TWI472421B - 具有金屬夾層的pvc/cpvc複合管及其製造方法 - Google Patents
具有金屬夾層的pvc/cpvc複合管及其製造方法 Download PDFInfo
- Publication number
- TWI472421B TWI472421B TW97145850A TW97145850A TWI472421B TW I472421 B TWI472421 B TW I472421B TW 97145850 A TW97145850 A TW 97145850A TW 97145850 A TW97145850 A TW 97145850A TW I472421 B TWI472421 B TW I472421B
- Authority
- TW
- Taiwan
- Prior art keywords
- conduit
- metal
- adhesive
- pvc
- cpvc
- Prior art date
Links
- 229910052751 metal Inorganic materials 0.000 title claims description 148
- 239000002184 metal Substances 0.000 title claims description 148
- 239000002131 composite material Substances 0.000 title claims description 93
- 238000000034 method Methods 0.000 title claims description 22
- 230000008569 process Effects 0.000 title description 13
- 239000011229 interlayer Substances 0.000 title description 3
- 239000000853 adhesive Substances 0.000 claims description 112
- 230000001070 adhesive effect Effects 0.000 claims description 111
- 239000010410 layer Substances 0.000 claims description 74
- 239000004800 polyvinyl chloride Substances 0.000 claims description 68
- 229920000915 polyvinyl chloride Polymers 0.000 claims description 64
- 229920000642 polymer Polymers 0.000 claims description 53
- 229910052782 aluminium Inorganic materials 0.000 claims description 21
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 18
- 239000003822 epoxy resin Substances 0.000 claims description 18
- 229920000647 polyepoxide Polymers 0.000 claims description 18
- 239000002904 solvent Substances 0.000 claims description 18
- 238000000576 coating method Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 14
- KWOLFJPFCHCOCG-UHFFFAOYSA-N Acetophenone Chemical compound CC(=O)C1=CC=CC=C1 KWOLFJPFCHCOCG-UHFFFAOYSA-N 0.000 claims description 12
- 239000012790 adhesive layer Substances 0.000 claims description 11
- 230000002093 peripheral effect Effects 0.000 claims description 11
- 239000012530 fluid Substances 0.000 claims description 10
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 239000004709 Chlorinated polyethylene Substances 0.000 claims description 8
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N formaldehyde Substances O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 8
- 229920001187 thermosetting polymer Polymers 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 7
- 239000011347 resin Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 6
- 229920000728 polyester Polymers 0.000 claims description 6
- 239000004698 Polyethylene Substances 0.000 claims description 5
- 238000004132 cross linking Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000004814 polyurethane Substances 0.000 claims description 5
- 229920002635 polyurethane Polymers 0.000 claims description 5
- 238000004513 sizing Methods 0.000 claims description 5
- 238000009966 trimming Methods 0.000 claims description 5
- 238000003466 welding Methods 0.000 claims description 5
- 230000008878 coupling Effects 0.000 claims description 4
- 238000010168 coupling process Methods 0.000 claims description 4
- 238000005859 coupling reaction Methods 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052753 mercury Inorganic materials 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 230000006698 induction Effects 0.000 claims description 2
- 229920000768 polyamine Polymers 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims 5
- 238000012986 modification Methods 0.000 claims 5
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical compound [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims 3
- 238000005260 corrosion Methods 0.000 claims 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims 1
- 238000004033 diameter control Methods 0.000 claims 1
- 235000019253 formic acid Nutrition 0.000 claims 1
- 238000005304 joining Methods 0.000 claims 1
- 229910052760 oxygen Inorganic materials 0.000 claims 1
- 239000001301 oxygen Substances 0.000 claims 1
