WO2006106776A1 - ポリエステル発泡シート - Google Patents
ポリエステル発泡シート Download PDFInfo
- Publication number
- WO2006106776A1 WO2006106776A1 PCT/JP2006/306555 JP2006306555W WO2006106776A1 WO 2006106776 A1 WO2006106776 A1 WO 2006106776A1 JP 2006306555 W JP2006306555 W JP 2006306555W WO 2006106776 A1 WO2006106776 A1 WO 2006106776A1
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- WO
- WIPO (PCT)
- Prior art keywords
- foam sheet
- sheet
- polyester foam
- weight
- polyester
- Prior art date
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/04—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent
- C08J9/12—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof using blowing gases generated by a previously added blowing agent by a physical blowing agent
- C08J9/125—Water, e.g. hydrated salts
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/22—After-treatment of expandable particles; Forming foamed products
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- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
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- Y10T428/249979—Specified thickness of void-containing component [absolute or relative] or numerical cell dimension
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
- Y10T—TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
- Y10T428/00—Stock material or miscellaneous articles
- Y10T428/249921—Web or sheet containing structurally defined element or component
- Y10T428/249953—Composite having voids in a component [e.g., porous, cellular, etc.]
- Y10T428/249986—Void-containing component contains also a solid fiber or solid particle
Definitions
- the present invention relates to a foamed sheet made of polyalkylene terephthalate and a molded body obtained by thermoforming the sheet. More specifically, the present invention has excellent flexibility, light weight, thermoformability, and vacuum molding.
- a foamed sheet made of polyalkylene terephthalate that can obtain a molded article having excellent lightness, heat resistance, chemical resistance, and weather resistance by thermoforming such as, and obtained by thermoforming the sheet It relates to a molded body.
- Thermoplastic polyester resin represented by polyethylene terephthalate (hereinafter abbreviated as “PET”) resin and polybutylene terephthalate (hereinafter abbreviated as “PBT”) resin has mechanical properties, heat resistance and chemical resistance. Because of its excellent dimensional stability, it is widely used for injection molded products, blow molded products, press molded products, and films.
- thermoplastic polyester resin is rarely used as a foam for food containers, packaging materials, building materials, optical reflectors and the like. This seems to be due to the following reasons. That is, in order to use for this purpose, it is necessary to form a PET foam sheet by heat forming such as vacuum forming. For this purpose, it is necessary to use an amorphous PET sheet. However, since PET resin has a low crystallization rate, it does not crystallize during normal molding processing, and the molded product has low heat resistance and can be obtained as an amorphous material with collapsed bubbles. Can not. On the other hand, PBT resin has a very high crystallization rate, so that only a crystal sheet can be obtained, and a compact cannot be obtained by thermoforming. In order to solve such problems, it is difficult to crystallize the PET resin by heating on the mold for a long time, although it is difficult from an industrial point of view. Therefore, the crystalline molded product obtained is inferior in flexibility.
- polytrimethylene terephthalate (hereinafter abbreviated as “PTT”) resin having a low crystal elastic modulus is used.
- the main component of the soot obtained by mixing thermoplastic resin and soot or void-forming inorganic fine particles and forming voids (independent cavities) at the interface with the fine resin interface or inorganic fine particles in the film stretching process
- a white polyester film which is a component and has an optical density of 0.3 or more (see, for example, Patent Document 2).
- trimethylene terephthalate units are composed of a trimethylene terephthalate polymer having a specific intrinsic viscosity and a terminal carboxylic acid content, and an apparent density of 0.001 to 1.
- a foam that is 2 gZcm 3 .
- Patent Document 3 In the low plan, there is a proposal of a sheet obtained by adding sodium hydrogen carbonate and using n-butane as a foaming agent, having a density of 0.36 gZcm 3 and a crystallinity of 23%.
- Patent Document 1 Japanese Patent Application Laid-Open No. 5-117501
- Patent Document 2 Japanese Patent Laid-Open No. 152152357
- Patent Document 3 Japanese Patent Laid-Open No. 2002-226619
- the present invention is to solve the problem for the purpose of providing a foamed sheet capable of obtaining a molded body having both flexibility and heat resistance by heat forming such as vacuum forming, and a formed body obtained by heat forming the sheet.
- the present inventors have achieved the above problems by forming an amorphous foamed sheet made of PTT, having fine bubbles and having an appropriate crystallization speed. As a result, the inventors have found that the present invention can be achieved.
- the present invention is as follows.
- the 50 to 100 weight 0/0 of the polyalkylene terephthalate is a polytrimethylene terephthalate over preparative, polyester foam sheet according to (1) or (2).
- polyester foam sheet according to any one of (1) to (4), having an average diameter of 1Z2 or less of the thickness of the polyester foam sheet and having bubbles of 0.001 to 100 m.
- the ⁇ composition forces the polyalkylene terephthalate from 50 to 99.9 weight 0/0 and, fluorine containing ⁇ 0.1 to 50% by weight (1) any one of - (5) Polyester foam sheet as described in 1.
- melt strength polyalkylene terephthalates 50 to 99.9 weight 0/0 and, contains a fluorine-based ⁇ 0.1 to 50 wt%, polyester foamed sheet manufacturing method according to (10).
- the base has a slit-like shape, and the step of cooling and solidifying includes the step of casting the melt on a metal roll, and the step of placing the cast melt in water.
- the method for producing a polyester foam sheet according to any one of (10) to (14).
- a molding method comprising a step of heating and molding the polyester foam sheet according to any one of (1) to (9).
- the polyester foam sheet has a step of heating to 30: L00 ° C and a step of forming using a mold of 60 to 180 ° C (18) or ( The forming method according to 19).
- the foamed sheet of the present invention has excellent flexibility, light weight, and heat moldability, and is excellent in light weight, flexibility, heat resistance, and resistance to heat forming such as vacuum forming.
- a molded product having chemical properties and weather resistance can be obtained. For this reason, it is useful for various applications such as food containers, packaging materials, building materials, optical reflectors and the like.
- the polyester foamed sheet of the present invention is a foamed sheet that also comprises a resin composition containing 50 to LOO% by weight of polyalkylene terephthalate (hereinafter abbreviated as “PArT”).
