WO2018051733A1 - 中空成形品および中空成形品の製造方法 - Google Patents
中空成形品および中空成形品の製造方法 Download PDFInfo
- Publication number
- WO2018051733A1 WO2018051733A1 PCT/JP2017/029789 JP2017029789W WO2018051733A1 WO 2018051733 A1 WO2018051733 A1 WO 2018051733A1 JP 2017029789 W JP2017029789 W JP 2017029789W WO 2018051733 A1 WO2018051733 A1 WO 2018051733A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- hollow molded
- molded article
- molded product
- polyamide
- resin
- Prior art date
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C1/00—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge
- F17C1/16—Pressure vessels, e.g. gas cylinder, gas tank, replaceable cartridge constructed of plastics materials
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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
- 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
- B29C66/71—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 characterised by the composition of the plastics material of the parts to be joined
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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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- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
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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
- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
- B29C45/0001—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor characterised by the choice of material
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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
- B29C48/022—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the choice of material
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
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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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- B29C69/00—Combinations of shaping techniques not provided for in a single one of main groups B29C39/00 - B29C67/00, e.g. associations of moulding and joining techniques; Apparatus therefore
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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
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/06—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using friction, e.g. spin welding
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/06—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using friction, e.g. spin welding
- B29C65/0672—Spin welding
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/08—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using ultrasonic vibrations
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
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- B29C65/1403—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation characterised by the type of electromagnetic or particle radiation
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/14—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using wave energy, i.e. electromagnetic radiation, or particle radiation
- B29C65/16—Laser beams
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/02—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure
- B29C65/18—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using heated tools
- B29C65/20—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by heating, with or without pressure using heated tools with direct contact, e.g. using "mirror"
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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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- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
- B29C65/72—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor by combined operations or combined techniques, e.g. welding and stitching
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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
- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/01—General aspects dealing with the joint area or with the area to be joined
- B29C66/02—Preparation of the material, in the area to be joined, prior to joining or welding
- B29C66/024—Thermal pre-treatments
- B29C66/0242—Heating, or preheating, e.g. drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
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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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- B29C66/54—Joining several hollow-preforms, e.g. half-shells, to form hollow articles, e.g. for making balls, containers; Joining several hollow-preforms, e.g. half-cylinders, to form 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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- B29K2077/00—Use of PA, i.e. polyamides, e.g. polyesteramides or derivatives thereof, as moulding material
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2260/00—Purposes of gas storage and gas handling
- F17C2260/03—Dealing with losses
- F17C2260/035—Dealing with losses of fluid
- F17C2260/036—Avoiding leaks
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F17—STORING OR DISTRIBUTING GASES OR LIQUIDS
- F17C—VESSELS FOR CONTAINING OR STORING COMPRESSED, LIQUEFIED OR SOLIDIFIED GASES; FIXED-CAPACITY GAS-HOLDERS; FILLING VESSELS WITH, OR DISCHARGING FROM VESSELS, COMPRESSED, LIQUEFIED, OR SOLIDIFIED GASES
- F17C2270/00—Applications
- F17C2270/01—Applications for fluid transport or storage
- F17C2270/0165—Applications for fluid transport or storage on the road
- F17C2270/0184—Fuel cells
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/32—Hydrogen storage
Definitions
- the present invention relates to a hollow molded product that comes into contact with high-pressure hydrogen having a welded portion. More specifically, it is a hollow molded product having a welded portion controlled to a specific spherulite size, and has excellent tensile strength at the welded portion, so that cracking at the welded portion can be prevented even after repeated filling and releasing of high-pressure hydrogen. Utilizing the characteristics that can suppress the occurrence, it is usefully used.
- a hydrogen tank liner having excellent gas barrier properties and excellent impact resistance even at low temperatures for example, a hydrogen tank liner made of a polyamide resin composition containing polyamide 6, copolymer polyamide, and an impact resistant material has been studied (for example, , See Patent Document 1).
- the hydrogen tank liner described in Patent Document 1 has an average spherulite size of the polyamide resin composition larger than 20 ⁇ m, and since the tensile strength at the welded portion is low, hydrogen gas permeation from the welded portion and There is a problem that hydrogen gas is easily dissolved in the resin, and cracking occurs in the welded portion of the hydrogen tank liner when filling and releasing of high-pressure hydrogen are repeated.
- the present invention has been made in view of the above-described problems of the prior art, and provides a hollow molded article that is excellent in tensile strength of a welded portion and that suppresses the occurrence of cracks in the welded portion even after repeated filling and releasing of high-pressure hydrogen.
- the present invention has the following configuration.
- a hollow in contact with high-pressure hydrogen characterized in that the tensile strength of the test piece including the joint portion of the hollow molded article is 80% or more with respect to the tensile strength of the test piece not including the joint portion of the hollow molded article. Molding.
- a method of manufacturing a hollow molded article wherein two or more divided bodies are selected from hot plate welding, infrared welding, and infrared welding / vibration welding in which vibration welding is performed after warming a welding portion with infrared rays Including a step of bonding by a method to form a hollow molded article, wherein the hollow molded article has an average spherulite size of 20 ⁇ m or less at a portion 500 ⁇ m inside from the surface of the hollow molded article, A method for producing a hollow molded article that is exposed to high-pressure hydrogen, wherein the tensile strength of the test piece containing 80% or more of the tensile strength of the test piece not including the joint portion of the hollow molded article.
- the hollow molded article of the present invention is excellent in tensile strength at the welded portion, and is capable of suppressing the occurrence of cracks in the welded portion even after repeated filling and releasing of high-pressure hydrogen. It can be usefully used as a molded article.
- a hollow molded article having a joint portion obtained by welding two or more divided bodies of the present invention by welding (hereinafter sometimes referred to as “hollow molded article”) is an average sphere at a portion 500 ⁇ m inside from the surface of the hollow molded article.
- the crystal size is 20 ⁇ m or less, and the tensile strength of the test piece including the joint portion of the hollow molded article is 80% or more with respect to the tensile strength of the test piece not including the joint portion joined by welding. It is a hollow molded product.
- the hollow molded article of the present invention is preferably made of a resin material, and is preferably made of a resin composition containing a resin component and other additives.
- the resin component is preferably a thermoplastic resin.
- the hollow molded product of the present invention has an average spherulite size of 20 ⁇ m or less at a portion 500 ⁇ m inside from the surface of the hollow molded product.
- a hollow molded product having an average spherulite size larger than 20 ⁇ m at the inner part of 500 ⁇ m from the surface of the hollow molded product cannot suppress the permeation of hydrogen gas or the dissolution of hydrogen into the resin, and is charged and released with high-pressure hydrogen. Defects are likely to occur when pressure is repeated.
- the hollow molded article can suppress the occurrence of defect points even when repeated filling and releasing of hydrogen at a higher pressure, so that the average spherulite size in the portion 500 ⁇ m inside from the surface of the hollow molded article may be 15 ⁇ m or less. More preferably, it is preferably 10 ⁇ m or less.
- the lower limit of the average spherulite size is not limited, but is usually about 0.01 ⁇ m.
- the average spherulite size is cut out from the surface of the hollow molded article 500 ⁇ m from the ultra-thin section, the section is observed with a polarizing microscope or a transmission electron microscope, a photograph of the spherulite is taken, and then image analysis is performed. It is a value obtained by calculating the number average of the diameter of the spherulites with an apparatus or the like.
- the method of setting the average spherulite size in the inner portion of 500 ⁇ m from the surface of the hollow molded product to 20 ⁇ m or less is not particularly limited as long as such a hollow molded product can be obtained.
- a method in which molding is performed while applying vibration energy a method in which molding is performed with a cycle cooling heating method in which a resin is shaped in a state in which the mold surface is cooled and then heated, and a polyamide is formed.
- Examples thereof include a method of adding a crystal nucleating agent to the resin and a method of using a polyamide resin composition in which two specific types of polyamide resins are blended.
- the hollow molded article of the present invention is preferably a hollow molded article made of a polyamide resin composition.
- a method using a polyamide resin composition blended with is preferably used.
- the hollow molded article of the present invention has a joint location where two or more divided bodies are joined by welding, and the tensile strength of the test piece including the joint location (hereinafter, sometimes referred to as the tensile strength of the joint location).
- the tensile strength is 80% or more with respect to the tensile strength of the test piece that does not include the joined portion joined by welding (hereinafter, may be referred to as tensile strength other than the joined portion). If the tensile strength of the part joined by welding is lower than 80% with respect to the tensile strength other than the part joined by welding, the permeation and dissolution of hydrogen gas from the welded part tends to occur, and high-pressure hydrogen filling and releasing pressure can be reduced. If it repeats, it will be easy to generate a crack in a welding part.
- the hollow molded product can further suppress the permeation of hydrogen gas from the welded portion and the dissolution of the hydrogen gas into the resin, and can suppress the occurrence of cracks in the welded portion even after repeated filling and releasing of high-pressure hydrogen.
- the tensile strength of the test piece including the joint portion where two or more divided bodies are joined by welding is 85% or more with respect to the tensile strength of the test piece not including the portion joined by welding, 90 % Or more is more preferable, and it is further more preferable that it is 95% or more.