- 239000003973 paint Substances 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 239000004801 Chlorinated PVC Substances 0.000 description 52
- 229920000457 chlorinated polyvinyl chloride Polymers 0.000 description 52
- 238000012360 testing method Methods 0.000 description 30
- 238000005452 bending Methods 0.000 description 5
- 229920003020 cross-linked polyethylene Polymers 0.000 description 5
- 239000004703 cross-linked polyethylene Substances 0.000 description 5
- 230000004927 fusion Effects 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 230000032798 delamination Effects 0.000 description 4
- 238000001125 extrusion Methods 0.000 description 4
- 239000004609 Impact Modifier Substances 0.000 description 3
- 239000006057 Non-nutritive feed additive Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 229920005670 poly(ethylene-vinyl chloride) Polymers 0.000 description 3
- 229920000098 polyolefin Polymers 0.000 description 3
- 238000012545 processing Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 230000002411 adverse Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 238000002347 injection Methods 0.000 description 2
- 239000007924 injection Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000007790 scraping Methods 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 229920003313 Bynel® Polymers 0.000 description 1
- BDAGIHXWWSANSR-UHFFFAOYSA-M Formate Chemical compound [O-]C=O BDAGIHXWWSANSR-UHFFFAOYSA-M 0.000 description 1
- 229920006385 Geon Polymers 0.000 description 1
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 239000002390 adhesive tape Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000007900 aqueous suspension Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000007767 bonding agent Substances 0.000 description 1
- 239000000292 calcium oxide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000011247 coating layer Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000012669 compression test Methods 0.000 description 1
- 239000000498 cooling water Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000006073 displacement reaction Methods 0.000 description 1
- 230000009477 glass transition Effects 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000010687 lubricating oil Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000004848 polyfunctional curative Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N urethane group Chemical group NC(=O)OCC JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L9/00—Rigid pipes
- F16L9/14—Compound tubes, i.e. made of materials not wholly covered by any one of the preceding groups
- F16L9/147—Compound tubes, i.e. made of materials not wholly covered by any one of the preceding groups comprising only layers of metal and plastics with or without reinforcement
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/15—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor incorporating preformed parts or layers, e.g. extrusion moulding around inserts
- B29C48/151—Coating hollow articles
- B29C48/152—Coating hollow articles the inner surfaces thereof
- B29C48/153—Coating both inner and outer surfaces
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- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D23/00—Producing tubular articles
- B29D23/001—Pipes; Pipe joints
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- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B1/00—Layered products having a non-planar shape
- B32B1/08—Tubular products
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- B32B15/00—Layered products comprising a layer of metal
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- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/082—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising vinyl resins; comprising acrylic resins
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- B32B15/00—Layered products comprising a layer of metal
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- B32B27/00—Layered products comprising a layer of synthetic resin