- PArT was selected from the power of terephthalic acid as the acid component, and the glycol component as the main component of aliphatic glycol groups, alicyclic glycol groups, and polyalkylene glycols having 2 to 12 carbon atoms in the alkylene moiety. At least one type of alkylene glycol power.
- Heat resistance and ease of sheet manufacture PArT ratio is 70 ⁇ : LOO wt% is preferred 80 ⁇ : LOO wt% is more preferred 90 ⁇ : LOO wt% Further preferred.
- alkylene glycol examples include, for example, ethylene glycol, 1,1-propanediol, 1,2-propanediol, 1,3-propanediol, 2,2-propanediol 1,2-butanediol, 1,3- Butanediol, 1,4-butane Diol, neopentyl glycol, 1,5-pentamethylene glycol, hexamethylene glycol, heptamethylene glycol, otatamethylene glycol, decamethylene glycol, dodecamethylene glycol, 1,2-cyclohexanediol, 1, 3- Examples include cyclohexanediol, 1,4-cyclohexanediol, 1,2-cyclohexanedimethanol, 1,3-cyclohexanedimethanol, 1,4-cyclohexanedimethanol and the like. Of these PArTs, taking into account the excellent heat resistance and ease of sheet manufacture, PET, PTT
- the PArT includes containing other copolymerization components.
- Copolymerization components include alkylene glycols other than those used mainly, 5-sodium sulfoisophthalic acid, 3,5-dicarboxylic acid benzenesulfonic acid tetramethylphosphonium salt, isophthalic acid, oxalic acid, succinic acid.
- Ester-forming monomers such as acid, adipic acid, dodecanedioic acid, fumanoleic acid, maleic acid, 1,4-cyclohexanedicarboxylic acid, polyethylene glycol, polypropylene glycol, polytetramethylene glycol and copolymers thereof. Can be mentioned.
- the amount of the component that causes random copolymerization to lower the crystal melting point and the ultimate crystallinity is 30 mol% or less. More preferably, it is 20 mol% or less, and more preferably 10 mol%.
- PArTs molded articles having excellent flexibility, heat formability, and excellent heat resistance, flexibility, chemical resistance, and weather resistance by heat forming such as vacuum forming.
- a sheet which can be obtained trimethylene glycol and 5 0-100 wt 0/0 acid component terephthalic acid PArT is for purposes to easily achieve the time was present invention (1, 3-propanedioic ol both
- TMG PTT repeating unit force having diol component
- it is preferable 50 to 100 weight 0/0 of the polyalkylene terephthalate is Poritorime Chi terephthalate.
- the degree of polymerization of PArT of the present invention is in the range of 0.5 to 4 dlZg with the intrinsic viscosity [ ⁇ ] as an index. It is preferable.
- the intrinsic viscosity is 0.5 dlZg or more, it becomes easy to produce a sheet, and it becomes easy to make the bubble size fine, and a foam sheet and a molded body having excellent strength and flexibility are obtained. It becomes easy.
- 4. OdlZg or less makes it easy to form a sheet.
- the intrinsic viscosity [7?] is more preferably in the range of 0.7 to 3 dlZg, more preferably in the range of 0.9 to 2.5 dlZg, and particularly preferably in the range of 0 to 2 dlZg.
- the PArT of the present invention preferably has a carboxyl end group concentration of 0 to 80 eqZ ton relative to the PArT component. This is because the weather resistance, chemical resistance, hydrolysis resistance, and heat resistance of the sheet and the molded product can be improved.
- the carboxyl end group concentration is more preferably 0 to 5 OeqZ ton or less, more preferably 0 to 30 eqZ ton or less, and 0 to 20 meqZkg is particularly preferred, and the lower the better.
- the content of the glycol dimer component in which the glycol component of PArT is bonded through an ether bond is 0 to 2% by weight.
- the glycol dimer component is a bis (3-hydroxypropyl) ether component in the case of PTT (structural formula: -OC H CH CH OCH CH CH O-, hereinafter abbreviated as “BPE”), and in the case of PET, bis (hydroxy)
- Shetyl) ether component (Structural formula: -OCH CH OCH CH 0-, hereinafter abbreviated as ": BEE")
- the foam sheet of the present invention includes cases where various organic substances and inorganic substances and various additive agents are included in addition to PArT. Even in such a case, the ratio of PArT needs to be in the above-mentioned range.
- NMR nuclear magnetic resonance spectrum
- PArT oligomers including unreacted monomers
- cyclic dimers and various glycol dimer components are included in the ratio of PArT.
- organic substances other than PArT include cyclic and linear PArT oligomers, monomers of acid components and glycol components constituting PArT, low-molecular-weight reactants derived therefrom, and resins other than PArT, and Various additives are mentioned.
- thermoplastic naphthalate such as polyethylene naphthalate and polypropylene naphthalate, thermosetting Polyester, Nylon 6, Nylon 66, Nylon 11, Nylon 12, Polyolefin, Polyethylene, Polypropylene such as Polypropylene, Polypropylene, Fluorine resin, Silicone resin, Polyphenylene sulfite, Epoxy resin Examples thereof include fat, talyl resin, and cellulose, and copolymerized resin of these.
- Inorganic substances other than PArT include inorganic fillers and inorganic lubricants such as glass fiber, carbon fiber, talc, my strength, wollastonite, kaolin clay, calcium carbonate, titanium dioxide, diacid-silica, and polymerization. A catalyst residue etc. are mentioned.
- additives include organic and inorganic dyes and pigments, matting agents, heat stabilizers, flame retardants, antistatic agents, antifoaming agents, color modifiers, antioxidants, ultraviolet absorbers, and crystal nucleating agents. , Brighteners, impurity scavengers, thickeners, surface conditioners and the like.
- pentavalent or Z and trivalent phosphorus compounds are preferably hindered phenol compounds.
- the addition amount of the phosphorus compound is preferably 2 to 500 ppm as the weight ratio of the phosphorus element in the resin composition, preferably 10 to 200 ppm.