- the measurement method of the tensile strength of the joining location which joined two or more division bodies by welding, and the tensile strength other than the said joining location is demonstrated.
- a rectangular test piece is cut out from a hollow molded article in order to measure the tensile strength of the joint where two or more pieces are joined by welding.
- a test piece cut out so that the joining portion joined by welding is positioned at the center in the long side direction of the test piece so as to be perpendicular to the long side direction and the short side is 10 mm is prepared.
- test piece cut into a rectangle so that the short side is 10 mm is prepared so that the tensile test can be performed in the same direction as the tensile direction of the sheet.
- the thickness of the hollow molded product of the present invention is not particularly limited, but is preferably in the range of 1 mm to 5 mm.
- the tensile strength of the joint portion and the tensile strength other than the joint portion are values measured using a test piece cut out from the hollow molded product having the thickness if the thickness of the hollow molded product is in the range of 1 mm to 5 mm. is there.
- the method of setting the tensile strength of the joint portion where two or more divided bodies are joined by welding to 80% or more with respect to the tensile strength other than the joint portion joined by welding is particularly as long as such a hollow molded article is obtained.
- a welding method selected from infrared welding and infrared welding / vibration welding in which vibration welding is performed after warming a welding portion with infrared rays is preferably used.
- the hollow molded article of the present invention has a ratio of the average spherulite size in the inner part of 700 ⁇ m from the surface of the hollow molded article to the average spherulite size in the part of 200 ⁇ m inside from the surface of the hollow molded article ((the inner part of 700 ⁇ m from the hollow molded article surface).
- the average spherulite size) / is preferably 1 or more and 2 or less.
- the ratio of the average spherulite size in the inner portion of 700 ⁇ m from the surface of the hollow molded product to the average spherulite size in the inner portion of 200 ⁇ m from the surface of the hollow molded product is smaller than 1, hydrogen gas is easily dissolved in the hollow molded product, When filling and releasing high-pressure hydrogen are repeated, defects are likely to occur.
- the ratio of the average spherulite size in the inner part of 700 ⁇ m from the surface of the hollow molded product to the average spherulite size in the inner part of 200 ⁇ m from the surface of the hollow molded product is larger than 2, hydrogen gas permeation or dissolution is likely to occur.
- the average spherulite size in the portion 700 ⁇ m inside from the surface of the hollow molded article is preferably 0.01 ⁇ m or more and 30 ⁇ m or less.
- the average spherulite size inside 200 micrometers from the hollow molded article surface It is preferable that they are 0.01 micrometer or more and 20 micrometers or less.
- the hollow molded article is a portion 700 ⁇ m inside from the surface of the hollow molded article because it can suppress the permeation and dissolution of hydrogen gas and suppress the generation of defect points even when repeated filling and releasing of high-pressure hydrogen.
- the ratio of the average spherulite size to the average spherulite size in the part 200 ⁇ m inside from the surface of the hollow molded product is preferably 1 or more and 1.8 or less, and more preferably 1 or more and 1.6 or less.
- the ratio between the average spherulite size in the portion 700 ⁇ m inside from the surface of the hollow molded product and the average spherulite size in the portion 200 ⁇ m inside from the surface of the hollow molded product can be obtained by the following method.
- An ultra-thin section is cut out from the inside of the hollow molded article 700 ⁇ m, the section is observed with a polarizing microscope or a transmission electron microscope, a photograph of a spherulite is taken, and the diameter of the spherulite is measured with an image analyzer or the like.
- An ultrathin section was created from the value obtained by calculating the number average and a position 200 ⁇ m from the surface of the hollow molded article, and the section was observed with a polarizing microscope or a transmission electron microscope, and a photograph of a spherulite was taken. Thereafter, a value obtained by calculating the number average of the diameters of the spherulites with an image analyzer or the like is obtained.
- the thickness of the hollow molded product in which the ratio of the average spherulite size in the inner portion of 700 ⁇ m from the surface of the hollow molded product of the present invention to the average spherulite size in the inner portion of 200 ⁇ m from the surface of the hollow molded product is 1 or more and 2 or less. However, the range of 1.4 mm to 5 mm is preferred.
- crystallization occurs during the cooling process in the mold, and the crystallization occurs in a state where the temperature changes and reflects the orientation during injection. This is different from the above-described crystallization under the isothermal standing.
- the ratio of the average spherulite size in the portion 700 ⁇ m inside from the surface of the hollow molded product to the average spherulite size in the portion 200 ⁇ m inside from the surface of the hollow molded product is 1 to 2 in order to obtain a hollow molded product,
- the injection speed is v (mm / s)
- the weight of the hollow molded product is w (g)
- the hollow molded product is hollow.
- a preferred example is a method of molding with w / (v / t) of 500 or less.
- the thickness of the hollow molded product means the thickness of the thinnest portion in the hollow molded product.
- the weight of the hollow molded product means the weight of each divided body constituting the hollow molded product.
- V / t is a value obtained by dividing the injection speed by the thickness of the hollow molded article, and when this value is increased, the orientation in the hollow molded article is increased and it becomes a standard for easy formation of crystal nuclei.
- w is the weight of the hollow molded product, and as the weight increases, the heat storage of the hollow molded product increases and the diffusion factor increases.
- the injection speed v (mm / s) is changed in accordance with the size and shape of the hollow molded product, and w / (v / t) is controlled to 500 or less, so that the inner portion of the hollow molded product is 700 ⁇ m inside.
- the ratio between the average spherulite size and the average spherulite size in the portion 200 ⁇ m inside from the surface of the hollow molded article can be 1 or more and 2 or less.
- the hollow molded product of the present invention is preferably divided into 16 parts, and the standard deviation of the average spherulite size in the portion 500 ⁇ m inside from the surface of each divided hollow molded product piece is preferably 6 or less. If the standard deviation of the average spherulite size in the inner part of 500 ⁇ m from the surface of each hollow molded product divided into 16 parts is larger than 6, the permeation amount of hydrogen gas and the dissolution of hydrogen gas in the hollow molded product The amount will vary, and if filling and releasing of high-pressure hydrogen are repeated, defect points are likely to occur.
- the hollow molded product is a portion 500 ⁇ m inside from the surface of each hollow molded product piece obtained by dividing the hollow molded product into 16 parts from the point that the occurrence of defect points can be suppressed even when repeated filling and releasing of higher pressure hydrogen.
- the standard deviation of the average spherulite size in is preferably 4 or less, and more preferably 2 or less.
- the standard deviation ⁇ of the average spherulite size in the inner portion of 500 ⁇ m from the surface of each hollow molded product divided into 16 hollow molded products is 500 ⁇ m from the surface of each hollow molded product divided into 16 hollow molded products. Cut out an ultrathin section from the inside, and observed each section with a polarizing microscope or a transmission electron microscope.
- the method of dividing the hollow molded product into 16 parts is not particularly limited, but it is preferable to divide the hollow molded product pieces so that the weights of the divided pieces are equal. For example, there are a method of dividing into 16 perpendicular to the cylinder direction and a method of dividing into 16 parallel to the cylindrical direction.
- the hollow molded product of the present invention is divided into 16 parts, and the thickness of the hollow molded product in which the standard deviation of the average spherulite size in the portion 500 ⁇ m inside from the surface of each divided hollow molded product piece is 6 or less is not particularly limited. A range of 1 mm to 5 mm is preferable.
- the standard deviation ⁇ when the mold temperature on the surface touching the mold resin is measured at 10 locations is the value obtained by measuring the mold temperature on the surface touching the mold resin at 10 locations with a thermometer (at each location).
- the mold temperature can be calculated by the following equation.
- ⁇ ⁇ V x: Average of mold temperatures at 10 locations x k : Mold temperature at each location (° C.)
- V Dispersion of mold temperature ⁇ : Standard deviation.
- thermometer there are no particular limitations on the location at which the mold temperature on the surface of the mold that touches the resin is measured at 10 locations with a thermometer, but it is preferable that the intervals between the measurement locations be equal.
- the hollow molded article of the present invention is preferably made of a polyamide resin composition.
- the intensity ratio between the Raman band derived from the ⁇ -type crystal and the Raman band derived from the ⁇ -type crystal (“ ⁇ -type crystal / ⁇ -type” in the Raman analysis in the portion 100 ⁇ m inside from the surface of the hollow molded product. It is preferable that it is 2.5 or less.
- the intensity ratio between the Raman band derived from the ⁇ -type crystal and the Raman band derived from the ⁇ -type crystal is an index representing the crystal form of the hollow molded article.
- the intensity ratio ( ⁇ type crystal / ⁇ type crystal) of the Raman band derived from ⁇ type crystal and the Raman band derived from ⁇ type crystal is 2.5 or less.
- the hollow molded article can further suppress the permeation of hydrogen gas and the dissolution of hydrogen into the resin, and can suppress the generation of defects even when repeated filling and releasing of hydrogen at a higher pressure. Further, since the hollow molded product can suppress the generation of defect points even when repeated filling and releasing of hydrogen at higher pressures, the Raman derived from the ⁇ -type crystal in the Raman analysis in the portion 100 ⁇ m inside from the surface of the hollow molded product.