- B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
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- B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
- B32B7/04—Interconnection of layers
- B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F16—ENGINEERING ELEMENTS AND UNITS; GENERAL MEASURES FOR PRODUCING AND MAINTAINING EFFECTIVE FUNCTIONING OF MACHINES OR INSTALLATIONS; THERMAL INSULATION IN GENERAL
- F16L—PIPES; JOINTS OR FITTINGS FOR PIPES; SUPPORTS FOR PIPES, CABLES OR PROTECTIVE TUBING; MEANS FOR THERMAL INSULATION IN GENERAL
- F16L47/00—Connecting arrangements or other fittings specially adapted to be made of plastics or to be used with pipes made of plastics
- F16L47/02—Welded joints; Adhesive joints
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- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
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- B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
- B29C48/12—Articles with an irregular circumference when viewed in cross-section, e.g. window profiles
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- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/15—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor incorporating preformed parts or layers, e.g. extrusion moulding around inserts
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- 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
- B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
- B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
- B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
- B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
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- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
- B29C65/4805—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding characterised by the type of adhesives
- B29C65/483—Reactive adhesives, e.g. chemically curing adhesives
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- 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
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/48—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor using adhesives, i.e. using supplementary joining material; solvent bonding
- B29C65/4895—Solvent bonding, i.e. the surfaces of the parts to be joined being treated with solvents, swelling or softening agents, without adhesives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/50—General aspects of joining tubular articles; General aspects of joining long products, i.e. bars or profiled elements; General aspects of joining single elements to tubular articles, hollow articles or bars; General aspects of joining several hollow-preforms to form hollow or tubular articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
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- B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
- B29K2027/06—PVC, i.e. polyvinylchloride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
- B29K2305/00—Use of metals, their alloys or their compounds, as reinforcement
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- 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
- B29L2009/003—Layered products comprising a metal layer
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- 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
- B29L2023/00—Tubular articles
- B29L2023/004—Bent tubes
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- 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
- B29L2023/00—Tubular articles
- B29L2023/005—Hoses, i.e. flexible
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B29L—INDEXING SCHEME ASSOCIATED WITH SUBCLASS B29C, RELATING TO PARTICULAR ARTICLES
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- B29L2023/22—Tubes or pipes, i.e. rigid
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- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2255/00—Coating on the layer surface
- B32B2255/06—Coating on the layer surface on metal layer