- Specific compounds include trimethyl phosphite, phosphoric acid, phosphorous acid, tris (2,4-di-tert-butylphenol) phosphite (Irgaf os from Chinoku Specialty Chemicals).
- the hindered phenolic compound is a phenolic derivative having a substituent having a steric hindrance adjacent to the phenolic hydroxyl group, and having one or more ester bonds in the molecule.
- the amount of hindered phenolic compound added is preferably from 0.001 to 1% by weight, more preferably from 0.01 to 0.2% by weight, based on the weight of the resin composition.
- the scavenger is preferably a polymer or oligomer of polyamide or polyesteramide, or a low molecular weight compound having an amide group or amine group.
- the addition amount is preferably 0.001 to 1% by weight, more preferably 0.01 to 0.2% by weight, based on the weight ratio of the resin composition.
- Specific compounds include polymers such as nylon 6.6, nylon 6, and nylon 4.6, such as polyamidya polyethyleneimine, and reaction product of N-phenylbenzeneamine and 2,4,4-trimethylpentene.
- These substances other than PArT may exist as particles or may be present in a polymer molecule.
- particles having an average particle size of 0.01 to: L00 m are added to PArT.
- the content is preferably 0.1 to 30% by weight. The presence of such particles makes it easy to have many fine bubbles.
- the average particle size is more preferably 0.1 to 50 / ⁇ ⁇ , more preferably 0.3 to 20 111, and particularly preferably 0.5 to LO / zm. ,. It is desirable that the particle content be larger as the average particle size of the particles is larger. The smaller the content, the smaller the content, but it is more preferable that the content is 0.5 to 20% by weight. More preferred is 2 to 10% by weight.
- the particles have a flat plate-like or needle-like protrusion that is preferable to a true sphere.
- the particles are preferably made of a material having low compatibility with PArT and low adhesion. Specific examples thereof include powerful powders such as talc and fluorinated resin represented by polytetramethylene, fluorine mica, plate-like alumina, and layered silicate.
- the resin composition contains 0.1 to 50% by weight of fluorine-based resin. By including the fluorinated resin, the reason is not clear, but it becomes easy to make fine bubbles.
- the fluorine-based resin itself has high heat resistance, not only the color tone of the fluorine-based resin itself is excellent even after melt molding, but the sheet is hardly colored. Furthermore, since it is relatively soft, the flexibility of the sheet is not impaired.
- Fluorine-based resin represents a synthetic polymer containing fluorine atoms in the molecule.
- Specific examples include polytetrafluoroethylene (hereinafter abbreviated as “PTFE”), tetrafluoroethylene-hexafluoropropylene copolymer (hereinafter abbreviated as “FEP”), tetrafluoroethylene- Perfluoroalkyl butyl ether copolymer (hereinafter abbreviated as “PFA”), polychlorotrifluoroethylene (hereinafter abbreviated as “PCTFE”), ethylene tetrafluoroethylene copolymer (hereinafter abbreviated as “ETFE”), low melting point ethylene Examples thereof include tetrafluoroethylene copolymer (hereinafter abbreviated as “LM-ETFE”), polyvinylidene fluoride (PVDF), and polyfluoride bur.
- PTFE polytetrafluoroethylene
- FEP
- those composed only of carbon atoms and fluorine atoms and having a melting point of 280 ° C or higher, more preferably 300 ° C or higher are preferred.
- PTFE and FEP are preferred, and PTFE is particularly preferred.
- the content of the fluorinated resin is preferably 0.2 to 50% by weight, more preferably 0.5 to 30% by weight, and further preferably 1 to 20% by weight. It is particularly preferably 2 to 10% by weight.
- Such a fluorinated resin has an average particle size of 0.01 to LOO ⁇ m, and is preferably contained in the foam sheet. The presence of such granular fluorinated resin facilitates having many fine bubbles.
- the fluorinated resin has an average particle size of 0.1 to 50 / zm, more preferably S, more preferably 0.3 to 20 111, and 0.5 to LO / zm. Particularly preferred. It is also preferable that the fluorinated resin has a flat plate-like or needle-like protrusion that is preferable to a true sphere.
- the average particle size can be obtained using image analysis software from a cross-sectional image of a sheet observed using a scanning electron microscope (hereinafter abbreviated as “SEM”).
- the thickness of the foam sheet can be appropriately selected depending on the purpose and application, but is preferably 1 ⁇ m to 10 mm in order to make use of the function of the foam sheet of the present invention. : L m or less Setting it above makes it easier to handle the sheet, and setting it to 10 mm or less makes it easier to heat form.
- the thickness is more preferably 10 ⁇ m to 5 mm, more preferably 50 ⁇ m to 3 mm, and even more preferably 100 ⁇ m to 2 mm.
- the polyester foam sheet of the present invention must first be lightweight and excellent in flexibility.
- the apparent density should be 0.05-1.25 g / cm 3 .
- Apparent density 0. 1 ⁇ :.. LgZcm 3 a it is favorable preferred, from 0.15 to 0 more preferably it forces a 8g / cm 3, 0. 2 ⁇ 0 further to be 7 g / cm 3 preferable.
- the polyester foam sheet of the present invention can be easily heat-formed, and crystallizes by heat forming to have heat resistance. For this reason, the polyester foam sheet of the present invention has a crystallinity that changes due to heat, and an appropriate change rate (crystallization rate).
- Whether or not the degree of crystallinity can be changed by heat depends on crystallization between 0 and 150 ° C when performing thermal analysis with an input-compensated differential calorimeter (hereinafter abbreviated as “DSC”). This can be understood by examining whether or not the exothermic peak is observed.
- the temperature at which an exothermic peak derived from crystallization is observed in the polyester foam sheet of the present invention when thermal analysis is performed with an input-compensated differential calorimeter is 0 to 150 ° C.
- an exothermic peak is observed, which means that a peak with a calorific value of lj / g or more is observed.
- the amount of heat is preferably 3 jZg or more, more preferably 5 jZg or more, and even more preferably lOjZg or more.
- the upper limit is usually 90jZg or less.