- the intensity ratio ( ⁇ -type crystal / ⁇ -type crystal) between the band and the Raman band derived from the ⁇ -type crystal is more preferably 2 or less, further preferably 1.5 or less, and particularly preferably 1 or less.
- the lower limit of the intensity ratio ( ⁇ -type crystal / ⁇ -type crystal) is not limited, but is usually about 0.01.
- the intensity ratio of the Raman band derived from the ⁇ -type crystal and the Raman band derived from the ⁇ -type crystal can be determined by the following method.
- a test piece is cut out from the inside of the hollow molded article 100 ⁇ m, and measured using a laser Raman spectroscopic analyzer (in Via manufactured by Renishaw Co.) with a laser spot diameter of 1 ⁇ m in the microscopic mode.
- the ratio ( ⁇ -type crystal / ⁇ -type crystal) is obtained from the intensity of the Raman band derived from ⁇ -type crystal observed near 1125 cm ⁇ 1 and the Raman band derived from ⁇ -type crystal observed near 1080 cm ⁇ 1. Is.
- the method of setting the ⁇ -type crystal) to 2.5 or less is not particularly limited as long as such a hollow molded product can be obtained, but when the hollow molded product is molded by injection molding, the injection speed is v (mm).
- the weight of the hollow molded product is w (g) and the thickness of the hollow molded product is t (mm)
- a preferred example is a method of molding with w / (v / t) of 400 or less, More preferably, the molding is performed at 350 or less, and further preferably 300 or less.
- the thickness of the hollow molded product means the thickness of the thinnest portion in the hollow molded product.
- the weight of the hollow molded product means the weight of each divided body constituting the hollow molded product.
- V / t is a value obtained by dividing the injection speed by the thickness of the hollow molded article. When this value is increased, the orientation in the hollow molded article is increased, and it becomes a standard that a ⁇ -type crystal is easily formed.
- w is the weight of the hollow molded article. As the weight increases, the heat storage of the hollow molded article increases, and it becomes a standard that the crystal is easily converted from the ⁇ -type crystal to the thermally stable ⁇ -type crystal.
- the intensity ratio of the Raman band derived from the ⁇ -type crystal and the Raman band derived from the ⁇ -type crystal can be 2.5 or less.
- the polyamide resin composition used when molding the hollow molded article of the present invention is preferably a polyamide resin composition comprising 0 to 50 parts by weight of other components per 100 parts by weight of the polyamide resin.
- a polyamide resin composition obtained by blending a crystal nucleating agent with a polyamide resin is preferable.
- the polyamide resin alone may not contain other components.
- the polyamide resin is a resin composed of a polymer having an amide bond, and is mainly composed of amino acid, lactam or diamine and dicarboxylic acid.
- the raw materials include amino acids such as 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid and paraaminomethylbenzoic acid, lactams such as ⁇ -caprolactam and ⁇ -laurolactam, tetramethylenediamine, penta Methylenediamine, hexamethylenediamine, 2-methylpentamethylenediamine, undecameethylenediamine, dodecamethylenediamine, 2,2,4- / 2,4,4-trimethylhexamethylenediamine, 5-methylnonamethylenediamine, metaxylene Diamine, paraxylylenediamine, 1,3-bis (aminomethyl) cyclohexane, 1,4-bis (aminomethyl) cyclohexane, 1,
- polyamide resins in the present invention include polycaproamide (polyamide 6), polyhexamethylene adipamide (polyamide 66), polypentamethylene adipamide (polyamide 56), polytetramethylene.
- Particularly preferable examples include polyamide 6 resin, polyamide 66 resin, polyamide 610 resin, polyamide 11 resin, polyamide 12 resin, polyamide 6/66 copolymer, polyamide 6/12 copolymer and the like.
- Particularly preferable examples include polyamide 6 resin, polyamide 66 resin, and polyamide 610 resin. Furthermore, it is practically preferable to use these polyamide resins as a mixture.
- polyamide 6 resin (A) and a melting point of 245 ° C. or less by DSC measurement were measured by cooling at a temperature of 250 ° C. to 20 ° C./min in light scattering measurement.
- a polyamide resin composition comprising a polyamide resin (C) having a shorter rise time of invariant Q than the invariant Q of polyamide 6 resin (A), wherein the polyamide 6 resin (A)
- a polyamide resin composition comprising 0.01 to 5 parts by weight of polyamide resin (C) per 100 parts by weight.
- the polyamide 6 resin (A) used in the present invention is a polyamide resin mainly composed of 6-aminocaproic acid and / or ⁇ -caprolactam. Other monomers may be copolymerized as long as the object of the present invention is not impaired.
- “to be used as a main raw material” includes a unit derived from 6-aminocaproic acid or a unit derived from ⁇ -caprolactam in a total of 50 mol% in a total of 100 mol% of monomer units constituting the polyamide resin. Means. More preferably, it contains 70 mol% or more, more preferably 90 mol% or more of 6-aminocaproic acid-derived units or ⁇ -caprolactam-derived units.
- Examples of other monomers to be copolymerized include, for example, amino acids such as 11-aminoundecanoic acid, 12-aminododecanoic acid and paraaminomethylbenzoic acid, lactams such as ⁇ -laurolactam; tetramethylenediamine, pentamethylenediamine, Aliphatic diamines such as hexamethylenediamine, 2-methylpentamethylenediamine, undecamethylenediamine, dodecamethylenediamine, 2,2,4- / 2,4,4-trimethylhexamethylenediamine, 5-methylnonamethylenediamine; Aromatic diamines such as metaxylenediamine and paraxylylenediamine; 1,3-bis (aminomethyl) cyclohexane, 1,4-bis (aminomethyl) cyclohexane, 1-amino-3-aminomethyl-3,5,5 -Trimethylcyclohexane, bis (4- Alicyclic diamines such
- the polyamide resin (C) used in the present invention is an invariant when the melting point by DSC measurement is 245 ° C. or less and the light scattering measurement is performed by cooling from a temperature of 250 ° C. at a rate of 20 ° C./min.
- the rise time of Q is a polyamide resin shorter than the rise time of invariant Q of the polyamide 6 resin (A).
- the melting point by DSC measurement of the polyamide 6 resin (A) and the polyamide resin (C) in the present invention can be determined by the following method. First, using a differential scanning calorimeter (DSC-7 manufactured by Perkin Elmer), two-point calibration (indium, lead) and baseline correction are performed. The sample amount was set to 8 to 10 mg, held at a temperature 15 ° C. higher than the temperature showing the maximum value of the melting curve obtained by heating at a heating rate of 20 ° C./min, and then cooled down at 20 ° C./min. Cool to 30 ° C at speed. Further, after being held at a temperature of 30 ° C. for 1 minute, the second temperature raising step is performed at a rate of 20 ° C./min, similarly to the first temperature raising step. The melting endothermic peak temperature observed in the second temperature raising step is defined as the melting point.
- DSC-7 differential scanning calorimeter
- the rise time of the invariant Q of the polyamide 6 resin (A) and the polyamide resin (C) in the present invention can be obtained by the following method. First, 8 to 10 mg of a sample is sandwiched between cover glasses and subjected to a hot stage “CSS-450W” manufactured by Linkham Co., and kept at a temperature of 250 ° C. for 30 seconds to melt the sample. Thereafter, the temperature is lowered to 180 ° C. at a rate of 20 ° C./min.
- the rise time of invariant Q is measured when the temperature drop start time is 0.
- the rise time of the invariant Q indicates a point in time when the value of the invariant Q at the start of cooling is 0 and the invariant Q starts to increase.
- FIG. 1 shows a graph of measurement results of invariant Q of polyamide 6 resin used in Example 1 described later.
- the horizontal axis represents the elapsed time from the start of temperature decrease, and the vertical axis represents the value of invariant Q.
- FIG. 1B is an enlarged view of FIG. In FIG. 1B, reference numeral 1 represents the rise time of the invariant Q.
- the polyamide resin (C) is not particularly limited as long as the melting point and the rise time of the invariant Q satisfy the above conditions.
- amino acid, lactam or diamine and dicarboxylic acid are obtained as main raw materials. be able to.
- Representative examples of the raw materials include, for example, amino acids such as 6-aminocaproic acid, 11-aminoundecanoic acid, 12-aminododecanoic acid and paraaminomethylbenzoic acid; lactams such as ⁇ -caprolactam and ⁇ -laurolactam; tetramethylenediamine , Pentamethylenediamine, hexamethylenediamine, 2-methylpentamethylenediamine, undecamethylenediamine, dodecamethylenediamine, 2,2,4- / 2,4,4-trimethylhexamethylenediamine, 5-methylnonamethylenediamine, etc.
- Aliphatic diamines such as metaxylenediamine and paraxylylenediamine; 1,3-bis (aminomethyl) cyclohexane, 1,4-bis (aminomethyl) cyclohexane, 1-amino-3-aminomethyl- 3,5,5-tri
- methylcyclohexane bis (4-aminocyclohexyl) methane, bis (3-methyl-4-aminocyclohexyl) methane, 2,2-bis (4-aminocyclohexyl) propane, bis (aminopropyl) piperazine, aminoethylpiperazine, etc.