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
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- B32B2597/00—Tubular articles, e.g. hoses, pipes
-
- 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
- Y10T156/00—Adhesive bonding and miscellaneous chemical manufacture
- Y10T156/10—Methods of surface bonding and/or assembly therefor
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Rigid Pipes And Flexible Pipes (AREA)
- Laminated Bodies (AREA)
- Lining Or Joining Of Plastics Or The Like (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
- Media Introduction/Drainage Providing Device (AREA)
Description
本發明係關於一種複合管,其擠壓出以致於具有:(i)一金屬導管,其係在夾層在(ii)聚氯乙烯(PVC,“poly vinyl chloride”)或氯化聚乙烯(CPVC,“chlorinated poly vinyl chloride")的內導管(其係黏固至該金屬導管的內表面)及(iii)一PVC或CPVC的外導管(其係黏固至金屬導管的外表面)之間。PVC/CPVC(簡稱為「聚合物」)之內與外導管係強力地黏固至金屬導管的內與外表面,以致該管符合熱和冷家庭用水的CTS與IPS管二者、及用於製程流體處理與消防灑水系統的工業系統之標準。一段管的每一終端(定義管端邊緣表面)之周邊截面係吻合嚴格的錐形套管與配件,不使微流體液滴流入在聚合物與金屬之間的環形邊界。
複合管(亦稱為多層金屬管)已揭示在許多參考案件中,例如在須與布希等人的美國專利案第6,293,311號(「'311專利」)之第1與第2頁列出的這些複合管,其與本發明所揭示的最相關。'311專利教示藉由擠壓PVC/CPVC的內導管形成的複合管;使用第一層膠黏劑予以塗覆;在縮小金屬帶橫截面以提供小於2mm的間隙之後,藉由對頭熔接該金屬帶的縱向邊緣以在塗膠的內導管上形成金屬導管;可選擇地,加熱該金屬包覆內導管以活性化該膠黏劑;使用第二膠黏劑層塗覆金屬導管的外表面;然後,擠壓PVC/CPVC的外導管在第二層膠黏劑上。
在'311專利中的膠黏劑係以兩階段施加。將第一層膠黏劑加熱使其活性化,以致於在縮小金屬導管之後,使下面的金屬導管黏著至內CPVC導管,形成三層導管。然後施加第二層膠黏劑(第10欄,第21-31行)。活性任何寬領域之膠黏劑的建議(如需要)並未提及任何特定的膠黏劑。而且,說明的範例是針對Estane58271聚氨脂,一種熱塑性、非熱活性化膠黏劑。未建議在導管中成形之前,於金屬帶的兩面預先塗覆熱固性雙層膠黏劑,從第一底漆層與第二面塗層之組合產生黏性,該組合係塗覆在金屬帶的每面上及乾凅。下述的此種雙層熱固性膠黏劑以下稱之為「雙層膠黏劑」。
311揭示關於縮小金屬以靠攏「在金屬中間層與在下面膠黏劑間的小於2.0mm的間隙」、及可選擇地加熱在下面膠黏劑使其「活性化」未能實現在環繞內導管周圍緊緊地形成金屬帶的嚴格要求,以致於在金屬帶的緊鄰邊緣之間留下小於0.5mm(0.020")的間隙,最佳地小於0.25mm(0.010"),及在緊鄰邊緣下方留下垂直空間,足以避免在下面之聚合物受到熔接雷射光束的燃燒,此空間從金屬的邊緣之下方垂直測量最好是在範圍從0.25mm(0.010")至0.75mm(0.030")。
在此使用的術語「管」是指符合CTS或IPS規定的複合管,不管其是管系或管。在此使用的術語「導管」是指聚合物的擠出之內與外管層,且是指夾在其間之管金屬;用來塗覆金屬導管的內與外表面之膠黏劑是指膠黏劑的內與外層。「PVC/CPVC」的導管意謂導管可為PVC或CPVC、或PVC和CPVC之混合。在複合管中,若內導管是PVC,外管可為PVC或CPVC;且若內導管是CPVC,外管可為PVC或CPVC;即是,在每一層之聚合物可相同或不同(「混合或匹配」)。PVC和CPVC係使用在此揭示佔多數的複合管之聚合物。PVC和CPVC化合物二者包含適量的其他聚合物材料,例如抗衝改良劑、加工助劑與潤滑油。導管PVC或CPVC化合物應該大於50重量百分率,最佳地大於70重量百分率,且更佳係大於PVC或CPVC、或PVC和CPVC之混合的80。
在州際商務中嚴格要求,該發明的複合管要符合ASTM F1281的第9.3、9.4、9.5節與ASTM D2846、ASTM D1785、AWWA C901、ASTM F493、PPI TR--3和NSF/ANSI標準14所特定測試條件之規定(其在此併入本文供參考)。符合前面標準的管以下是指「符合測試條件」的管。除了符合規定的測試條件之外,複合管在1.205MPa(175psi)的高壓與82.2℃(180℉)高溫下,可使用在水、水溶液、水懸浮液及流體的管路系統中操作,管本質上對這些處理液是惰性的。「惰性」意謂聚合物不會顯著地與流過其之流體起反應,且實質上在流體中不是可溶解的。
在製造於'311專利中所揭示的發明時,沒有理由指定複合管符合任何特定的ASTM標準的規定,且沒有理由決定複合管性能特徵的限制。在測檢時,其後很快發現,使用在'311專利中建議的各種膠黏劑所形成的複合管於相當短時間只適用在環境室溫範圍從20℃至25℃(68℉至77℉),及低壓範圍從790至928KPa(100至120psig)。
更具體地說,該管未能符合在ASTM D2846/D2846M-06所規定之高溫與壓力範圍內所規定的測試條件與在此規定的最小環剝強度。
隨後將明白:特別是關於PVC/CPVC,在過去六年,在包括不斷調查與測試處理條件艱難地測試以不同方式及在廣泛範圍的條件上施加的各種膠黏劑,及在形成複合管的製程中測試各種機器之大量嘗試錯誤量之後,只有狹義指定的製程條件及使用雙層膠黏劑塗覆作為底漆層,然後在金屬帶上,以非常薄塗覆作為面塗層,當加熱超過48.9℃(120℉)的乾塗層可造成有效的膠黏劑,提供金屬、鋁或鋼黏合至PVC/CPVC,以致於複合管符合規定的ASTM測試條件。
'311專利的PVC/CPVC複合管在所規定測試條件下失敗,因為至少兩理由:在聚合物與金屬間的不足黏著性及不充分熔接以形成金屬導管。而且,儘管所有連接係使用以溶劑為主之黏劑的溶劑黏合,但是使用在'311專利中描述的配件構成管路系統,在連接處會滲漏,因為配件未能密封每一終端(邊緣,或管端的周邊)的周邊截面,即在管端壓入配件之前,截面係依序曝露聚合物、膠黏劑、金屬、膠黏劑和聚合物的各層。膠黏劑的雙層是相當薄,以致於實質無法用肉眼看到。
在聚合物與金屬之間的不充分黏著性由於下列而得以證實:(i)在連續周邊層的邊界在聚合物與金屬之間的分離,即是在邊緣的聚合物/膠黏劑/金屬介面;(ii)在65.5℃(150℉),1300KPa(175psig)壓力下的管破裂;及(iii)當複合管中的金屬是鋁,且管彎曲180°,半徑小於約6倍管直徑,以形成U管中時的在聚合物與金屬之間的分離;例如,若額定直徑2.54cm(1")的管使用彎曲工具或在心軸上形成具有小於約15.24cm(6")半徑的U彎管彎曲。
由於沒有足夠膠黏性所造成的失敗典型不會發生在聚乙稀(PE,"polyethylene")或交聯聚乙稀(PEX,"polyethylene")內與外層之複合管,因為使用的膠黏劑典型是馬來聚烯烴膠黏劑。膠黏劑的結構是當加熱時,其會併合入與膠黏劑接觸的PEX之表面,如此對金屬表面和聚烯烴提供優良的黏著性。此外,在PEX複合/多層管路系統中,因為連接係使用機械式配件製成,所以滲漏可最小。這些配件係束緊在配件中的管之周邊表面、環繞內金屬襯套周圍,因而密封連接。此選擇不能使用在所有配件為溶劑黏合的PVC/CPVC管路系統中。沒有任何先前技術參考文件曾揭示或識別擠出的PVC/CPVC對鋼或鋁之有效膠黏劑,而能夠使熟諳此項技術人士發現膠黏劑及在沒有過度嘗試錯誤的使用它。沒有任何先前技術文件合理地識別一膠黏劑在金屬與內和外PVC/CPVC導管之間提供必要黏合,其黏合係強到足夠符合規定的ASTM測試條件,並可長時間提供連續使用。在先前技術的說明範例中使用的膠黏劑對於對目前實際應用來說是無效的。
發現
:
(i)雖然本質上,在'311專利中揭示的任何膠黏劑是有用,且只說明特定的膠黏劑,然而沒有一樣有效的符合規定的測試條件-只有來自法國可羅馬市Mercural Corp.,公司的商用CIRE-10B,相信是從下列選擇的雙層膠黏劑:(i)含有用於底漆之高分子量聚酯膠黏劑之熱固性環氧樹脂,與熱活性、交聯聚胺基甲酸脂之面塗層;(ii)苯乙酮/-甲醛樹脂,其可選擇性以環氧樹脂改質;及(iii)基於該改質環氧樹脂的高分子共聚酯-胺基甲酸酯-聚合物之抗腐蝕底漆。連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層。進一步如金屬帶塗覆由底漆層引起的雙層膠黏劑,接著在使用前一終飾層並予以乾凅,在先前技術中沒有建議任何膠黏劑當作將CPVC至金屬的膠黏劑使用,而有效地提供符合規定ASTM測試條件所需的膠黏劑;