- the rate of change in crystallinity is moderate, which means that the foam sheet force isothermic crystallization peak time is 5-60 seconds, the temperature is 100-150 ° C
- the peak time of isothermal crystallization of the resin composition constituting the polyester foam sheet of the present invention is 5 to 60 seconds at any temperature of 100 to 150 ° C.
- the peak time of isothermal crystallization is observed when the sheet is melted and then rapidly cooled and kept at a predetermined temperature.
- the endothermic force derived from crystallization can be calculated as the time to show the S peak.
- the temperature range where the peak time of isothermal crystallization is 5 to 60 seconds is the cooling temperature range of 100 to 150 ° C.
- the above peak time is measured every ° C. When both adjacent points were at the peak time, the temperature range was calculated assuming that the two peak points all satisfied the peak time.
- the above temperature range is preferably 5 ° C or higher continuously, more preferably 10 ° C or higher, more preferably 20 ° C or higher, more preferably 100 to 150 ° C. Especially preferred is a peak time of 5 to 60 seconds.
- the polyester foam sheet of the present invention preferably has a crystallization peak time in the range of 30 to 120 ° C with a temperature force of 1 to 600 seconds.
- the crystallization peak time of the sheet can be obtained by measuring the time during which the endothermic amount resulting from crystallization observed when the sheet is rapidly heated to a predetermined temperature and held as it is, Determine the heating temperature by measuring the peak time every 5 ° C in the range of 30 to 120 ° C.
- the crystallization peak time as described above indicates the crystallization rate, and the crystallization peak time as described above in the temperature range described above indicates that the heat formability is good and that the heat forming is performed. It shows that it can be easily crystallized to impart heat resistance.
- the temperature range is preferably 5 ° C or higher continuously, more preferably 10 ° C or higher, and particularly preferably 20 ° C or higher.
- the foamed sheet preferably has a crystallinity of 20% or less.
- the crystallinity was obtained from the ratio of the crystal peak area to the total area of the diffraction pattern obtained by wide-angle X-ray diffraction.
- the degree of crystallinity is preferably 15% or less, more preferably 10% or less, still more preferably 5% or less, and more preferably 0% (no crystal peak is observed). preferable.
- the heat of crystal melting when thermal analysis is performed by DSC is 20 jZg or more. Having such an amount of heat indicates that the degree of crystallization is increased by thermoforming, which means that the heat resistance is increased.
- the heat of crystal fusion is more preferably 30 jZg or more, more preferably 35 jZg or more, and still more preferably 40 jZg or more.
- the composition of PArT described above can be selected as appropriate, The force that can be achieved by adding an additive such as a crystal nucleating agent.
- an additive such as a crystal nucleating agent.
- PTT as PArT makes it easy to obtain the foam sheet intended by the present invention.
- the average diameter of the bubbles is preferably 1Z2 or less of the polyester foam sheet thickness and 0.001 to 100 / ⁇ ⁇ .
- the ratio of the average size (S) in the plane direction to the average size ()) in the thickness direction is preferably 0.5 to 10 for the bubbles.
- the average diameter of the bubble indicates the average diameter of the bubble cross section
- the average size in the surface direction of the bubble (S) indicates the average value of the size (length) in the direction parallel to the sheet surface of the bubble cross section
- the average size ( ⁇ ) in the thickness direction of the bubble is the average value of the size (height) in the direction perpendicular to the sheet surface of the bubble cross section.
- the average diameter of the bubbles is 1Z10 or less of the thickness of the sheet, and more preferably 0.01 to 50 / ⁇ ⁇ , and more preferably 1Z50 or less and 0.1 to 30 111. It is particularly preferably 1/100 or less and 0.5 to 20 / ⁇ ⁇ . SZT is more preferably from 0.7 to 5, more preferably from 0.8 to 3, particularly preferably from 1 to 2.
- the sheet of the present invention is desired to have good color tone.
- the color tone is preferably not pigmented or dyed, and it is preferable that L *, which is an indicator of lightness, is 80 or more, more preferably 85 or more, and 90 or more, depending on the state. There is no upper limit for L *, but it is usually 100 or less.
- b *, which is an index representing yellowness is preferably ⁇ 5 to: L0, more preferably ⁇ 3 to 8, and further preferably ⁇ 2 to 5.
- the sheet of the present invention preferably has a value obtained by dividing the tensile elastic modulus by the density of 50 to 1500 MPa'cm 3 Zg.
- the tensile modulus is the average value in the MD and TD directions.
- the value obtained by dividing the bow I tensile modulus by density is more preferably 100 to 1200 MPa ⁇ cm 3 Zg, 200 to: L 100 MPa'cm 3 / g Force S More preferably, 300 to 1000 MPa ' cm Especially preferred to be 3 Zg.
- the foam sheet of the present invention has a weight of ⁇ ? : Mix the melted material consisting of the chopped material in a gaseous state at the melting temperature and normal pressure of the PArT and dissolve it, then extrude it from the die and mold it. It can be obtained by cooling and solidifying.
- the melt indicates that it is in a fluid state, and it is not necessary that all the components melt.
- the PArT composition is supplied to the supply part of the extruder, and the composition is melted and sent out by rotation of the screw, and is extruded from a die such as a slit through a heated channel.
- the PArT composition can be obtained by a conventionally known method.
- the PTT composition is made from dimethyl terephthalate and trimethylene glycol, and if necessary, other copolymerization components as raw materials, and titanium tetrabutoxide as a catalyst at normal pressure at a temperature of 180 to 260 ° C. After the transesterification reaction, it can be obtained by performing a polycondensation reaction at 220 to 270 ° C. under reduced pressure.
- the melt preferably contains particles having an average particle diameter of 0.01 to 100 ⁇ m, but the particles have an average particle diameter of 0.01 to: particles having a LOO m It is preferable to be added as By adding such particles, it becomes easy to have many fine bubbles.
- the average particle size of 0.1 to 50 111 is preferred to be 0.3 to 20 m.
- Power S is more preferred 0.5 to: LO m in particular preferable.