- Alicyclic diamines such as adipic acid, suberic acid, azelaic acid, sebacic acid, dodecanedioic acid; terephthalic acid, isophthalic acid, 2-chloroterephthalic acid, 2-methylterephthalic acid, 5-methylisophthalic acid
- Aromatic dicarboxylic acids such as 5-sodium sulfoisophthalic acid, hexahydroterephthalic acid, hexahydroisophthalic acid; 1,4-cyclohexanedicarboxylic acid, 1,3-cyclohexanedicarboxylic acid, 1,2-cyclohexanedicarboxylic acid, 1, 3-cyclopen Alicyclic dicarboxylic acids such as Njikarubon acid.
- polyamide homopolymers or copolymers derived from these raw materials can be used. Two or more of these polyamide resins may be blended.
- polyamide 610 resin is more preferable because the average spherulite size becomes finer.
- the degree of polymerization of the polyamide 6 resin (A) and the polyamide resin (C) is not particularly limited, and the relative viscosity measured at 25 ° C. in a 98% concentrated sulfuric acid solution having a sample concentration of 0.01 g / ml is 1.5 to A range of 7.0 is preferred.
- the relative viscosity is 1.5 or more, the melt viscosity of the polyamide resin composition at the time of molding becomes moderately high, the air entrainment at the time of molding can be suppressed, and the moldability can be further improved.
- the relative viscosity is more preferably 1.8 or more.
- the relative viscosity is if the relative viscosity is 7.0 or less, the melt viscosity at the time of molding of the polyamide resin composition becomes moderately low, and the moldability can be further improved.
- the amount of amino terminal groups of the polyamide 6 resin (A) and the polyamide resin (C) is not particularly limited, but is preferably in the range of 1.0 to 10.0 ⁇ 10 ⁇ 5 mol / g.
- the amino terminal group amount is in the range of 1.0 to 10.0 ⁇ 10 ⁇ 5 mol / g, a sufficient degree of polymerization can be obtained, and the mechanical strength of the molded product can be improved.
- the amino terminal group amount of the polyamide resin is determined by dissolving the polyamide resin in a phenol / ethanol mixed solvent (83.5: 16.5 (volume ratio)) and titrating with a 0.02N aqueous hydrochloric acid solution. Can be sought.
- the polyamide resin composition preferably contains a crystal nucleating agent.
- the crystal nucleating agent include inorganic crystal nucleating agents and organic crystal nucleating agents.
- inorganic crystal nucleating agents include talc, kaolinite, montmorillonite, mica, synthetic mica, clay, zeolite, silica, graphite, carbon black, zinc oxide, magnesium oxide, calcium oxide, titanium oxide, calcium sulfide, and nitriding.
- examples thereof include metal salts of boron, magnesium carbonate, calcium carbonate, barium sulfate, aluminum oxide, neodymium oxide, and phenylphosphonate. These may be used alone or in combination of two or more.
- These inorganic crystal nucleating agents are preferably modified with an organic substance in order to improve dispersibility in the resin composition.
- organic crystal nucleating agents include sodium benzoate, potassium benzoate, lithium benzoate, calcium benzoate, magnesium benzoate, barium benzoate, lithium terephthalate, sodium terephthalate, potassium terephthalate, calcium oxalate , Sodium laurate, potassium laurate, sodium myristate, potassium myristate, calcium myristate, sodium octacosanoate, calcium octacosanoate, sodium stearate, potassium stearate, lithium stearate, calcium stearate, magnesium stearate, stearic acid Barium, sodium montanate, calcium montanate, sodium toluate, sodium salicylate, potassium salicylate, zinc salicylate, Luminium dibenzoate, potassium dibenzoate, lithium dibenzoate, organic carboxylic acid metal salts such as sodium ⁇ -naphthalate, sodium cyclohexanecarboxylate, organic sulfonates such as sodium p-
- amide wax examples include an amide compound obtained by reacting a monocarboxylic acid and a diamine, an amide compound obtained by reacting a monoamine and a polybasic acid, an amide compound obtained by reacting a monocarboxylic acid, a polybasic acid and a diamine. Is mentioned. These can be obtained by dehydration reaction of the corresponding amine and carboxylic acid.
- the monoamine is preferably a monoamine having 5 or more carbon atoms, and specific examples thereof include pentylamine, hexylamine, heptylamine, octylamine, nonylamine, decylamine, dodecylamine, stearylamine, cyclohexylamine, and benzylamine. These may be used in combination of two or more. Of these, higher aliphatic monoamines having 10 to 20 carbon atoms are particularly preferred. If the carbon number is greater than 20, the compatibility with the polyamide resin is lowered, and there is a risk of precipitation.
- the monocarboxylic acid is preferably an aliphatic monocarboxylic acid or hydroxycarboxylic acid having 5 or more carbon atoms. Specific examples thereof include valeric acid, caproic acid, caprylic acid, lauric acid, myristic acid, palmitic acid, stearic acid, olein. Examples thereof include acid, linoleic acid, behenic acid, montanic acid, 12-hydroxystearic acid, benzoic acid, and the like. Two or more of these may be used in combination. Of these, higher aliphatic monocarboxylic acids having 10 to 30 carbon atoms are particularly preferred. If the number of carbon atoms is greater than 30, the compatibility with the polyamide 6 resin is lowered and there is a risk of precipitation.
- diamine examples include ethylenediamine, 1,3-diaminopropane, 1,4-diaminopropane, tetramethylenediamine, hexamethylenediamine, nonamethylenediamine, undecamethylenediamine, dodecamethylenediamine, metaxylylenediamine, Paraxylylenediamine, tolylenediamine, phenylenediamine, isophoronediamine and the like may be mentioned, and two or more of these may be used in combination. Of these, ethylenediamine is particularly preferred.
- the polybasic acid is a dicarboxylic acid or higher carboxylic acid, and specific examples thereof include aliphatic dicarboxylic acids such as malonic acid, succinic acid, adipic acid, sebacic acid, pimelic acid, azelaic acid, phthalic acid, terephthalic acid, and the like. Examples thereof include aromatic dicarboxylic acids such as acid and isophthalic acid, and alicyclic dicarboxylic acids such as cyclohexanedicarboxylic acid and cyclohexylsuccinic acid. These may be used in combination of two or more.
- an amide compound obtained by reacting a higher aliphatic monocarboxylic acid, a polybasic acid and a diamine is particularly suitable.
- an amide compound obtained by reacting stearic acid, sebacic acid and ethylenediamine is preferred.
- the mixing ratio of each component is preferably in the range of 0.18 to 1.0 mol of polybasic acid and 1.0 to 2.2 mol of diamine with respect to 2 mol of higher aliphatic monocarboxylic acid.
- the range of 0.5 mol to 1.0 mol of polybasic acid and 1.5 mol to 2.0 mol of diamine is more preferable with respect to 2 mol of higher aliphatic monocarboxylic acid.
- the compounding amount of the crystal nucleating agent in the polyamide resin composition forming the hollow molded article of the present invention is preferably 0.01 to 10 parts by weight with respect to 100 parts by weight of the polyamide resin. Even when an amide wax is used as the crystal nucleating agent, it is preferable to blend 0.01 to 10 parts by weight of the amide wax with 100 parts by weight of the polyamide resin.
- thermoplastic resins other than polyamide resins examples include thermoplastic resins other than polyamide resins, various additives, impact resistant materials, fillers, and the like.
- thermoplastic resins other than the polyamide resin in the present invention include, for example, polyester resins, polyphenylene sulfide resins, polyphenylene oxide resins, polycarbonate resins, polylactic acid resins, polyacetal resins, polysulfone resins, tetrafluoropolyethylene resins, and polyetherimide resins.
- various additives include, for example, colorants, antioxidants such as hindered phenols and hindered amines, mold release agents such as ethylenebisstearylamide and higher fatty acid esters, copper compounds, plasticizers, and heat stabilizers. , Lubricants, UV inhibitors, colorants, flame retardants, foaming agents, and the like.
- Examples of the impact resistant material in the present invention include olefin resins, acrylic rubbers, silicone rubbers, fluorine rubbers, styrene rubbers, nitrile rubbers, vinyl rubbers, urethane rubbers, polyamide elastomers, polyester elastomers, ionomers. Etc. Two or more of these may be blended.
- olefin resins are preferably used because of their excellent impact resistance.
- the olefin resin is a thermoplastic resin obtained by polymerizing olefin monomers such as ethylene, propylene, butene, isoprene, and pentene.
- the copolymer of 2 or more types of olefin monomers may be sufficient, and the copolymer of these olefin monomers and another monomer may be sufficient.
- the olefin resin include polymers such as polyethylene, polypropylene, polystyrene, poly 1-butene, poly 1-pentene, and polymethyl pentene or copolymers thereof; ethylene / ⁇ -olefin copolymer, ethylene / ⁇ , ⁇ -unsaturated carboxylic acid ester copolymer, ⁇ -olefin / ⁇ , ⁇ -unsaturated carboxylic acid ester copolymer, [copolymer of (ethylene and / or propylene) and vinyl alcohol ester] Polyolefin obtained by partially hydrolyzing, a copolymer of (ethylene and / or propylene) and (unsaturated carboxylic acid and / or unsaturated carboxylic ester), [(ethylene and / or propylene) and (unsaturated) Copolymer of saturated carboxylic acid and / or unsaturated carboxylic acid ester) Polyolefins obtained by at least a portion
- an ethylene / ⁇ -olefin copolymer and an ethylene / ⁇ , ⁇ -unsaturated carboxylic acid ester copolymer are more preferable, and an ethylene / ⁇ -olefin copolymer is more preferable.