(ii)如在'311專利中的說明,循序地在內導管上塗覆環氧基樹脂膠黏劑,然後在成形的金屬導管上將其塗覆,無法提供服合規定測試條件的黏合;
(iii)雷射熔接金屬帶不能提供所要求的連續熔接以確保服務在壓力下之因為金屬帶的邊緣會氧化;
(iv)在金屬帶的縱向邊緣之間的間隙(間隙是藉由在環繞內導管周圍形成金屬帶而成形)不能受控制,因為擠出的內導管的外徑不被控制在目前認為決定性的限制內;
(v)在重新施加的膠黏劑上擠壓外層,而不同時施以真空以將外層加壓至金屬上,則產生的複合管不符合規定的ASTM測試條件;及,
(vi)可彎曲管只使用具有狹義定義厚度與直徑範圍的鋁導管製成。
「可彎曲」意謂複合管可以半徑6倍於管的直徑彎曲180°,沒有在層間分層或損壞管不會在依據必需的測試條件的規定下有害地影響它的性能。「可彎曲」意謂複合管可彎曲180°。6倍管直徑意謂彎曲的半徑是6倍的管直徑。可彎曲管在規定的測試條件下,作用上不會有層間分層,或損壞管,以致有害地影響其性能,具有大於6倍管直徑的半徑。
在'311專利中揭示的配件稱聲設計來避免在其周邊邊界的聚合物和金屬層之分層。致侵入微流體液滴。然而,分層典型會由於在垂直截面(垂直於管的長度,亦稱為管終端的邊緣)表面上的周邊黏合劑的劣化而發生。
'311專利的襯套9具有管狀本體(筒體),其有一凸緣從筒體徑向延伸。筒體係插在複合管的終端,且當壓入管端時,襯套凸緣的內周邊表面會鄰接其邊緣。襯套的凸緣周邊具有與複合管的外徑相同的直徑,所以具插入襯套的管端可插在彎管、聯接器或其他配件。然而,雖然'311專利陳述第3A圖、第3B圖與第3C圖說明插入物或襯套9可選擇性用來連結該發明的多層複合管與習知配件(錐形或圓柱),但是其陳述襯套的空心本體是「具徑向(sic
)延伸凸緣的圓柱」(參見'311,第8欄,第59-64列)。當圓柱筒體塗覆黏合劑,並插入管端時,黏合劑會藉由與介面的刮離而移置,結果不足的膠黏劑會影響筒體的外表面與內導管的內表面之間的密封。然後,在管中壓力下的流體迫使本身通過襯套與內導管之間的最小環隙(因為黏合劑刮離而留下),且流體會在管的邊緣中攻擊聚合物與金屬的介面。相同的問題適用於軸向延伸在'311專利的第6A圖與第6B圖中所說明聯接器的邊緣部分8。
此外,'311專利未重視複合管的整個直徑是受到ASTM D2846標準規格的規範。同時,在測試PVC/CPVC的各種壁厚度之後,小於約0.6mm(0.025")厚度的PVC/CPVC之外層無法溶劑黏合在配件,因為當該層塗上以溶劑為主之黏劑時,該層會失去其完整性及其接合劑。
本發明的方法係利用在不同的擠壓方法中使用的基本步驟,與對本方法為唯一的步驟之組合。後者唯一的步驟需要藉由先施加一底漆層,然後施加足夠量的終飾層以使PVC/CPVC黏著至金屬,以在金屬帶的兩側面塗覆上述「雙層膠黏劑」,以便複合管可符合規定的ASTM標準。雙層膠黏劑提供至少一塗覆,其包含能夠在溫度超過48.9℃(120℉)上起反應的硬化劑。當乾燥處理時,所得到的膠黏劑係提供無溶劑薄的乾層。在經塗覆膠黏劑之帶環繞第一PVC/CPVC壓出物周圍形成具有緊密相鄰邊緣的金屬導管之前,新修整該帶的縱向邊緣,並當雷射熔接邊緣不會燃燒下方第一壓出物下時,將該帶黏著至該第一壓出物,造成金屬導管緊密環繞內導管。下述其他步驟係提供具外導管的複合管,內與外導管係黏固接合至金屬導管,以致於符合規定的ASTM標準。
若要符合商業PVC/CPVC管所規定測試條件,整個方法之每一步驟係調適以合併目前發現在上述複合管之生產中為決定性之製程條件。製程步驟的狹義定義之限制包括要求在金屬護套黏著至內導管之後,該金屬護套之外徑係周邊束緊在指定的限制內,以確保獲得膠黏劑的必要接合強度。壓力愈高,接合強度更佳;但是過度壓力,易導致內導管陷縮。這些步驟的組合可能造成意外的效果。
該製程的結果在於基於壓力設計基礎,滿足法規的複合管具有直徑範圍從12.7mm(0.5")至50.8mm(2"),整個具有相同的壁厚度或不同的壁厚度(若需要)。目前皆可製造,且所有尺寸符合所規定的測試條件。為了滿足溶劑黏合,壁厚度係大於0.635mm,且最好是在範圍從0.8128mm(0.032")至1.626mm(0.064")。複合管符合ASTM F1281的第9.3、9.4、9.5節及ASTM D2846的第9.3.1節的規定;IPS配件符合ASTM F438和ASTM F439的規定;及CTS配件符合ASTM D2846的規定。
進一步,假如在該金屬帶之每一側面上塗覆一底漆層與一上塗覆層以形成一雙面塗層帶之後,雙層膠黏劑在使用前先乾凅只有特定的雙層膠黏劑發現是有效地提供使PVC/CPVC接合至金屬帶所需的黏著性,而所足以形成複合管將能通過規定測試條件。膠黏合劑的強度是無法預期,以致於時常造成內聚失敗。當嘗試將聚合物層自金屬分離造成扯開聚合物,或接合至聚合物之金屬層而不是在黏接介面上聚合物自金屬分開時,此失敗便會發生。在膠黏劑與金屬的介面是看不到分離。
本質上,當金屬緊固成形在擠製的內導管之後,金屬帶的兩緊鄰縱向邊緣所形成的間隙為使得熔接是連續且沒有「凸起」。若凸起的上表面隆起 超過金屬護套表面的0.51mm(0.020"),該凸起便是不許可,最好是隆起低於0.254mm(0.010"),以便熔接的上表面能夠順利匹配金屬導管的相鄰周圍區域。金屬的限制最大厚度允許周圍地壓迫被覆管的必要步驟,這是在以外導管被覆該金屬護套內導管前的必要處理步驟。
為了要確保連續縱向熔接,在金屬帶環繞內導管周圍成形之前,金屬帶的兩邊緣之每一者(不管鋁、或鐵族金屬,例如鋼)修整不超過10分鐘,最好不再超過1分鐘。邊緣的氧化會造成不良熔接。熔接新切割的邊緣可最小化氧化;此外,使用具有不足以燃燒如在此所述垂直隔開的下方內導管之強度的雷射會影響熔接,且減少在內導管的周圍表面上的膠黏接合劑的強度。
不管雙層膠黏劑為良好的膠黏性,膠黏劑接合的強度不會完全顯現內聚黏合,直到金屬護套周圍地壓迫以減少內導管的直徑,並維持金屬導管的外徑在±0.08mm(0.003")的指定限制內,並加熱。
用於製造任意長度複合管的製程包含在溫度範圍從約182℃(360℉)至-215℃(420℉),在第一擠壓機中擠壓聚乙烯(氯乙烯)或氯化聚乙烯(氯乙烯)的第一導管,以提供複合管的一熱內導管,該內導管具有厚度範圍從0.8mm(0.032")至1.0mm(0.040"),且直徑控制在±0.08mm(0.003")內;真空定尺寸及冷卻該熱內導管至溫度範圍從21℃(70℉)至37.74℃(100℉),並使用一經定尺寸用的套管控制其直徑在±0.08mm(0.003")的範圍內;
饋送鋁、或鐵族金屬之塗層帶(兩側面上使用無溶劑雙層膠黏塗覆及乾凅)至修邊機,該金屬具有厚度範圍從0.2mm(0.008")至1.2mm(0.048"),如此形成塗覆以厚度範圍從10μm至50μm的雙層膠黏劑之雙面塗層帶;修整雙面塗層帶的兩邊成具有0.5mm(0.020")公差的預定寬度;
縱向饋送此修整雙面塗層帶相鄰且接近內導管,並緊固地環繞內導管之周圍形成該塗層帶,如此提供具有小於0.5mm(0.020")的預定寬度之間隙的緊鄰邊緣;
在沒有燃燒在下方的內導管的狀況下,雷射熔接該金屬帶以封閉該間隙,因而提供一連續熔接之金屬導管緊貼地環繞該內導管;
周圍地束緊該熔接的金屬導管,以產生縮小內導管之外徑範圍從0.8%至1.5%;
感應加熱該包了護套及束緊管至溫度範圍從約149℃(300℉)至171℃(340℉);
在溫度範圍從約182℃(360℉)至215℃(420℉),在一第二擠壓機中擠製出聚乙烯(氯乙烯)或氯化聚乙烯(氯乙烯)的第二導管,同時施加真空範圍從汞的大約30.5-55.9cm(12-22")因在塗了膠黏劑金屬與外導管之間的環形空隙形成負壓,以便使該熱外導管膠黏固定至金屬,該外導管具有厚度範圍從0.8mm(0.032")至1.0mm(0.040"),及直徑被控制在±0.08mm(0.003")範圍內;及,
冷卻該複合管。
以前面方法形成的複合管[該管具有一內與外壁,每一者具有需要的壁厚度0.813mm+0.203mm(0.032"+0.008");及具有一金屬導管在其間,其具有厚度範圍0.2mm(0.008")至1.2mm(0.047")之間]發現符合具有額定直徑從12.54mm(0.5")至50.8mm(2")之所有管的規定測試條件。此管(具有比對應的金屬管薄的壁厚度)允許在管路系統中有較高流量與較低的壓力降。當金屬是鋁,且需要複合管是可彎曲時,要求管能夠維持想要的曲率。由於鋁導管是可彎曲,所以內與外導管的厚度係控制彎曲度。具有0.064"厚度之每一導管可提供有限度的彎曲度,不致損壞管或使彎管回復至無法接受程度的彎曲位置。如複合鋼管將不彎曲,則較厚的金屬與較厚的聚合物層可使用在鋼導管上。
前述本發明將配合附圖的示意說明並參照下面的製程步驟,及代表用來在一配件與複合管的一端之間進行防漏連接之特別的配件之詳細描述得以更佳地瞭解,其中圖式的相同數字是類似的元件。
請參考第1A圖,複合管概括地以參考數字10表示,其包含:一擠製的PVC/CPVC內導管12;一金屬導管13,最好由鋁、或鐵族金屬製成在內導管12上形成並將其包覆;PVC/CPVC製外導管14,其係擠製在金屬導管13上而將其包覆。一雙層膠黏劑的內膠黏劑層15將金屬導管13內聚地結合至內導管12;及一雙層膠黏劑的外膠黏劑層16將金屬導管13內聚地結合至外導管14。內及外導管可由相同或不同的聚合物擠製成。