- the content of the particles is preferably as small as possible as the average particle size of the particles is large, but is preferably as low as 0.5 to 20% by weight. It is even more preferable that it is 2 to 10% by weight. It is also preferable that the particles have a flat plate-like or needle-like projection that is preferable to a true sphere.
- the particles are preferably made of materials that have low compatibility with PArT and low adhesion.
- the melt preferably contains a fluorinated resin.
- the fluorinated resin has an average particle size of 0.01-100 It is preferable to add as m particles. By adding such particles, it becomes easy to include the granular fluorine-based resin of 0.01 to LOO / zm as described above in the foam sheet. It is more preferable that the added particles have an average particle size of 0.1 to 50 m, more preferably 0.3 to 20 ⁇ m, and particularly preferably 0.5 to 10 ⁇ m. preferable.
- the particles have protrusions that are preferably flat plate-like or needle-like than spherical.
- the average particle size is a value obtained by determining the particle size of particles dispersed in water using a laser light diffraction Z scattering method. Such fluorinated resin is baked by the production method and unfired, but in the present invention, unfired is preferable because it is easy to reduce the size of the bubbles.
- Preferred additives for producing foamed sheets such as particles including fluorinated resin are additives added at the time of polymerization, melt kneading after polymerization, or the like. These can be added by a combination method, etc., and can be appropriately selected depending on the kind and amount of additives, required performance, and the like.
- various additives are added by melt-kneading, the PTT composition obtained by polymerization is cooled and solidified, or in a molten or uniaxial or biaxial extruder together with various additives. Can be done.
- the extruder a single-screw or twin-screw extruder, a tandem extruder in which two or more of these are connected in series, and the like can be used. It is preferable to use an optimum screw according to the properties of the PArT composition to be applied and the properties of the substance gas to be injected. It is desirable to set the extruder to a temperature at which unmelted material does not remain and the thermal decomposition of the composition can be suppressed, and it is desirable to set the melting point of the PArT composition to +30 to 30 ° C.
- a filter is installed between the extruder and the die to remove foreign substances, a gear pump or the like is provided to improve quantitative supply, and the dispersion of the injected substance is performed.
- a static mixer is installed to improve the performance, and a heat exchange unit is installed to keep the temperature constant.
- it is desirable to appropriately select the pressure and temperature so that the substance injected in the vicinity of the equipment does not become large bubbles.
- a material that is in a gaseous state at a normal pressure of the melting temperature into the melt Only by injecting such a substance can an excellent foam sheet be obtained.
- Such materials are preferably in a gaseous state even at room temperature and pressure in view of ease of handling.
- Specific examples include inert compound blowing agents such as nitrogen, carbon dioxide, helium, argon, water, ethane, propane, butane, ethylene, propylene, petroleum ether, pentanes, hexanes, heptanes, toluene, trichloro.
- Aliphatic hydrocarbon blowing agents such as methane, tetrachloromethane, trichlorofluoromethane, methanol, 2-propanol, isopropyl ether, methylethylketone, methyl chloride, dichloroethane, chloroform, fluoromethane, difluoromethane, trifluoroethane, Examples include chlorotrifluoromethane, dichlorodifluoromethane, chlorochloroethane, dichlorotetrafluoroethane, and the like.
- fluorocarbons include CFC series CFCs such as CFCs (Rll, R-12), CFC substitutes (R-134a), CFC-11, CFC-12, CFC-113, CFC-114, etc.
- Freon halogeno-hydrocarbon foaming agents and the like.
- nitrogen, helium, argon, and water are preferred, and nitrogen is particularly preferred from the viewpoint of not proceeding with crystallization of the sheet and reducing the bubble size.
- the amount to be injected is preferably 0.05 to 10% by weight from the viewpoints of making the bubbles fine and improving the surface state of the sheet.
- the injection amount is more preferably 0.1 to 5% by weight.
- the injection method may be any time as long as it is between the extruder and the die, but it is preferable to inject it with the extruder because the substance can be uniformly injected into the melt.
- the melt is then extruded from the die and formed into a sheet shape, and the pressure is released and the molten material is foamed.
- Force that can be selected as appropriate according to the shape of the target sheet.
- straight slits such as T-die and I-die and circles called round dies are used. It is desirable to use a circumferential slit.
- the structure of the base is appropriately designed so that foaming does not occur in the base.
- the pressure of the melt at the inlet of the die is lOMPa or more.
- the melt formed into a sheet and then foamed is then cooled and solidified, but in the present invention, it is preferable to quickly cool and solidify so as to suppress crystallization of the sheet and enlargement of bubbles.
- Examples of such a cooling and solidification method include a method in which the melt is brought into contact with a solid such as a cooling roll that is controlled below the crystallization temperature of the PArT composition, a method in which the sheet is brought into contact with a liquid such as water, and the like. And a combination of these methods. Of these, the method in which the melt is cast on a roll and then placed in water and cooled and solidified is most preferred. In addition, solids such as cooling rolls are preferably made of metal with good heat conduction.
- the temperature of the solid or liquid to be contacted is more preferably 0 to 50 ° C, more preferably 0 to 30 ° C, and particularly preferably 0 to 20 ° C.
- the time from the extrusion from the die to contact with the solid or liquid is preferably 0.05 to 10 seconds, more preferably 0.1 to 5 seconds, and 0.2 to 2 seconds. Especially preferred to be.
- the foamed sheet of the present invention can be formed into a foamed molded article by thermoforming.
- the foamed molded body is preferably crystallized at the time of thermoforming. By doing in this way, heat resistance can be improved.
- the degree of crystallization it is preferable that the exothermic peak derived from crystallization observed at 0 to 150 ° C when thermal analysis is performed by DSC is 5 jZg or less. It is even more preferred that it is less than UZg.
- the crystallinity is preferably 10% or more, more preferably 20% or more.
- the crystallinity is a value obtained by wide-angle X-ray diffraction.
- the apparent density is 0.5 05-1 is preferably 25gZcm a 3 instrument 0. 1:.. And more preferably LgZcm a 3 instrument 0. 15-0 that 8gZcm is 3 Even more preferred is U, especially preferred to be 0.2 to 0.7 gZcm 3 .