- the polyolefin resin may be modified with an unsaturated carboxylic acid and / or a derivative thereof.
- the derivative of unsaturated carboxylic acid is a compound obtained by substituting the hydroxy group portion of the carboxyl group of unsaturated carboxylic acid with another substituent, and includes a metal salt, an acid halide, an ester, an acid of unsaturated carboxylic acid. Anhydrides, amides and imides.
- Examples of the unsaturated carboxylic acid or derivative thereof include acrylic acid, methacrylic acid, maleic acid, fumaric acid, itaconic acid, crotonic acid, methylmaleic acid, methyl fumaric acid, mesaconic acid, citraconic acid, glutaconic acid and carboxylic acids thereof.
- the filler may be a fibrous filler or a non-fibrous filler, or a combination of a fibrous filler and a non-fibrous filler.
- the fibrous filler include glass fiber, glass milled fiber, carbon fiber, potassium titanate whisker, zinc oxide whisker, aluminum borate whisker, aramid fiber, alumina fiber, silicon carbide fiber, ceramic fiber, asbestos fiber, and stone powder. Examples thereof include fibers and metal fibers.
- Non-fibrous fillers include, for example, silicates such as wollastonite, zeolite, sericite, kaolin, mica, clay, pyrophyllite, bentonite, asbestos, talc, alumina silicate; alumina, silicon oxide, magnesium oxide, oxidation Metal oxides such as zirconium, titanium oxide and iron oxide; metal carbonates such as calcium carbonate, magnesium carbonate and dolomite; metal sulfates such as calcium sulfate and barium sulfate; magnesium hydroxide, calcium hydroxide and aluminum hydroxide Metal hydroxide; glass beads, ceramic beads, boron nitride, silicon carbide and the like. These may be hollow.
- silicates such as wollastonite, zeolite, sericite, kaolin, mica, clay, pyrophyllite, bentonite, asbestos, talc, alumina silicate
- alumina silicon oxide, magnesium oxide, oxidation Metal oxides such as zircon
- these fibrous and / or non-fibrous fillers after pretreatment with a coupling agent in terms of obtaining superior mechanical properties.
- the coupling agent include isocyanate compounds, organic silane compounds, organic titanate compounds, organic borane compounds, and epoxy compounds.
- Examples of the method of molding two or more divided bodies constituting the hollow molded article of the present invention include extrusion molding, injection molding, and compression molding. Of these, extrusion molding and injection molding are preferred.
- a hollow molded article can be obtained by joining two or more divided bodies constituting the obtained hollow molded article by welding. For example, in the case of forming a cylindrical hollow molded product, the hollow molded product is joined by welding two molded products having a shape obtained by dividing the hollow molded product in half in a direction perpendicular to the height of the cylinder.
- Forming method method of forming a hollow molded product by welding two molded products having a shape that is divided in half in the horizontal direction with respect to the height of the cylinder, both ends of the hollow molded product
- a method of forming a hollow molded product by joining two end plates having a semicircular shape, an elliptical shape, and the like and a cylindrical body portion by welding is included, but is not limited thereto. It is not a thing.
- Examples of the welding include hot plate welding, infrared welding, and infrared / vibration welding in which vibration welding is performed after warming the welded portion with infrared rays. Of these, infrared welding and infrared / vibration welding are preferable. On the other hand, ultrasonic welding is unsuitable for hollow molded products of the size of business cards or larger. Laser welding, vibration welding, and spin welding result in insufficient weld strength, and repeated high-pressure hydrogen filling and releasing pressure. And cracks are likely to occur at the welded part.
- the hollow molded article of the present invention is used for a hollow molded article that comes into contact with high-pressure hydrogen having a welded portion, taking advantage of the excellent feature that the occurrence of cracks at the welded portion is suppressed even when charging and releasing of high-pressure hydrogen are repeated. It is done.
- the hollow molded product that comes into contact with high-pressure hydrogen having a welded portion here is a hollow molded product that has a welded portion that comes into contact with hydrogen at a pressure equal to or higher than normal pressure.
- it Since it exerts an effect of suppressing the occurrence of cracks in the welded portion when repeated filling and releasing of high-pressure hydrogen, it is preferably used for hollow molded article applications having a welded portion that comes into contact with hydrogen at a pressure of 20 MPa or higher, and has a pressure of 30 MPa or higher. It is preferably used depending on the use of a hollow molded article having a welded portion that comes into contact with hydrogen. As for the upper limit of the working pressure, it is preferably used for hollow molded product applications having a welded part that comes into contact with hydrogen at a pressure of 200 MPa or less, and is preferably used for hollow molded product applications that have a welded part that comes into contact with hydrogen at 150 MPa or less.
- the hollow molded article having a welded portion that touches the surface is more preferably used for a hollow molded product having a welded portion that touches the surface.
- the hollow molded article having a welded portion that comes into contact with high-pressure hydrogen include a high-pressure hydrogen tank and a high-pressure hydrogen tank liner. Especially, it can use preferably for the tank liner for high pressure hydrogen.
- a particularly preferable embodiment is an embodiment in which a hollow molded article that comes into contact with high-pressure hydrogen having a welded portion according to the present invention is used as a resin liner for a tank for high-pressure hydrogen formed by reinforcing the outside of a resin liner with carbon fiber reinforced resin.
- the hollow molded article of the present invention can be used as a high-pressure hydrogen tank in which a carbon fiber reinforced resin (CFRP) reinforcing layer is laminated on the surface layer of the hollow molded article.
- CFRP carbon fiber reinforced resin
- CFRP reinforcing layer is laminated on the surface layer of the tank liner because strength and elastic modulus that can withstand high pressure can be expressed.
- the CFRP reinforcing layer is composed of carbon fibers and a matrix resin.
- the carbon fiber preferably has a tensile elastic modulus of 50 to 700 GPa from the viewpoint of bending properties and strength, and more preferably 200 to 700 GPa in view of the specific rigidity, which is more cost effective. Considering the viewpoint, the one of 200 to 450 GPa is most preferable.
- the tensile strength of the carbon fiber alone is preferably 1500 to 7000 MPa, and preferably 3000 to 7000 MPa from the viewpoint of specific strength.
- the density of the carbon fiber is preferably 1.60 to 3.00, more preferably 1.70 to 2.00 from the viewpoint of weight reduction, and most preferably 1.70 to 1.90 from the viewpoint of cost performance.
- the fiber diameter of the carbon fiber is preferably 5 to 30 ⁇ m, more preferably 5 to 20 ⁇ m from the viewpoint of handleability, and most preferably 5 to 10 ⁇ m from the viewpoint of weight reduction.
- Carbon fibers may be used alone or in combination with reinforcing fibers other than carbon fibers. Examples of reinforcing fibers other than carbon fibers include glass fibers and aramid fibers.
- Vf is preferably 20 to 80% from the viewpoint of rigidity, and from the viewpoint of productivity and required rigidity. To Vf is preferably 40 to 80%.
- the matrix resin constituting the CFRP reinforcing layer may be a thermosetting resin or a thermoplastic resin.
- the matrix resin is a thermosetting resin
- examples of the main material include an epoxy resin, an unsaturated polyester resin, a vinyl ester resin, a phenol resin, a polyurethane resin, and a silicone resin. Only one of these may be used, or two or more may be mixed and used. Epoxy resins are particularly preferred. Examples of the epoxy resin include bisphenol A type epoxy resin, bisphenol F type epoxy resin, bisphenol S type epoxy resin, phenol novolac type epoxy resin, isocyanate modified bisphenol A type epoxy resin and the like. When a thermosetting resin is employed for the matrix resin, it is possible to add an appropriate curing agent or reaction accelerator to the thermosetting resin component.
- the matrix resin is a thermoplastic resin
- the main materials are polyethylene resin, polypropylene resin, polyvinyl chloride resin, ABS resin, polystyrene resin, AS resin, polyamide resin, polyacetal resin, polycarbonate resin, thermoplastic polyester resin, PPS resin Fluorine resin, polyetherimide resin, polyetherketone resin, polyimide resin and the like.
- thermoplastic resins may be used alone, as a mixture of two or more kinds, or as a copolymer. In the case of a mixture, a compatibilizer may be used in combination.
- brominated flame retardants, silicon-based flame retardants, red phosphorus, and the like may be added as flame retardants.
- FW filament winding
- TW tape winding
- SW sheet winding
- RTM hand layup method
- RTM Resin Transfer Molding
- FW method, SW method and TW method are basically the same molding method from the viewpoint of applying a matrix resin to a strand-like carbon fiber and laminating it on the liner.
- the name is different depending on whether it is wound in a filament (thread) form, a tape (tape form in which yarns are bundled to some extent) form, or a sheet (sheet form in which tapes are bundled to some extent).