請參考第1B圖,其顯示一段管20,其中內及外聚合物導管皆是19.05mm(0.75")額定直徑,每一聚合物導管具有0.813mm(0.032")的壁厚度;而且,鋁夾層厚度是0.4mm(0.016")。此管已使用彎曲工具被彎曲至90°,其中彎曲半徑是11.43cm(4.5")。為了保持穩定的90°彎曲,即於無限期間維持其90°構形,該管要彎曲至約100°。當從彎曲工具移開時,彎臂會短時間回彈(小於1小時)至90°,並保持在此狀態。雖然在指定半徑上的90°彎曲是嚴重彎曲,如圖所示,但是內導管或外導管並不會分層,且兩者皆不會在彎曲的半徑中撕裂。
內或外導管的壁厚度是範圍窄地予以限制,因為厚度小於0.635mm(0.025")會太薄而無法可靠溶劑黏固;而厚度大於3.18mm(0.125")在彎曲的半徑中會有裂開的傾向,即使導管內聚地結合至金屬亦然。
若導管是以PVC製成,可擠壓的PVC係廣泛地在全世界各地皆可得到可能之化合物,並用來製造廣範圍之物件及符合需要測試條件的管。若導管是以CPVC製成,可擠壓的CPVC亦可廣泛地在全世界各地皆可得到,且主要用來製造符合需要測試條件的管。不需要更詳細描述,但是各種要點將在下面予以提供。
根據ASTM-D1243的特性粘度(I.V.,Inherent Viscosity)PVC的分子量範圍可從約0.2至約2.0,最佳地,從約0.4至1.6,最佳地從約0.7至1.2。擠壓級PVC包括各種添加劑,包括加工助劑、穩定劑、抗衝改性劑等。最佳商用PVC是Oxyvinyl's Geon1344。
可擠壓的CPVC在25℃典型地具有密度範圍從約1.45g/cc至約1.67g/cc,較佳地是在25℃具有範圍從約1.51g/cc至1.58g/cc;而且,以微差掃描熱量計(DSC,Differential Scanning Calorimeter)測量,玻璃轉化溫度(Tg)範圍是從110℃至150℃,較佳地範圍從約120℃至140℃,正如擠壓級PVC,擠壓級CPVC包括各種添加劑,其包括加工助劑、穩定劑、抗衝改性劑等。用於擠壓管的大部分較佳商用CPVC可從Lubrizol Advanced Materials,Inc.公司的Temprite® 88620 TAN 309獲得。
請參考第2圖,圖解說明兩複合管10(只顯示一管)之一者的終端,每一端具有相同的額定直徑,將與具有筒體31的PVC/CPVC的聯接器30一起接合,其中相對的前與後部分32和33係分別向外呈錐形化,以便該筒體的每一終端的直徑可如ASTM 2846第6.1.3.1節所示予以提供,其在此係以引用方式併入本文供參考。(圖中並未顯示在筒體之每一部分中的向外呈錐形)。
在筒體31中,在大約其中點附近,有一徑向延伸內部凸緣34,在使用膠黏劑塗覆管端的外表面之後,該管端的邊緣17牢靠地抵壓在此凸緣34,所以管端可溶劑黏合(未顯示第二管的終端)聯接器合件。緊鄰凸緣34之每一前與後部分的內徑其範圍從約0.025mm至0.25mm(0.001至0.010"),大於將插入的筒體部分之管外徑。在管10的終端插入筒體31的前部分32之前,該端需充份使用膠黏劑塗覆,如此塗覆了該端的外表面及其邊緣。
徑向凸緣34係徑向向內延伸至少等於在筒體31的外徑與內導管12的內徑之間的距離,最好是大於其間距離的10%。雖然筒體中的錐度輕微,但是足以確保有足夠的膠黏劑保留在終端的外導管14的外表面上與邊緣17上,直到抵壓在凸緣34。由於內與外導管12和14的周圍端係分別如此地溶劑黏合在凸緣34上,所以在內導管12與金屬導管13之間的邊界與在外導管14與金屬導管13之間的邊界係每一者密封,以防止在複合管10中的壓力下,微水滴或其他流體液滴之滲透。
複合管10的終端可類似以溶劑為主之膠黏劑予以溶劑黏合入具有至少一管接合筒體之PVC/CPVC配件,例如管帽、L形管、內外接彎頭、T形管件,其適宜地定尺寸以配合該管的尺寸。彎頭的每一筒體係向外呈錐形,且鄰近彎曲處的筒體內部部分具有直徑範圍從約0.025mm至0.25mm(0.001"至0.010"),大於該管的外徑。因該管與管配件組合係類似第2圖所示的組合,故並未在圖中說明。
請參考特別是第3A圖係顯示例如使用在PEX管的習知金屬襯套40,其具有一徑向向外延伸周圍凸緣41與一圓柱筒體42。但是金屬襯套不是溶劑可黏合的,且為了在此使用,需要提供到目前從未製造的PVC/CPVC襯套。
請參考第3B圖,其係顯示一新穎的襯套50的端視圖,該襯套具有一向內成錐形之筒體51與一徑向向外延伸的凸緣52。筒體51是呈垂直向錐形,以致於筒體端53的內徑(遠離凸緣52的末端)符合下面公佈有關0.5"CTS、0.75"CTS和1"CTS的管徑之尺寸規定。較大管的尺寸是藉由類比計算加以決定。
上述尺寸規定筒體的內部錐度是範圍,是相對於在筒體與徑向凸緣相交點水平線,大於0.4°但小於4°。
請參考第3C圖,其係顯示沿著第3B圖中的襯套50的平面C-C所作之截面端視圖。習知的襯套40的圓柱筒體42以假想線顯示而錐形筒體51以實線顯示。在凸緣52的筒體51之外徑係對應至複合管10的內導管的內徑。當凸緣52在複合管10(參見第2圖)的終端的邊緣17壓下時,因為筒體52是向內成錐形,所以在襯套的外表面上塗覆的膠黏劑是在凸緣52上密封邊緣17,並避免在管中的壓力下,流體注入複合管的邊界。筒體51的端53是呈錐形。
請參考第4圖,其係顯示複合管10的一終端17與襯套50之總成,該襯套已套在該管的終端。因為在襯套之筒體中成向內部錐形,在筒體插入管內之前,於筒體51的外表面與凸緣52的面對表面上塗覆之以溶劑為主之黏劑54是不會被刮除。該以溶劑為主之黏劑54之一部分係保留在內導管12的內表面的塗覆表面上與在管的邊緣17上,造成流體密封連接,密封在聚合物導管12和14與金屬導管13之間的邊界而防止在壓力下,注入微流體液滴。由於凸緣52的周圍表面與外導管14的外表面具有相同直徑,所以該總成可插入標準配件。
請參考第5A圖,其係顯示一較佳的聯接器60,其具有一圓柱外筒體61,該圓柱外筒體具有約位於筒體61中點的徑向向內延伸凸緣62,且同軸地支撐一錐形內筒體形構件63,其具有相對前端64與後端65,以錐形狀朝向中心收斂,其斜度範圍從大於0.4°至小於4°。錐形筒體之每一端係作為襯套50的錐形筒體51(參見第4圖),且凸緣62如襯套50的錐形凸緣52的功能,除了凸緣62係作為管的共同凸緣,每一終端可抵壓在基上。當管10的終端之表面塗覆予膠黏劑並插入聯接器60的一端時,膠黏劑保留在該端的表面上,並向凸緣62推擠。第5B圖顯示具錐形端64和65的較佳聯接器60,其中將錐形狀予以特寫。如第4圖所示,當管10的終端抵壓凸緣62時,膠黏劑提供溶劑黏合流體密封,其亦密封在聚合物導管12和14與金屬導管13之間的邊界,防止在壓力下注入微流體液滴。
請參考第6圖,其係圖解說明製造複合管10之製程步驟。上述聯接器及襯套之每一者具有向外呈錐形開口之及所有其他配件,例如L形管、內外接彎頭、T形管件及其他類似件,能夠以適當組態之模具以習知方式予以射出成形。除了製程條件改變以調適將擠壓聚合物的物理性質之外,PVC或CPVC的製程步驟是相同的。下面提供的製程條件係用於CPVC,且更特別地係用於製造具有額定直徑12.54mm(0.50")的複合管,每一內與外導管具有厚度0.813mm(0.032")且在其間夾有一厚度4mm(0.016")的鋁導管。
除了修整在兩面塗覆有膠黏劑之經塗覆之金屬帶邊緣的步驟之外(其步驟可獨立於其他製程步驟,假設該金屬帶是在饋送至金屬成形與熔接步驟之前進行修整),該等製程步驟是連續的,而且如下所述:
(1)擠壓內導管:
Temprite88620 TAN 309 CPVC的粉末是從漏斗饋送至雙螺桿擠壓機,其在溫度範圍從193℃至204℃(380℉至400℉)操作,以產生一具有外徑15.9mm(0.625”)之擠出物:
(2)冷卻內導管:
熱內導管是以定尺寸模具與套管中進行真空定尺寸,以控制內導管的外徑在±76.2μm(0.003")的限制內,並透過一管模予以擠出,以產生薄厚壁管0.8mm(0.032")厚度,其公差受控制至+0.008mm(0.0003")。然後,已定尺寸之導管冷卻至溫度範圍從21℃(70℉)至37.74℃(100℉)。較佳地,在經冷卻的內導管饋送至一金屬成形與熔接機之前,經冷卻的內導管會拉過一調整輥,以控制導管的直徑與厚度。
(3)饋送鋁帶至一修邊機:
在兩面上塗裝雙層膠黏劑(乾凅後形成具有厚度範圍從10μm至50μm之薄乾層)的一鋁帶之邊緣(5.7cm(2.25")寬與0.4mm(0.016")厚)係重新修整至寬度5.0cm(1.97"),公差±50.8μm(0.002")。
(4)成形及熔接金屬帶以形成金屬導管:
當修整過的金屬帶進入成形與熔接機時,該金屬帶係緊位在內導管之下方被饋送。該金屬帶是在環繞內導管的周圍成形,所以修整過的邊緣提供約0.25mm(0.010")的間隙,小到足夠讓適當強度的雷射連續縱向對頭式熔接該金屬條,以便造形金屬導管。選擇雷射強度,以便不使過度加熱該被覆之內導管損壞內層的聚合物,然而提供完全穿透金屬厚度的熔接。
(5)束緊該被覆內導管:
為了確保被覆內導管的外徑維持在±0.254mm(±0.010"),其係圍繞地束緊在相對部署之有槽輥軸之間;藉著計算,外徑的公差係藉由減少內導管的外徑範圍從0.8%至1.5%予以維護。