- the shape of the molded body can be appropriately selected depending on the application. For example, box shape, cup shape
- Examples of a method for heat-molding such a molded body include press molding, straight molding, drape molding, plug assist molding, vacuum molding, vacuum pressure molding, and pressure molding.
- vacuum / pressure forming is more preferable.
- the sheet When forming, it is preferable to first heat the sheet to a temperature of 30 ° C to 100 ° C by means of heater radiation or a heating plate. By doing so, it becomes easy to soften the sheet without crystallizing, and the moldability and transferability are improved.
- the temperature is more preferably 35 to 90 ° C, more preferably 40 to 80 ° C, and even more preferably 45 to 70 ° C.
- the sheet is formed by contacting with a mold, and the mold temperature at this time is preferably 60 ° C to 180 ° C.
- the foamed sheet is almost in an amorphous state at the time of shaping in order to ensure moldability, but after shaping, it is important to crystallize the molded body in order to ensure heat resistance. is there.
- the mold temperature is preferably 65 ° C or higher, and in order to prevent mold force release or bubble collapse after molding, it should be 180 ° C or lower. Is desirable.
- the mold temperature is more preferably 80 to 160 ° C, and particularly preferably 100 to 150 ° C.
- One of the preferable methods is to raise the temperature of the mold after molding or to heat the sheet to the temperature within the above range by heating from the outside.
- the contact time with the mold is preferably 1 to 600 seconds, more preferably 2 to 300 seconds, more preferably 5 to 200 seconds, and even more preferably 10 to 100 seconds. Is particularly preferred!
- the heat molding may be performed by stacking two or more foam sheets.
- the foamed sheet of the present invention is crystallized by contacting with a rotating roll heated to 60 to 180 ° C. Can be obtained at At this time, the roll surface has various patterns including mirror surface and satin. By doing so, a film having a desired surface shape or a sheet-like molded body can be obtained.
- the contact time with the rotating roll is preferably 1 to 600 seconds, more preferably 2 to 300 seconds, more preferably 5 to 200 seconds, and more preferably 10 to LOO seconds. It is particularly preferred.
- PArT content PArT content, PTT content, glycol dimer component content
- Intrinsic viscosity is 35 ° C using an Ostwald viscometer. -Specific viscosity in black mouth phenol r? Sp and concentration C (g / 100 milliliters) ratio 7? Sp / C was extrapolated to zero concentration, and obtained according to the following formula.
- the foamed sheet was dried at 50 ° C., and the weight when the constant value was reached was divided by the volume. The volume was determined by immersing the sheet in water. [0078] (5) Amount of heat of crystallization derived from crystallization
- the degree of crystallinity was determined from the ratio of the crystal peak area in the diffraction pattern obtained by wide-angle X-ray diffraction to the total area.
- wide-angle X-ray diffraction was performed by the following method.
- Measuring device Wide-angle X-ray diffractometer Rotorflex RU-200 (manufactured by Rigaku Corporation (currently Rigaku Corporation))
- X-ray source CuK o; ray
- Integration time 1 second As the diffraction intensity, the true diffraction intensity obtained from the diffraction intensity obtained by measuring the sample and the air scattering intensity according to the following formula was used.
- the particle size of the powder dispersed in water was determined as the equivalent circle diameter using a Microtrac FRA particle size analyzer manufactured by Nikkiso Co., Ltd. using a laser light diffraction Z scattering method.
- the ratio of the average bubble size to the average size in the plane direction (S) and the average size in the thickness direction (T) SZT runs through the sheet cross section in both the MD direction (sheet longitudinal direction) and TD direction (sheet width direction). It was obtained using an image analysis software from a cross-sectional image observed using a vertical electron microscope (hereinafter abbreviated as “SEM”). Image-Pro Plus ver. 4.0 (Branetron Co., Ltd.) was used as image analysis software. The average bubble diameter was determined by averaging the average values of the major and uniaxial projections of the equivalent ellipse obtained by approximating the bubble cross-section to an ellipse in each of the MD and TD directions. .
- S and T are the bounding rectangle of the bubble (the average value of the height and width of the smallest rectangle that completely encloses the entire bubble and has a side parallel to the sheet surface direction, and the MD and TD directions. It was calculated on average in each direction.
- a cup-shaped molded product in which the sheet is in contact with the inner diameter of the mouth 200 mm, bottom inner diameter 190 mm, depth 50 mm, and bottom peripheral force 3 ⁇ 41 by vacuum / pressure forming, and the bottom transferability is evaluated as follows: did.
- ⁇ Flat bottom diameter is 185mm or more
- ⁇ The diameter of the flat bottom is 180 or more and less than 185mm
- the tensile modulus was obtained by a tensile test according to ASTM D882, and a value obtained by dividing the modulus by density was used as a method for evaluating flexibility.
- the cup-shaped product molded during the heat formability evaluation was heat-treated at 150 ° C. for 10 minutes, and then placed on a flat plate, and the float around the bottom (gap) was evaluated as follows.
- the sheet was extruded from a T die having a spacing of 0.5 mm at a linear speed of 5 mZ and formed into a sheet shape. At this time, 0.1% by weight of nitrogen with respect to the composition was injected from the middle of the extruder to be mixed and dissolved with the melt. The melt pressure at the T-die inlet was 15 MPa. The melt extruded from the T-die was cast on a metal rotating tool 50 mm away, and then introduced into cooling water to be cooled and solidified to obtain a foam sheet.
- the rotating roll and the cooling water were controlled to be 10 ° C, and the time from the extrusion of the melt to the contact with the rotating roll was 0.6 seconds, which was 68 ° which is the crystallization temperature of the composition. It took 20 seconds or less to cool to below C.
- the obtained foamed sheet had a thickness of lmm and a width of 100mm, and even when bent at 180 °, the sheet did not crack and was strong.
- the intrinsic viscosity [ ⁇ ?] was 1.15 dlZg, the carboxyl end group concentration was 15 eqZ ton, the BPE content was 0.5% by weight, and the density was 0.6 gZcm3.