- a filament thread
- tape tape form in which yarns are bundled to some extent
- sheet sheet form in which tapes are bundled to some extent
- the matrix resin is a thermosetting resin
- after wrapping carbon fiber and uncured matrix resin around the liner it is necessary to perform resin curing treatment under conditions suitable for the resin used in a batch furnace (oven) or continuous curing furnace in order to cure the resin. There is.
- the matrix resin is a thermoplastic resin
- the fiber orientation design of carbon fibers When obtaining the high-pressure hydrogen tank of the present invention by the FW method, TW method, SW method, etc., the most important thing is the fiber orientation design of carbon fibers.
- a carbon fiber strand continuous fiber
- a prepreg in which a carbon fiber strand is impregnated with a resin is wound around a liner and molded.
- the high-pressure hydrogen tank a tank liner in which a valve is fixed by insert molding or an O-ring is preferable. It is preferable to fix the valve by insert molding or O-ring because the airtightness of high-pressure hydrogen is increased.
- the valve functions as a high-pressure hydrogen filling port and a discharge port.
- the material of the metal part used as the valve include carbon steel, manganese steel, chrome molybdenum steel, stainless steel, and aluminum alloy.
- Examples of carbon steel include carbon steel pipe for pressure piping, carbon steel pipe for high pressure piping, steel pipe for low temperature piping, and carbon steel for machine structure.
- Examples of manganese steel include seamless steel pipes for high-pressure gas containers, manganese steel materials for machine structures, and manganese chromium steel materials.
- Examples of chrome molybdenum steel and low alloy steel include seamless steel pipes for high-pressure gas containers, alloy steel pipes for machine structures, nickel chrome molybdenum steel materials, and chrome molybdenum steel materials.
- Examples of stainless steel include stainless steel forgings for pressure, stainless steel pipes for piping, stainless steel bars, hot rolled stainless steel plates and steel strips, cold rolled stainless steel plates and steel strips.
- Examples of the aluminum alloy include aluminum and aluminum alloy plates, strips, bars, wires, seamless pipes, and forged products.
- annealing normalizing, for manganese steel, normalizing, quenching and tempering, for chromium molybdenum steel and low alloy steel, quenching and tempering, stainless steel
- a material subjected to hardening and tempering may be applied to the aluminum alloy.
- a solution subjected to solution treatment and T6 aging treatment may be applied.
- the most preferred embodiment of the high-pressure hydrogen tank of the present invention is such that a CFRP reinforcing layer is laminated on the surface layer of the tank liner made of the polyamide resin composition of the present invention, and the valve is inserted into the tank liner by insert molding or O-ring. This is a high-pressure hydrogen tank that is fixed.
- Tensile strength retention ratio of welded portion (tensile strength of test piece including a portion joined by welding) / (tensile strength of test piece not including a portion joined by welding) ⁇ 100 (4) Average spherulite size (average spherulite size) at the inner part of 500 ⁇ m from the surface of the hollow molded product From the 500 ⁇ m inner part of the surface of the hollow molded article obtained in each Example and Comparative Example, an ultrathin section was cut out using an ultramicrotome, and a photograph of a spherulite was taken with a polarizing optical microscope for the ultrathin section, From the photograph, the diameter of 50 or more spherulites was measured using an image analyzer, and the average spherulite size was calculated as the number average value.
- Ratio of (inner layer) average spherulite size in the inner portion of 700 ⁇ m from the surface of the hollow molded product / (outer layer) average spherulite size in the inner portion of 200 ⁇ m from the surface of the hollow molded product (ratio of the inner layer / outer layer of the hollow molded product)
- An ultrathin section was cut out from the inner part of 700 ⁇ m on the surface of the hollow molded article obtained in Examples 10 to 21 and Comparative Examples 6 and 7, using an ultramicrotome. A photograph was taken, the diameter of 50 or more spherulites was measured from the photograph using an image analyzer, and the average spherulite size was calculated as the number average value.
- a standard deviation ⁇ was calculated from the average spherulite size x of each obtained hollow molded product piece by the following formula.
- Formula 3) ⁇ ⁇ V x: average of 16 average spherulite sizes
- x k average spherulite size ( ⁇ m) at each location
- V dispersion of average spherulite size ⁇ : standard deviation.
- the intensity ratio of the Raman band derived from the ⁇ -type crystal observed near 1125 cm ⁇ 1 and the intensity of the Raman band derived from the ⁇ -type crystal observed near 1080 cm ⁇ 1 was measured with a laser spot diameter of 1 ⁇ m. ( ⁇ -type crystal / ⁇ -type crystal) was calculated. Detailed conditions are shown below.
- Laser power 50mW Diffraction grating; Single 3000gr / mm Slit; 65 ⁇ m Detector: CCD / RENISHA 1024 ⁇ 256.
- PA6 / PA66 copolymer Polyamide 6 / polyamide 66 copolymer (melting point 190 ° C., crystallization temperature drop: 122 ° C., relative viscosity 4.20 at 25 ° C. in a 98% concentrated sulfuric acid solution having a resin concentration of 0.01 g / ml.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellet, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., injection speed 60 mm / second, cooling time 150 seconds, holding pressure 20 MPa, holding pressure 10 seconds, mold 30 ° C.
- a cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under the condition that the mold surface was cooled to cool the mold surface and the resin was shaped and heated for 10 seconds after flowing a heating medium at 80 ° C. .
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under molding conditions of seconds. Using two obtained cylindrical molded products, the plane portions were arranged so as to be parallel, and the plane portions were heated with infrared rays for 60 seconds, and then vibrated so that the amount of penetration was 2 mm. Vibration welding) was performed to obtain a hollow molded product having a welded portion. Tables 1 and 2 show the results of evaluation by the above-described method using the obtained hollow molded article.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under molding conditions of seconds. Using two obtained cylindrical molded products, the plane part is arranged so as to be parallel, the plane part is heated with infrared rays for 90 seconds, and then pressurized so that the amount of penetration is 2 mm. ) To obtain a hollow molded article having a welded portion. Table 1 shows the results of evaluation by the above-described method using the obtained hollow molded article.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under molding conditions of seconds.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under molding conditions of seconds. Using two obtained cylindrical molded products, the plane portions are arranged in parallel, and are welded (vibration welding) by vibrating so that the amount of penetration is 2 mm. A hollow molded product having a welded portion is obtained. Obtained. The results of evaluation by the above-described method using the obtained hollow molded article are shown in Table 2.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection-molded under molding conditions of seconds.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., mold temperature: 80 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 Under a molding condition of seconds, a cylindrical molded product on the laser beam transmitting side having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection molded.
- the hollow molded article having the welded portion having an average spherulite size of 20 ⁇ m or less within 500 ⁇ m from the surface of the hollow molded article, and the location where two or more divided bodies are joined by welding
- a hollow molded product for the first time capable of suppressing the occurrence of cracks in the welded portion even when repeated filling and releasing of high-pressure hydrogen by setting the tensile strength to 80% or more of the tensile strength other than the part joined by welding.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying.
- a vacuum dryer For the purpose of confirming the weight of the hollow molded product from the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., cooling time 150 seconds, holding pressure 20 MPa, holding pressure time 10 seconds, A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection molded under molding conditions of a mold temperature of 80 ° C. and an injection speed of 30 mm / second, and the weight of the obtained cylindrical molded product was measured.
- a cylinder temperature 250 ° C.
- cooling time 150 seconds, maintained using an injection molding machine with a clamping force of 1000 t. Pressure of 20 MPa, holding time of 10 seconds, mold was cooled by flowing a 30 ° C. coolant to cool the mold surface, and after 10 seconds of shaping the resin, 80 ° C.
- injection speed v (mm / S) is a molding condition in which the measured weight w (g) and thickness t (mm) to w / (v / t) of the cylindrical molded product is 500 or less, and the diameter is 500 mm, the height is 400 mm, A cylindrical molded product having a thickness of 3 mm was injection molded.
- the plane portions were arranged so as to be parallel, and the plane portions were heated with infrared rays for 60 seconds, and then vibrated so that the amount of penetration was 2 mm. Vibration welding) was performed to obtain a hollow molded product having a welded portion.
- Table 3 The results of evaluation by the above-described method using the obtained hollow molded article are shown in Table 3.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying.
- a vacuum dryer For the purpose of confirming the weight of the hollow molded product from the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., cooling time 150 seconds, holding pressure 20 MPa, holding pressure time 10 seconds, A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection molded under molding conditions of a mold temperature of 80 ° C. and an injection speed of 30 mm / second, and the weight of the obtained cylindrical molded product was measured.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying.
- a vacuum dryer For the purpose of confirming the weight of the hollow molded product from the obtained pellets, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., cooling time 150 seconds, holding pressure 20 MPa, holding pressure time 10 seconds, A cylindrical molded product having a diameter of 500 mm, a height of 400 mm, and a thickness of 3 mm was injection molded under molding conditions of a mold temperature of 80 ° C. and an injection speed of 30 mm / second, and the weight of the obtained cylindrical molded product was measured.