(6)加熱束緊之被覆內導管:
束緊之被覆內導管是在感應加熱器中加熱至溫度範圍從約149℃(300℉)至171℃(340℉),以活性化雙層膠黏劑,確保獲得的膠黏接合劑只將會內聚不足而失敗,並將金屬表面預熱至金屬將隨後被覆聚合物外層之溫度。
(7)擠壓外導管:
加熱的被覆內導管係導入十字頭模具的密封前室,其中在外導管要擠製在加熱的膠黏劑塗覆的金屬上之前,施加真空。範圍從汞的31cm至56cm(12-22")之真空會在圍繞金屬導管周圍建立負壓,以便擠至金屬導管之聚合物可強力吸至膠黏劑塗覆的金屬,因而當聚合物是在溫度範圍從193℃至204℃(380℉至400℉)塗覆在膠黏劑時,確保活性化黏合劑與內聚結合。該十字頭模具可確保外導管的厚度是0.032",控制在±50.8μm(0.002")公差範圍內。
(8)冷卻完成的複合管:
在熱複合管切成選定長度或軋成選定長度的管線圈之前,來自十字頭模具的熱複合管是在冷卻水箱中冷卻至室溫。當測試時,發現能夠符合計算的規定測試條件,使該管在管路系統中提供十年的使用。
從前面所述可清楚明白,在先前技術廣泛冀望之揭示十分缺乏提議製作符合規定測試條件的複合管所需的狹義定義之步驟。
膠黏接合劑的強度臨限可藉由顯示黏著PVC或CPVC至前述金屬的數據加以證明,使用先前技術建議或認為的膠黏劑係無法提供內聚結合。對於符合需要測試條件的複合管而言,本質上,每一聚合物導管係可接受黏合至金屬導管。「可接受黏合」意謂在沒有任何機械式咬合或聚合物與金屬的連鎖下,在90°剝離及2ins/min的應變率上測量,聚合物黏合至金屬是至少0.9kg/cm(51b.ft/inch)。
2.54cm(1")額定直徑管(含CPVC的內與外導管,每一者具有1.016mm(0.040")厚度及具有1.016mm(0.040")厚的鋁夾層)的最小剝離強度在三個不同溫度上是以1b.ft/in(N/mm)為單位,針對Bynel40-E529,商用以聚烯烴為主之膠黏劑,且特別地有效的Mercural雙層膠黏劑是在下表1中顯示:
以不同膠黏劑的其他環剝測試:
下列商用膠黏劑之每一者係藉由塗刷膠黏劑以施加薄層至19.05mm(0.75")額定直徑鋁管。約1.016mm(0.040")的Temprite88620 TAN 309 CPVC之外層然後在鋁管上擠出。然後,經冷卻、塗覆的管在短距離上縱向分割,至少足夠讓該分割的聚合物的一邊緣箝住,並以如在ASTM D3167中詳細描述從管周邊表面剝離。只在82℃進行測試,以決定其是否通過。此測試的失敗宣告膠黏劑無法使用。
PVC/CPVC導管厚度的決定性可藉由下列數據證明,其顯示厚度大於3.18mm(0.125")無法以雙層膠黏劑提供內聚結合;且厚度小於0.635mm(0.025")無法提供溶劑黏合導管,因為當黏合劑塗覆管的終端插入配件的筒體時,塗覆膠黏劑的外導管之薄周層有位移或滑離金屬導管的傾向。下面顯示的數據是指出在管的終端上的外導管是否位移的視覺觀察。在規定的測試條件下,任何位移置將導致接合失敗。
每一者的三個樣本係可測試。數據如下所示:
組合的管與配件之流體靜力承受壓力測試:
六組溶劑黏合的配件與19.05mm(0.75")額定直徑管(其具有CPVC內與外導管,每一者具有壁厚度1.016mm(0.040");及一鋁導管,其具有厚度1.0mm(0.040"),其每一端在插於彎管前係與襯套安裝,於82.2℃(180℉),經歷6分鐘加壓至3.9MPa(551psi)。
所有樣本通過。
六個其他組的溶劑黏合配件與19.05mm(0.75")額定直徑複合CPVC管(類似上面使用的類似物),於82.2℃(180℉),經歷4小時加壓至2.88MPa(403psi)。
所有樣本通過。
使用數組具PVC內與外導管、與混合的內與外PVC/CPVC導管的溶劑黏合配件預期會有類似結果。
10...複合管
12...擠出的內導管
13...金屬導管
14...外導管
15...內膠黏劑層
16...外膠黏劑層
17...邊緣
20...管
30...聯接器
31...筒體
32...前部分
33...後部分
34...凸緣
40...金屬襯套
41...周圍凸緣
42...圓柱筒體
50...襯套
51...筒體
52...凸緣
53...筒體端
54...溶劑為主之黏合劑
60...聯接器
61...圓柱外筒體
62...凸緣
63...錐形內筒體形構件
64...前端
65...後端
第1A圖為複合管的縱剖面之立體圖。
第1B圖為一段已彎曲90°管的部分斷面立體圖。
第2圖為一聯接器的部分斷面之側視圖,其係顯示一習知聯接器具有相對向外成錐形之端(或承窩),每一錐形端是根據ASTM D2846的第6.1.3.3節予以定尺寸。(圖中未顯示該聯接器之每一前及後端或承窩之錐度)。
第3A圖為一習知PVC/CPVC襯套之側視圖,其具有如'311專利所示的一圓柱筒體。
第3B圖為具有一錐形筒體的新穎襯套之上視圖,其中錐形筒體具有下面規定之尺寸(錐度作誇大表示)。
第3C圖為沿著第3B圖的平面3C-3C所作之斷面圖,其顯示在第3B圖所示之新穎襯套的錐形筒體,且參照'311專利的襯套其圓柱筒體係假想線表示。
第4圖為複合管之斷面圖,顯示複合管已插入第3圖所示新穎襯套,為了清楚,未顯示襯套錐形狀。
第5A圖為一較佳聯接器之斷面立體圖,其可用於接合兩段管或管線圈毋須將第3圖顯示的襯套插入在每一管之一端,該聯接器具有一在筒體兩端中間處以徑向延伸內凸緣與管之內壁隔開的內同軸筒體,且每一筒體係相對地錐形化(此圖未顯示錐度)。
第5B圖為在第5A圖中顯示的聯接器之斷面圖,其係顯示相對錐形筒體(錐度已被誇張)。
第6圖為在第1圖所顯示用於製造複合管的製程步驟之圖解表示圖。
10...複合管
12...擠出的內導管
13...金屬導管
14...外導管
15...內膠黏劑層
16...外膠黏劑層
Claims (11)
- 一種用於製造具有任意長度複合管之方法,其包括:(a)在溫度範圍從約182℃至215℃(360℉-420℉),在第一擠壓機中擠壓出聚氯乙烯(PVC)或氯化聚乙烯(CPVC)之第一導管,以提供用於該複合管的熱內導管,該內導管具有厚度範圍從大於0.635mm至3.18mm(0.025"-0.125"),且直徑控制在±76.2μm(0.003")範圍內;(b)真空定徑及冷卻該熱內導管至溫度範圍從21℃至37.74℃(70℉至100℉),並使用一定徑套管控制其直徑在±76.2μm(0.003")範圍內;(c)饋送鋁或鐵金屬之塗層帶至一修邊機,該塗層帶係在兩邊施加一雙層膠黏劑作為一底漆層及一外飾層予以塗層並乾凅,以形成塗覆了無溶劑膠黏劑之雙面塗層帶,該鋁或鐵金屬之塗層帶厚度範圍從0.2mm至1.2mm(0.008"至0.048");(d)修整該雙面塗層帶的兩條縱向側邊,以提供公差±0.08mm(0.003")預定寬度的經修整雙面塗層帶;(e)在該內導管下方,饋送該經修整的雙面塗層帶,並環繞該內導管周圍緊密地成形該經修整雙面塗層帶,以在該經修整雙面塗層帶的相鄰縱向邊緣之間提供小於0.5mm(0.020")的預定寬度之間隙;(f)在不會燃燒在下方之內導管情況下,雷射熔接該 經修整雙面塗層帶以封閉該間隙,以提供一連續熔接之金屬導管緊貼地環繞該內導管;(g)在周圍束緊該熔接的金屬導管,以產生縮小內導管外徑範圍從0.8%至1.5%;(h)感應加熱該包覆了護套及束緊的管至溫度範圍從約149℃(300℉)至171℃(340℉);(i)在溫度範圍從約182℃至215℃(360℉至420℉),在一第二擠壓機中壓出PVC或CPVC的第二導管,同時施加真空範圍從汞的大約38至51cm(15-20"),以在塗了膠黏劑之金屬與將被塗覆的外導管之間的環形空隙形成負壓,使該熱外導管膠黏固定至金屬,該外導管具有厚度範圍從大於0.635mm(0.025")至3.18mm(0.125"),且直徑控制在±50.8μm(0.002")的範圍內;及(j)冷卻該複合管。
- 如申請專利範圍第1項之方法,其中包括在步驟(b)提供調整輥以中間定徑及冷卻該內導管;及饋送該經修整雙面塗層帶至金屬成形及熔接步驟(e)。
- 如申請專利範圍第1項之方法,其中塗覆該雙層膠黏劑厚度範圍從10μm至50μm,並從由下列所組成的群組中選取:(i)含有用於底漆層之高分子量聚酯膠黏劑之熱固性環氧樹脂、與用於面塗層之熱活性、交聯聚胺基甲酸 脂;(ii)苯乙酮/-甲醛樹脂,其可選擇性使用環氧樹脂改質;及(iii)基於該環氧樹脂改質的高分子共聚酯-胺基甲酸酯-聚合物之防腐蝕底漆、連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層。