- the sheet has a resin composition that has an isothermal crystallization peak time of 5-60 seconds over the entire range of 100-150 ° C, the crystallization heat of the sheet is 15jZg, and the isothermal crystallization peak time is 30-120. It was between 1 and 600 seconds over 20 ° C range at ° C.
- the obtained sheet was molded by a vacuum / pressure forming method to obtain a cup-shaped molded product having an inner diameter of 200 mm and a depth of 50 mm.
- the sheet was first heated to 55 ° C with heater radiation, and then contacted with an aluminum mold heated to 120 ° C at a degree of vacuum of 720mmH and a pressure of 0.2MPa. This was carried out by holding for 120 seconds for crystallization.
- the obtained foamed molded article was a lightweight molded article with an apparent density of 0.6 g / cm3. In DSC evaluation, no exothermic peak due to crystallization was observed between 0 and 150 ° C, the crystallinity obtained from wide-angle X-ray diffraction was 20%, and excellent heat resistance. Te! /
- a foamed sheet was obtained in the same manner as in Example 1 except that the added particles were changed to those shown in Table 1, respectively. The results are shown in Table 2. In either case, the sheet had excellent lightness and flexibility within the scope of the present invention. Of these, the sheet of Example 2 was excellent in whiteness, with L * of 95 and b * of 1.
- Example 5 a test was performed without adding particles. As a result, a sheet having excellent lightness and flexibility was obtained although the bubble diameter was considerably large.
- a foamed sheet was obtained in the same manner as in Example 1 except that the thickness of the sheet was changed by changing the extrusion amount and the interval between the T dies. At this time, the interval of the T dies was adjusted so that the pressure of the melt at the T die inlet was lOMPa or more. The results are shown in Table 2. In either case, the sheet had excellent lightness and flexibility within the scope of the present invention.
- Example 8 when vacuum-pressure forming was carried out in the same manner as in Example 1, all the sheets were excellent in formability, and the obtained formed article had excellent heat resistance! (Example 8)
- PTT PTT having an intrinsic viscosity [r?] Of 0.9 dl / g, a carboxyl end group concentration of 20 eq / ton, and a BPE content of 0.5% by weight was used in Example 2.
- a foam sheet was obtained in the same manner as in Example 1 except that the same PTFE was used. At this time, the interval between the T dies was adjusted so that the pressure of the melt at the T die inlet was lOMPa or more. The results are shown in Table 2. In either case, the sheet had excellent lightness and flexibility within the scope of the present invention. Also, L * was 9 5 and b * was 1, which was excellent in whiteness.
- the metal rotating roll was cooled and solidified without being cooled or introduced into water to obtain a foamed sheet. At this time, the temperature of the rotating roll rose to 60 ° C by the heat brought in by the melt, and it took 2 minutes to cool the sheet to 68 ° C or less, which is the crystallization temperature. The results are shown in Table 2. The obtained sheet was inferior in flexibility, being split into two when bent at 180 °.
- Comparative Example 2 has an intrinsic viscosity [7?] Of 0.85 dl / g and a carboxyl end group concentration of 30 eq / ton, 95% by weight, and Comparative Example 3 has an intrinsic viscosity [ r?] was 1.0 dlZg, and a foamed sheet was obtained in the same manner as in Example 1 except that 95% by weight of PBT having a carboxyl end group concentration of 50 eqZ tons was used.
- the temperatures of the extruder and T-die were set 30 ° C higher than in Example 1. The results are shown in Table 2.
- a foamed sheet was obtained in the same manner as in Example 1 except that 75 parts by weight of PTT and 20% by weight of PBT used in Comparative Example 3 were used instead of 95 parts by weight of PTT. At this time, the interval between the T dies was adjusted so that the pressure of the melt at the T die inlet was lOMPa or more. The results are shown in Table 2. In either case, the sheet had excellent lightness and flexibility within the scope of the present invention.
- the intrinsic viscosity [r?] Is 1. 3 dl / g, melting point carboxyl end group concentration LOeq / ton, relative to 1 3 ⁇ 95 parts by weight of BPE (DE) including chromatic ratio 0.5 wt% 310 More than ° C, average particle size of 3.5 ⁇ m, calcined ⁇ PTFE powder with a melting point of 225 ° C with 5 parts by weight of PTFE powder.
- a sheet was obtained in the same manner as in Example 1 except that a 4 mm T-die was used.
- the obtained foamed sheet had a thickness of 0.5 mm, a width of 100 mm, an L * force of 5, and a b * of 1, which was excellent in whiteness.
- the intrinsic viscosity [ ⁇ ?] Is 1.15dlZg, and the carboxyl end group concentration is 15 eq / ton, BPE content was 0.5% by weight, and the apparent density was 0.6 g / cm3.
- the sheet has isothermal crystallization peak time of 5 to 60 seconds over the entire range of 100 to 150 ° C. It consists of a resin composition and the heat of crystallization of the sheet is 15jZg. The peak time was between 1 and 600 seconds over a range of 20 ° C and above at 30-120 ° C. Further, no diffraction peak derived from the crystal was observed by wide-angle X-ray diffraction, and the crystallinity was 0%.
- a foamed sheet was obtained in the same manner as in Example 1 except that the kind of PTFE particles added and Z or the amount of applied force were changed to those shown in Table 1, respectively. The results are shown in Table 2. In either case, the sheet was excellent and had characteristics within the scope of the present invention.
- a foamed sheet was obtained in the same manner as in Example 1 except that the thickness of the sheet was changed by changing the extrusion amount and the interval between the T dies, and the type of PTFE particles added was changed to the one shown in Table 1. It was. At this time, the distance between the T dies was adjusted so that the melt pressure at the T die inlet would be lOMPa or more. The results are shown in Table 2. The obtained sheet was an excellent sheet having characteristics within the scope of the present invention.
- Intrinsic viscosity [r?] Is 0.778dlZg, carboxyl end group concentration is 7eqZ ton, BPE (DE) content is 0.
- BPE (DE) content is 0.
- a soot composition with a melting point of 225 ° C with 5% by weight added, melted by feeding it to a 50mm ⁇ single screw extruder set at 265 ° C, and then through a channel heated to the same temperature as the extruder, The sheet was extruded from a T die with a width of 550 mm and a spacing of 1.5 mm at a linear speed of 5 mZ to form a sheet.
