
- the hollow body is flushed with an inert gas in order to remove the fluorine-containing treatment gas, and the process is optionally repeated.
- the reaction of the elemental fluorine present in the treatment gas with the plastic of the inner surface of the hollow body is highly exothermic and can lead to combustion of the plastic when critical process parameters are ex- ceeded. This disadvantageous effect is counteracted by means of cooling of the hollow body and/or of the treatment gas.
- the treatment gas substantially contains an inert gas, such as nitrogen, argon, helium and the like.
- an inert gas such as nitrogen, argon, helium and the like.
- additives such as oxygen, carbon monoxide and carbon dioxide or mixtures of these gases are added to the treatment gas for improving the colourability and the barrier effect with respect to oil, and chlorine and bromine and mixtures of these gases are added to said treatment gas for reducing the flammability.
- the substitution rate of the chemical reaction which leads to the incorporation of fluorine into the plastic of the inner surface of the hollow body depends substantially on the temperature and the fluorine concentration.
- the reaction takes place faster and substitution rate increases with increasing temperature and activation, respectively. Conversely, a higher substitution rate results in an increase in the temperature, owing to the exothermic course of the reaction.
- a precondition for maintaining t he reaction is the supply of elemental fluorine. If the temperature falls below a certain value, the chemical reaction takes place very slowly and the substi- tution rate tends to zero even with a sufficient supply of fluorine.
- the methods according to the invention for the production of a hollow body made of plastic having a fluorinated inner surface by means of gas-phase fluorination utilize the temperature dependency of the chemical reaction between fluorine and plastic.
- the method according to the invention is carried out by blow extrusion with inline fluorination.
- a parison is extruded from a thermoplastic, the gap width of the extrusion die being varied so that one or more defined zones of the parison have predetermined different wall thicknesses.
- the parison is first blown with a fluid - preferably nitrogen - to give a hollow body within a closed cooled supporting mould so that the hollow body fills the inner contours of the supporting mould, the wall thicknesses being increased/reduced in one or more defined regions of the hollow body and the cooling of the inner surface being ef- fected more slowly/faster.
- the hollow body is completely filled with the fluorine-containing gas, fluorine being incorporated in the defined regions of the inner surface to a greater/lesser extent owing to the higher/lower temperatures.
- the wall thickness of the parison and hence of the hollow body is adjusted in a controlled manner vary- ing the gap width of the extrusion die by means of computer-controlled final control elements during the extrusion of the parison.
- An extrusion head whose outer die is fixed while the inner mandrel, which has a specially shaped lateral surface, is vertically adjustable is frequently used for this purpose. During the extrusion, the mandrel is moved vertically, with the result that the width of the gap between outer die and inner mandrel changes.
- Extrusion heads having combined axial and radial gap width adjustment are used for producing complex wall thickness profiles.
- the supporting mould typically consists of two solid blocks of aluminium, one half of the outer mould of the hollow body to be produced being cut into each of the blocks.
- the blocks have a multiplicity of bores through which water having a temperature in the range from 5 to 15°C is passed for cooling.
- a parison comprising a thermoplastic is extruded and first blown with a fluid - preferably nitrogen - to give a hollow body within a closed cooled supporting mould so that the hollow body fills the inner contours of the supporting mould, the cooling being reduced in one or more defined zones of the supporting mould and the cooling of those regions of the inner surface of the hol- low body which are congruent with these zones taking place more slowly.
- the hollow body is completely filled with a fluorine-containing gas, fluorine being incorporated to a greater extent in the congruent regions of the inner surface owing to the higher temperatures of the congruent regions.
- defined zones of the inner contours of the supporting mould are coated with a thermally insulating paint.
- the cooling is reduced by reducing the amount of cooling water flowing through the sup- porting mould in the defined zones.
- the cooling water supply is throttled locally or the number and/or the cross section of the cooling bores in the supporting mould are reduced.
- a further method according to the invention relates to offline fluorination in which, for the formation of fluorocarbon and hydrofluorocarbon compounds, the inner surface of a hollow body made of plastic is exposed to the action of a defined amount of a fluorine-containing treatment gas and the hollow body is thermostatted on its outside so that the temperature in one or more defined regions of the outside is at least ⁇ 2°C, in particular at least ⁇ 5 0 C and particularly preferably at least ⁇ 10°C above the mean temperature of the outside.
- the hollow body is thereby preferably treated on its outside with one or more fluids having different temperatures.
- the temperature of the treatment gas fed in is preferably adjusted to room temperature in the range from 15 to 40 0 C. Examples
- the extruded parisons were blown with nitrogen in a water-cooled supporting mould.
- the inline fluorination was effected with a fluorine-nitrogen gas mixture having fluorine contents between 1 and 2.5% by volume at a pressure of 9.8 bar and in treatment times from 15 to 25 sec.
- test pieces having a fluorinated inner surface of about 0.2 cm 2 were punched out of the PFTs produced and were chemically analysed using a Fluoride Analyzer Model 9000 F from Antek Instruments, which operates according to the following method: combustion of the sample volume in an oxygen stream at a temperature of 1050°C, organic fluorine compounds being quantitatively converted into hydrogen fluoride; precipitation of the HF gas formed in the combustion in a buffered solution and measurement of the fluoride content of the solution obtained by means of an ion-sensitive electrode.
- the wall thickness of the test pieces was determined prior to punching out of the PFT by means of ultrasound.
- Fig. 2 shows the measured values of examples 1 to 4 in graphic form.
- the graph shows trend lines (shown as solid or dashed lines), which were determined on the basis of linear regression.
Abstract
Description
Claims
Priority Applications (6)
Application Number | Priority Date | Filing Date | Title |
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ES07711926.1T ES2565681T3 (en) | 2006-03-17 | 2007-03-13 | Method for manufacturing a hollow body made of plastic that has a barrier layer on its inner surface |
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KR1020087022594A KR101392003B1 (en) | 2006-03-17 | 2008-09-16 | Hollow body made of plastic having a barrier layer on its inner surface and a method for manufacturing the same |
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Also Published As
Publication number | Publication date |
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CN101415755B (en) | 2012-01-18 |
KR20080108461A (en) | 2008-12-15 |
ZA200807153B (en) | 2009-05-27 |
DE102006012367B4 (en) | 2015-07-16 |
EP1999198A1 (en) | 2008-12-10 |
ES2565681T3 (en) | 2016-04-06 |
DE102006012367A1 (en) | 2007-09-20 |
KR101392003B1 (en) | 2014-05-07 |
PL1999198T3 (en) | 2016-06-30 |
US20110305856A1 (en) | 2011-12-15 |
EP1999198B1 (en) | 2016-02-03 |
CN101415755A (en) | 2009-04-22 |
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