- 一種複合管總成,包括具有任意長度之複合管及一聚氯乙烯/氯化聚乙烯(PVC/CPVC)管配件,其中該複合管包括:(a)一聚氯乙烯(PVC)或氯化聚乙烯(CPVC)之第一導管,其厚度範圍從0.813mm至3.18mm(0.032"-0.125")、且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑範圍,作為該複合管的內導管;(b)一鋁或鐵金屬之第二金屬導管,其兩邊塗覆厚度範圍從10μm至50μm的乾的無溶劑雙層膠黏劑層,該第二金屬導管具有一縱向熔接,平滑地匹配厚度範圍從0.2mm至1.2mm的該第二金屬導管的相鄰周圍區域,該第二金屬導管緊密地圍繞該內導管的周圍,並內聚地結合至該內導管,其中該雙層膠黏劑係從由下列所組成的群組中選取:(i)含有用於底漆層之高分子量聚酯膠黏劑之熱固性環氧樹脂、與用於面塗層之熱活性、交聯聚胺基甲酸脂;(ii)苯乙酮/-甲醛樹脂,其可選擇性使用環氧樹脂改質;及(iii)基於該環氧樹脂改質的高分子共聚酯-胺基甲酸酯-聚合物之防腐蝕底漆、連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層;及 (c)一PVC或CPVC之第三導管,其厚度範圍從0.635mm至3.18mm(0.025"至0.125"),且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑,作為該複合管的外導管,該第三導管係使用黏合劑黏著地固定至該金屬導管;其中該PVC/CPVC管配件具有安裝該複合管的一終端的管接合筒體,並使用一溶劑型接著劑進行溶劑黏接以提供一流體密封連接。
- 如申請專利範圍第4項之複合管總成,其中該第二金屬導管係由鋼製成。
- 一種複合管總成,包括具有任意長度的複合管及一PVC/CPVC管聯接器,其中該複合管包括:(a)一聚氯乙烯(PVC)或氯化聚乙烯(CPVC)之第一導管,其厚度範圍從0.813mm至3.18mm(0.032"-0.125")、且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑範圍,作為該複合管的內導管;(b)一鋁或鐵金屬之第二金屬導管,其兩邊塗覆厚度範圍從10μm至50μm的乾的無溶劑雙層膠黏劑層,該第二金屬導管具有一縱向熔接,平滑地匹配厚度範圍從0.2mm至1.2mm的該第二金屬導管的相鄰周圍區域,該第二金屬導管緊密地圍繞該內導管的周圍,並內聚地結合至該內導管,其中該雙層膠黏劑係從由下列所組成的群組中選取:(i)含有用於底漆層之高分子量聚酯膠黏劑之熱固性環氧樹脂、與用於面塗層之熱活性、交聯聚胺基 甲酸脂;(ii)苯乙酮/-甲醛樹脂,其可選擇性使用環氧樹脂改質;及(iii)基於該環氧樹脂改質的高分子共聚酯-胺基甲酸酯-聚合物之防腐蝕底漆、連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層;及(c)一PVC或CPVC之第三導管,其厚度範圍從0.635mm至3.18mm(0.025"至0.125"),且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑,作為該複合管的外導管,該第三導管係使用黏合劑黏著地固定至該金屬導管;其中該PVC/CPVC管聯接器具有管接合筒體,該管接合筒體具有相對向外成錐形的前及後筒體部分,該管接合筒體約在其中心點具有一徑向向內延伸的凸緣,且該複合管係插入並使用溶劑型接著劑予以溶劑黏接在該筒體的至少一部分。
- 如申請專利範圍第6項之複合管總成,其中該第二金屬導管係由鋼製成。
- 一種複合管總成,包括具有任意長度的複合管及一PVC/CPVC管聯接器,該複合管包括:(a)一聚氯乙烯(PVC)或氯化聚乙烯(CPVC)之第一導管,其厚度範圍從0.813mm至3.18mm(0.032"-0.125")、且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑範圍,作為該複合管的內導管;(b)一鋁或鐵金屬之第二金屬導管,其兩邊塗覆厚度範圍從10μm至50μm的乾的無溶劑雙層膠黏劑層,該第 二金屬導管具有一縱向熔接,平滑地匹配厚度範圍從0.2mm至1.2mm的該第二金屬導管的相鄰周圍區域,該第二金屬導管緊密地圍繞該內導管的周圍,並內聚地結合至該內導管,其中該雙層膠黏劑係從由下列所組成的群組中選取:(i)含有用於底漆層之高分子量聚酯膠黏劑之熱固性環氧樹脂、與用於面塗層之熱活性、交聯聚胺基甲酸脂;(ii)苯乙酮/-甲醛樹脂,其可選擇性使用環氧樹脂改質;及(iii)基於該環氧樹脂改質的高分子共聚酯-胺基甲酸酯-聚合物之防腐蝕底漆、連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層;及(c)一PVC或CPVC之第三導管,其厚度範圍從0.635mm至3.18mm(0.025"至0.125"),且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑,作為該複合管的外導管,該第三導管係使用黏合劑黏著地固定至該金屬導管;其中該PVC/CPVC管聯接器具有:接合管之圓柱外筒體,該接合管之圓柱外筒體具有相對之前及後圓柱筒體部分,該接合管之圓柱外筒體約在其中心點附近具有一徑向向內延伸的凸緣;和內筒體,該內筒體被該凸緣同軸地支撐,且該複合管係插入並使用溶劑型接著劑予以溶劑黏接在該接合管之圓柱外筒體的至少一部分。
- 如申請專利範圍第8項之複合管總成,其中該第二金屬導管係由鋼製成。
- 一種複合管總成,包括具有任意長度的複合管及一 PVC/CPVC襯套,其中該複合管包括:(a)一聚氯乙烯(PVC)或氯化聚乙烯(CPVC)之第一導管,其厚度範圍從0.813mm至3.18mm(0.032"-0.125")、且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑範圍,作為該複合管的內導管;(b)一鋁或鐵金屬之第二金屬導管,其兩邊塗覆厚度範圍從10μm至50μm的乾的無溶劑雙層膠黏劑層,該第二金屬導管具有一縱向熔接,平滑地匹配厚度範圍從0.2mm至1.2mm的該第二金屬導管的相鄰周圍區域,該第二金屬導管緊密地圍繞該內導管的周圍,並內聚地結合至該內導管,其中該雙層膠黏劑係從由下列所組成的群組中選取:(i)含有用於底漆層之高分子量聚酯膠黏劑之熱固性環氧樹脂、與用於面塗層之熱活性、交聯聚胺基甲酸脂;(ii)苯乙酮/-甲醛樹脂,其可選擇性使用環氧樹脂改質;及(iii)基於該環氧樹脂改質的高分子共聚酯-胺基甲酸酯-聚合物之防腐蝕底漆、連同基於高分子交聯共聚酯-胺基甲酸酯-聚合物之面塗層;及(c)一PVC或CPVC之第三導管,其厚度範圍從0.635mm至3.18mm(0.025"至0.125"),且直徑範圍從12.54mm至50.8mm(0.5"至2.0")額定直徑,作為該複合管的外導管,該第三導管係使用黏合劑黏著地固定至該金屬導管;其中該PVC/CPVC襯套被插入該複合管的一端,該PVC/CPVC襯套具有一錐形筒體且在該錐形筒體的一前 端有一徑向向外延伸的凸緣,該凸緣的外徑實質與該複合管的外徑相同,該錐形筒體另一後端的錐形筒體外徑係小於該錐形筒體前端的直徑,所以該錐形筒體的向內錐度相對於水平面是在大於1°但小於10°範圍內,且該錐形筒體是使用溶劑型接著劑予以溶劑黏接在該複合管的一端。
- 如申請專利範圍第10項之複合管總成,其中該第二金屬導管係由鋼製成。
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TW100147608A TW201223736A (en) | 2007-11-30 | 2008-11-27 | PVC/CPVC composite pipe with metal interlayer and process for making it |
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BRPI0819452A2 (pt) | 2019-09-24 |
EP2514588A1 (en) | 2012-10-24 |
KR20100100928A (ko) | 2010-09-15 |
MX2010005784A (es) | 2010-06-09 |
US20120175006A1 (en) | 2012-07-12 |
CO6280412A2 (es) | 2011-05-20 |
US20090139661A1 (en) | 2009-06-04 |
TW201223736A (en) | 2012-06-16 |
CA2762007A1 (en) | 2009-06-04 |
CR11458A (es) | 2010-06-30 |
EP2514588B1 (en) | 2014-03-19 |
AU2008329731A1 (en) | 2009-06-04 |
TW200932497A (en) | 2009-08-01 |
KR20120014035A (ko) | 2012-02-15 |
KR101567892B1 (ko) | 2015-11-10 |
CN102494209A (zh) | 2012-06-13 |
EP2214901A1 (en) | 2010-08-11 |
CA2706852C (en) | 2016-04-12 |
WO2009070629A1 (en) | 2009-06-04 |
CA2706852A1 (en) | 2009-06-04 |
EP2214901B1 (en) | 2014-03-05 |
CN101878110B (zh) | 2014-08-13 |
CN101878110A (zh) | 2010-11-03 |
AR069515A1 (es) | 2010-01-27 |
AU2008329731B2 (en) | 2013-04-04 |
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