- the obtained foamed sheet has a thickness of 3 mm, a width of 500 mm, an intrinsic viscosity [ ⁇ ] of 0.75 dl / g, a carboxyl end group concentration of l leq / ton, and a BPE content of 0.5% by weight.
- the density was 0.36 gZcm3.
- the sheet was crystallized with a heat of crystallization of OjZg and a crystallinity of 23%, and when folded at 180 °, it was split into two, and the sheet was inferior in flexibility.
- This example is an example of copolymerized PET.
- the foamed sheet of the present invention has excellent flexibility, light weight, heat formability, and excellent lightness, flexibility, heat resistance, chemical resistance, by heat forming such as vacuum forming.
- a molded article having weather resistance can be obtained. For this reason, it is useful for various applications such as food containers, packaging materials, building materials, optical reflectors and the like.
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- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
- Extrusion Moulding Of Plastics Or The Like (AREA)
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Abstract
Description
Claims
Priority Applications (4)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN2006800109296A CN101155863B (zh) | 2005-03-30 | 2006-03-29 | 聚酯泡沫片 |
JP2007512816A JPWO2006106776A1 (ja) | 2005-03-30 | 2006-03-29 | ポリエステル発泡シート |
US11/886,148 US20080280118A1 (en) | 2005-03-30 | 2006-03-29 | Polyester Foamed Sheet |
EP06730503A EP1865022A4 (en) | 2005-03-30 | 2006-03-29 | DAMAGED POLYESTER FOIL |
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JP2005098111 | 2005-03-30 | ||
JP2005-098111 | 2005-03-30 | ||
JP2005109799 | 2005-04-06 | ||
JP2005-109799 | 2005-04-06 |
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WO2006106776A1 true WO2006106776A1 (ja) | 2006-10-12 |
Family
ID=37073335
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/JP2006/306555 WO2006106776A1 (ja) | 2005-03-30 | 2006-03-29 | ポリエステル発泡シート |
Country Status (7)
Country | Link |
---|---|
US (1) | US20080280118A1 (ja) |
EP (1) | EP1865022A4 (ja) |
JP (1) | JPWO2006106776A1 (ja) |
KR (1) | KR20070119660A (ja) |
CN (1) | CN101155863B (ja) |
TW (1) | TW200700479A (ja) |
WO (1) | WO2006106776A1 (ja) |
Cited By (6)
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JPS6095515A (ja) * | 1983-09-26 | 1985-05-28 | テクトロニツクス・インコーポレイテツド | カラーフイルタ |
JP2013076011A (ja) * | 2011-09-30 | 2013-04-25 | Sekisui Plastics Co Ltd | ポリ乳酸系樹脂発泡シート、及び、ポリ乳酸系樹脂発泡シートの製造方法 |
JP2015098587A (ja) * | 2013-10-18 | 2015-05-28 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡粒子及びその製造方法、発泡成形体及びその製造方法、並びに複合発泡体 |
JP2016151004A (ja) * | 2015-02-19 | 2016-08-22 | 積水化成品工業株式会社 | 樹脂発泡シート及び繊維強化複合体 |
WO2018105606A1 (ja) * | 2016-12-05 | 2018-06-14 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡シートおよび熱可塑性ポリエステル系樹脂発泡容器 |
JP2018090761A (ja) * | 2016-12-05 | 2018-06-14 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡シートおよび熱可塑性ポリエステル系樹脂発泡容器 |
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Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US11351743B2 (en) * | 2018-07-24 | 2022-06-07 | The Boeing Company | Co-consolidation of thermoplastic parts |
KR102443537B1 (ko) * | 2020-04-21 | 2022-09-16 | 주식회사 휴비스 | 카르복실 말단기의 당량이 제어된 폴리에스테르 발포시트 |
CN113336997B (zh) * | 2021-06-01 | 2022-04-22 | 中山大学 | 一种聚酯发泡片材及其半连续制备方法 |
JP2023012300A (ja) * | 2021-07-13 | 2023-01-25 | 株式会社リコー | 発泡シート、製造物及び発泡シートの製造方法 |
CN113789035B (zh) * | 2021-09-06 | 2023-07-11 | 北京工商大学 | 一种取向的pbt微纳孔泡沫材料及其制备方法 |
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JPS6095515A (ja) * | 1983-09-26 | 1985-05-28 | テクトロニツクス・インコーポレイテツド | カラーフイルタ |
JP2013076011A (ja) * | 2011-09-30 | 2013-04-25 | Sekisui Plastics Co Ltd | ポリ乳酸系樹脂発泡シート、及び、ポリ乳酸系樹脂発泡シートの製造方法 |
JP2015098587A (ja) * | 2013-10-18 | 2015-05-28 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡粒子及びその製造方法、発泡成形体及びその製造方法、並びに複合発泡体 |
JP2016151004A (ja) * | 2015-02-19 | 2016-08-22 | 積水化成品工業株式会社 | 樹脂発泡シート及び繊維強化複合体 |
WO2018105606A1 (ja) * | 2016-12-05 | 2018-06-14 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡シートおよび熱可塑性ポリエステル系樹脂発泡容器 |
JP2018090761A (ja) * | 2016-12-05 | 2018-06-14 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡シートおよび熱可塑性ポリエステル系樹脂発泡容器 |
JP2019173022A (ja) * | 2016-12-05 | 2019-10-10 | 積水化成品工業株式会社 | 熱可塑性ポリエステル系樹脂発泡シートおよび熱可塑性ポリエステル系樹脂発泡容器 |
Also Published As
Publication number | Publication date |
---|---|
JPWO2006106776A1 (ja) | 2008-09-11 |
EP1865022A4 (en) | 2010-04-21 |
US20080280118A1 (en) | 2008-11-13 |
KR20070119660A (ko) | 2007-12-20 |
CN101155863A (zh) | 2008-04-02 |
TW200700479A (en) | 2007-01-01 |
CN101155863B (zh) | 2012-04-04 |
EP1865022A1 (en) | 2007-12-12 |
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