- the hollow molded article having the welded portion having an average spherulite size of 20 ⁇ m or less within 500 ⁇ m from the surface of the hollow molded article, and the location where two or more divided bodies are joined by welding
- a hollow molded product for the first time capable of suppressing the occurrence of cracks in the welded portion even when repeated filling and releasing of high-pressure hydrogen by setting the tensile strength to 80% or more of the tensile strength other than the part joined by welding.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellet, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 seconds, The mold temperature was set to 80 ° C using two mold temperature controllers, and the molding conditions were such that the standard deviation when the mold temperature on the surface touching the resin was measured at 10 locations was controlled to 5.2, and the diameter was 500 mm and the height was 400 mm. A cylindrical molded product having a thickness of 3 mm was injection molded.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C.
- the gut discharged from the die at a rate of 20 kg / h was rapidly cooled by passing through a cooling bath filled with water adjusted to 10 ° C. over 10 seconds, and then pelletized with a strand cutter to obtain pellets. .
- the obtained pellets were vacuum-dried with a vacuum dryer at a temperature of 80 ° C. for 12 hours to obtain pellets after drying. From the obtained pellet, using an injection molding machine with a clamping force of 1000 t, cylinder temperature: 250 ° C., injection speed 60 mm / second, holding pressure 20 MPa, holding pressure 10 seconds, cooling time 150 seconds, Using a mold temperature controller, the temperature was set to 80 ° C, and the molding conditions were controlled so that the standard deviation was 11.2 when the mold temperature on the surface touching the resin was measured at 11.2. The diameter was 500 mm and the height was 400 mm. A cylindrical molded product having a thickness of 3 mm was injection molded.
- the hollow molded article having the welded portion having an average spherulite size of 20 ⁇ m or less within 500 ⁇ m from the surface of the hollow molded article, and the location where two or more divided bodies are joined by welding
- a hollow molded product for the first time capable of suppressing the occurrence of cracks in the welded portion even when repeated filling and releasing of high-pressure hydrogen by setting the tensile strength to 80% or more of the tensile strength other than the part joined by welding.
- the hollow molded article of the present invention is extremely useful as a hollow molded article that comes into contact with high-pressure hydrogen having a welded part because cracks can be suppressed at the welded part even when high-pressure hydrogen is repeatedly charged and released.
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Abstract
Description
(式1) G∝βexp(-K/T(ΔT)f)
β:拡散因子
K:結晶核形成因子
ΔT:過冷却度(融点-結晶化温度)
f:補正定数
つまり結晶化温度が高い場合、結晶核形成因子は低下し、温度と共に増加する拡散因子が高くなるため一つの結晶核からの成長が進行する。その結果、球晶サイズは大きくなる。逆に結晶化温度が低い場合、結晶核形成因子が高まり、かつ拡散因子が低下するため一つの結晶核からの成長が抑制される。その結果、球晶サイズは小さくなる。
式1)x =(1/16)Σxk (k=1~16)
式2)V =(1/16)Σ(xk-x)2 (k=1~16)
式3)σ =√V
x:16箇所の平均球晶サイズの平均
xk:各箇所での平均球晶サイズ(μm)
V:平均球晶サイズの分散
σ:標準偏差。
式1)x =(1/10)Σxk (k=1~10)
式2)V =(1/10)Σ(xk-x)2(k=1~10)
式3)σ =√V
x:10箇所の金型温度の平均
xk:各箇所での金型温度(℃)
V:金型温度の分散
σ:標準偏差。
各実施例および比較例により得られた中空成形品について、X線CT解析を行い、溶着部の亀裂の有無を観察した。亀裂のない中空成形品をオートクレーブに入れた後、オートクレーブ中に水素ガスを圧力30MPaまで3分間かけて注入し、2時間保持した後、1分間かけて常圧になるまで減圧した。これを1サイクルとして700サイクル繰り返した。700サイクル繰り返し後の中空成形品について、X線CT解析を行い、溶着部の1mm以上の亀裂の有無を観察した。
実施例10~32および比較例6~9により得られた中空成形品について、X線CT解析を行い、欠陥点の有無を観察した。亀裂のない中空成形品をオートクレーブに入れた後、オートクレーブ中に水素ガスを圧力30MPaまで3分間かけて注入し、2時間保持した後、1分間かけて常圧になるまで減圧した。これを1サイクルとして700サイクル繰り返した。700サイクル繰り返し後の中空成形品について、X線CT解析を行い、10μm以上の欠陥点の有無を観察した。
各実施例および比較例により得られた中空成形品(厚み3mm)から、高さ100mm、幅10mmで、溶着により接合した箇所が高さ方向の中心に、高さ方向に垂直となるよう切り出した試験片と、溶着により接合した箇所を含まず、かつ溶着により接合した箇所を含む試験片と同一方向に引張試験を実施できるように切り出した試験片各5本について、温度23℃、湿度50%の条件で30分間調湿後、10mm/分の速度で引張試験を実施し、引張強度を評価した。各5本測定した平均の値を引張強度とし、得られた引張強度結果から溶着部引張強度保持率を算出した。
溶着部引張強度保持率=(溶着により接合した箇所を含む試験片の引張強度)/(溶着により接合した箇所を含まない試験片の引張強度)×100
(4)中空成形品表面から500μm内側の部分における平均球晶サイズ(平均球晶サイズ)
各実施例および比較例により得られた中空成形品表面の500μm内側の部分から、ウルトラミクロトームを用いて超薄切片を切り出し、その超薄切片について、偏光光学顕微鏡で球晶の写真を撮影し、その写真から画像解析装置を用い、50個以上の球晶の直径を測定し、その数平均値として平均球晶サイズを算出した。
実施例10~21および比較例6、7により得られた中空成形品表面の700μm内側の部分から、ウルトラミクロトームを用いて超薄切片を切り出し、その超薄切片について、偏光光学顕微鏡で球晶の写真を撮影し、その写真から画像解析装置を用い、50個以上の球晶の直径を測定し、その数平均値として平均球晶サイズを算出した。各実施例および比較例により得られた中空成形品表面の200μm内側の部分から、ウルトラミクロトームを用いて超薄切片を切り出し、その超薄切片について、偏光光学顕微鏡で球晶の写真を撮影し、その写真から画像解析装置を用い、50個以上の球晶の直径を測定し、その数平均値として平均球晶サイズを算出した。算出した中空成形品表面の700μm内側の部分の平均球晶サイズと中空成形品表面から200μm内側の部分の平均球晶サイズから比を算出した。
実施例22~32および比較例8、9により得られた中空成形品を円筒の高さ方向に平行に、円筒断面の円を16等分するように切断することで16分割し、得られた各中空成形品片の各表面の500μm内側の部分から、ウルトラミクロトームを用いて超薄切片を切り出し、その各超薄切片について、偏光光学顕微鏡で各球晶の写真を撮影し、その写真から画像解析装置を用い、各球晶の直径の数平均値として各箇所での平均球晶サイズを算出した。得られた各中空成形品片の平均球晶サイズxから、下記式により標準偏差σを算出した。
式1)x =(1/16)Σxk (k=1~16)
式2)V =(1/16)Σ(xk-x)2 (k=1~16)
式3)σ =√V
x:16箇所の平均球晶サイズの平均
xk:各箇所での平均球晶サイズ(μm)
V:平均球晶サイズの分散
σ:標準偏差。
実施例10~21および比較例6、7により得られた中空成形品表面から100μm内側の部分から試験片を切り出し、レーザーラマン分光分析装置(レニショー社製in Via)を用い、顕微モードで試料位置におけるレーザーのスポット径を1μmとして測定し、1125cm-1付近に認められるα型結晶に由来するラマンバンドの強度と、1080cm-1付近に認められるγ型結晶に由来するラマンバンドの強度から強度比(α型結晶/γ型結晶)を算出した。詳細条件を以下に示す。
装置:レニショー社製in Via
条件:測定モード;顕微ラマン
対物レンズ;×100
ビーム径;1μm
光源;YAG2nd532nm
レーザーパワー;50mW
回折格子;Single 3000gr/mm
スリット;65μm
検出器;CCD/RENISHAW 1024×256 。
各実施例および比較例において配合したポリアミド6樹脂(A)およびポリアミド樹脂(C)について、示差走査熱量計(パーキンエルマー社製DSC-7)を用い、2点校正(インジウム、鉛)、ベースライン補正を行った後、サンプル量を8~10mgとして、昇温速度20℃/分の条件で昇温して得られる融解曲線の最大値を示す温度より15℃高い温度で1分間保持した後、降温速度20℃/分の条件で30℃まで冷却した。さらに、30℃で1分間保持した後、20℃/分の速度で2回目の昇温工程を行った。この2回目の昇温工程において、観測された融解吸熱ピーク温度を融点とした。
各実施例および比較例において配合したポリアミド6樹脂(A)およびポリアミド樹脂(C)について、8~10mgをカバーガラスに挟み、リンカム社製ホットステージ「CSS-450W」に供し、温度250℃で30秒保持し、サンプルを溶融させた。その後、20℃/分の速度で、180℃まで降温させた。その際、大塚電子株式会社製高分子フィルムダイナミックス解析装置「DYNA-3000」を使用し、モード:1次元スキャン(1×512)、X方向:中央部4素子分を積算し1データとしてカウント、NDフィルター:5%、測定間隔:1秒、露光時間:500ミリ秒、ゴニオ角度:20度の条件で、降温開始時点を0とした時の、インバリアントQの立ち上がり時間を計測した。
(A)ポリアミド6樹脂
PA6:ポリアミド6樹脂(融点223℃、樹脂濃度0.01g/mlの98%濃硫酸溶液中25℃における相対粘度2.70、インバリアントQの立ち上がり時間175秒)
(C)ポリアミド樹脂
PA610:ポリアミド610樹脂(融点226℃、樹脂濃度0.01g/mlの98%濃硫酸溶液中25℃における相対粘度3.50、インバリアントQの立ち上がり時間165秒)
PA6/PA66共重合体:ポリアミド6/ポリアミド66共重合体(融点190℃、降温結晶化温度:122℃、樹脂濃度0.01g/mlの98%濃硫酸溶液中25℃における相対粘度4.20)
(B)アミド系ワックス
アミド系ワックス:エチレンジアミン・ステアリン酸・セバシン酸重縮合物「“ライトアマイド ”WH-255」(共栄社化学(株)製、融点255℃)
無機核剤:マイクロタルク「“NanoAce”(登録商標)D-600」(日本タルク(株)製、メジアン径(D50)0.5μm)
耐衝撃材1:無水マレイン酸変性エチレン/1-ブテン共重合体「“タフマー”(登録商標)MH7020」(三井化学(株)製)。
耐衝撃材2:無水マレイン酸変性エチレン/1-ブテン共重合体「“タフマー”(登録商標)MH5040」(三井化学(株)製)。
表1記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、射出速度60mm/秒、冷却時間150秒、保圧20MPa、保圧時間10秒、金型は30℃の冷媒を流して型表面を冷却し、樹脂を賦形した10秒後に80℃の熱媒を流して加熱する条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表1に記載した。
表1および表2記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表1および表2に記載した。
表1記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を90秒間赤外線にて加熱した後、溶け込み量が2mmになるよう加圧して溶着(赤外線溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表1に記載した。
表1記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、熱板温度280℃の熱板で平面部を加熱した後、溶け込み量が2mmになるよう加圧して溶着(熱板溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表1に記載した。
表2記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、溶け込み量が2mmになるよう振動させて溶着(振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表2に記載した。
表2記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、溶け込み量が2mmになるよう回転させて溶着(スピン溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表2に記載した。
表2記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmのレーザー光線透過側の円筒状成形品を射出成形した。また、得られたペレット100重量部に、カーボンブラックを0.4重量部配合した材料を用いて、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、金型温度:80℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒の成形条件で、直径500mm、高さ400mm、厚み3mmのレーザー光線吸収側の円筒状成形品を射出成形した。得られたレーザー光線透過側の円筒状成形品、レーザー光線吸収側の円筒状成形品、各1個用いて、平面部を平行になる様に配置し、溶け込み量が2mmになるようレーザー光線を照射して溶着(レーザー溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表2に記載した。
表3に記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、中空成形品の重量を確認する目的で、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、冷却時間150秒、保圧20MPa、保圧時間10秒、金型温度:80℃、射出速度30mm/秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形し、得られた円筒状成形品の重量を測定した。
表3および表4記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、中空成形品の重量を確認する目的で、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、冷却時間150秒、保圧20MPa、保圧時間10秒、金型温度:80℃、射出速度30mm/秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形し、得られた円筒状成形品の重量を測定した。
表3記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、中空成形品の重量を確認する目的で、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、冷却時間150秒、保圧20MPa、保圧時間10秒、金型温度:80℃、射出速度30mm/秒の成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形し、得られた円筒状成形品の重量を測定した。
表5に記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、射出速度60mm/秒、冷却時間150秒、保圧20MPa、保圧時間10秒、金型は、金型温調機を2台用いて30℃に設定し、樹脂に触れる表面の金型温度を10箇所測定した際の標準偏差が6.4に制御され、かつ樹脂を賦形した10秒後に80℃の熱媒を流して加熱する条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表5に記載した。
表5および表6記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒、金型は、金型温調機を2台用いて80℃に設定し、樹脂に触れる表面の金型温度を10箇所測定した際の標準偏差が5.2に制御された成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表5および表6に記載した。
表5に記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒、金型は、金型温調機を4台用いて80℃に設定し、樹脂に触れる表面の金型温度を10箇所測定した際の標準偏差が3.3に制御された成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表5に記載した。
表5記載の各原料を、シリンダー温度を240℃に設定し、ニーディングゾーンを1つ設けたスクリューアレンジとし、スクリュー回転数を150rpmとした2軸スクリュー押出機(JSW社製TEX30α-35BW-7V)(L/D=45(なお、ここでのLは原料供給口から吐出口までの長さであり、Dはスクリューの直径である。))に供給して溶融混練した。20kg/hの速度でダイから吐出されたガットを、10℃に温調した水を満たした冷却バス中を10秒間かけて通過させることにより急冷した後、ストランドカッターでペレタイズし、ペレットを得た。得られたペレットを、真空乾燥機で、温度80℃、12時間真空乾燥し、乾燥後ペレットを得た。得られたペレットから、型締め力1000tの射出成形機を用いて、シリンダー温度:250℃、射出速度60mm/秒、保圧20MPa、保圧時間10秒、冷却時間150秒、金型は、金型温調機を1台用いて80℃に設定し、樹脂に触れる表面の金型温度を10箇所測定した際の標準偏差が11.2に制御された成形条件で、直径500mm、高さ400mm、厚み3mmの円筒状成形品を射出成形した。得られた円筒状成形品を2個用いて、平面部を平行になる様に配置し、平面部を60秒間赤外線にて加熱した後、溶け込み量が2mmになるよう振動して溶着(赤外線/振動溶着)を行い、溶着部を有する中空成形品を得た。得られた中空成形品を用いて、前述の方法により評価した結果を表5に記載した。
Claims (9)
- 2つ以上の分割体を溶着により接合した接合箇所を有する中空成形品であって、前記中空成形品は、前記中空成形品の表面から500μm内側の部分における平均球晶サイズが20μm以下であり、前記中空成形品の接合箇所を含む試験片の引張強度が、前記中空成形品の接合箇所を含まない試験片の引張強度に対して80%以上であることを特徴とする、高圧水素に触れる中空成形品。
- 前記中空成形品が、中空成形品表面から700μm内側の部分における平均球晶サイズと中空成形品表面から200μm内側の部分における平均球晶サイズとの比が1以上2以下であることを特徴とする請求項1に記載の中空成形品。
- 前記中空成形品を16分割したそれぞれの中空成形品の表面から500μm内側の部分における平均球晶サイズの標準偏差が6以下であることを特徴とする請求項1または2に記載の中空成形品。
- 前記中空成形品がポリアミド樹脂組成物からなることを特徴とする請求項1~3のいずれかに記載の中空成形品。
- 前記中空成形品が中空成形品表面から100μm内側の部分のラマン分析においてα型結晶に由来するラマンバンドとγ型結晶に由来するラマンバンドとの強度比が2.5以下であることを特徴とする請求項4記載の中空成形品。
- 前記ポリアミド樹脂組成物が、ポリアミド6樹脂(A)100重量部に対し、アミド系ワックス(B)を0.01~10重量部配合してなるポリアミド樹脂組成物であることを特徴とする請求項4または5に記載の中空成形品。
- 前記ポリアミド樹脂組成物が、ポリアミド6樹脂(A)、および、DSC測定による融点が245℃以下であり、光散乱測定において温度250℃から20℃/分の速度で冷却して測定した際のインバリアントQの立ち上がり時間がポリアミド6樹脂(A)のインバリアントQの立ち上がり時間よりも短いポリアミド樹脂(C)を配合してなるポリアミド樹脂組成物であって、前記ポリアミド6樹脂(A)100重量部に対して、前記ポリアミド樹脂(C)を0.01~5重量部配合してなるポリアミド樹脂組成物であることを特徴とする請求項4~6のいずれかに記載の中空成形品。
- 中空成形品の製造方法であって、2つ以上の分割体を熱板溶着、赤外線溶着、および赤外線にて溶着部を温めた後に振動溶着を行う赤外線/振動溶着より選ばれたいずれかの溶着方法により接合して中空成形品を形成する工程を含み、前記中空成形品は、前記中空成形品の表面から500μm内側の部分における平均球晶サイズが20μm以下であり、前記中空成形品の接合箇所を含む試験片の引張強度が、前記中空成形品の接合箇所を含まない試験片の引張強度に対して80%以上であることを特徴とする、高圧水素に触れる中空成形品の製造方法。
- 前記中空成形品を構成する2つ以上の分割体を射出成形法および押出成形法より選ばれた成形法で成形することを特徴とする請求項8記載の中空成形品の製造方法。
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CA3036633A1 (en) | 2018-03-22 |
JP6327404B1 (ja) | 2018-05-23 |
KR20190049718A (ko) | 2019-05-09 |
CN109716011B (zh) | 2021-03-12 |
US20190232572A1 (en) | 2019-08-01 |
EP3514438A4 (en) | 2020-04-29 |
EP3514438B1 (en) | 2023-08-09 |
JPWO2018051733A1 (ja) | 2018-09-13 |
CN109716011A (zh) | 2019-05-03 |
KR102279328B1 (ko) | 2021-07-21 |
US11529766B2 (en) | 2022-12-20 |
EP3514438A1 (en) | 2019-07-24 |
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