WO2022190631A1 - 樹脂組成物および成形体 - Google Patents
樹脂組成物および成形体 Download PDFInfo
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- WO2022190631A1 WO2022190631A1 PCT/JP2022/001332 JP2022001332W WO2022190631A1 WO 2022190631 A1 WO2022190631 A1 WO 2022190631A1 JP 2022001332 W JP2022001332 W JP 2022001332W WO 2022190631 A1 WO2022190631 A1 WO 2022190631A1
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- resin composition
- mass
- parts
- heat storage
- compound
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/10—Esters; Ether-esters
- C08K5/101—Esters; Ether-esters of monocarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/04—Ingredients treated with organic substances
- C08K9/06—Ingredients treated with organic substances with silicon-containing compounds
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/002—Physical properties
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/009—Additives being defined by their hardness
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/34—Silicon-containing compounds
- C08K3/36—Silica
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/22—Expanded, porous or hollow particles
- C08K7/24—Expanded, porous or hollow particles inorganic
Definitions
- the present invention relates to a resin composition and a molded article, and more particularly to a thermoplastic resin composition capable of controlling temperature sensation and a molded article thereof.
- the concept is to make it difficult for the temperature to change even at high temperatures in the middle of summer or low temperatures in the middle of winter, and to make it difficult to feel hot or cold when touched. This is due to the mechanism that energy is spent on the phase transition (solid ⁇ liquid, liquid ⁇ solid), and by maintaining the phase transition temperature for a certain period of time, it is possible to delay the rise and fall of the temperature. is. Examples based on this concept include sheets that provide a cooling sensation, and materials that suppress the temperature rise of the steering wheel and instrument panel, which become hot inside the vehicle during the summer.
- Patent Document 1 discloses, as a resin composition containing a phase transition material as described above, a thermoplastic resin having a heat of crystal fusion ( ⁇ Hm) of 100 J/g or less, and heat-storing microcapsules, wherein the heat of crystal fusion (A heat storage resin composition having a ⁇ Hm) of 50 J/g or more is disclosed.
- a heat storage material is composed of a thermoplastic resin and heat storage material particles dispersed in the thermoplastic resin and containing a heat storage material, and the particle size of the heat storage material particles satisfies specific conditions. Particle-containing resin pellets are disclosed.
- a resin composition containing a phase transition material such as a heat storage compound is required to have high heat resistance depending on the application. There was a problem of insufficient sex. Also, when using a thermoplastic resin with high heat resistance, it may be necessary to melt-knead the phase change material and the thermoplastic resin at a relatively high temperature (for example, a temperature of 200 ° C. or higher). is required to have heat resistance that can withstand the process temperature during melt-kneading with the resin. In addition, the resulting molded article is required to have the property that the phase transition material does not leak out from the resin (does not bleed out), as well as brittleness resistance and lightness. However, in the prior art, such considerations have not been sufficiently made.
- the present invention has process heat resistance that can be handled even when melt-kneaded with a resin at a relatively high temperature, and does not leak from the resin when formed into a molded product (bleed out).
- the present invention provides a resin composition containing a heat accumulating compound having a characteristic that does not prevent heat, and capable of controlling temperature sensation, and capable of obtaining a molded article having excellent brittleness resistance and light weight, and a molded article made of the resin composition. The task is to
- the present inventors have made intensive studies to solve the above problems. As a result, the inventors have found that the above problems can be solved by a resin composition containing specific amounts of a specific thermoplastic resin, a heat storage compound and a porous inorganic compound, and have completed the present invention. Embodiment examples of the present invention are shown below.
- thermoplastic resin (A) that satisfies the following requirements (a-1) to (a-3); 10 to 100 parts by mass of a heat storage compound (B) having a flash point of 200° C. or higher (different from the component (A)); 1.5 to 20 parts by mass of a porous inorganic compound (C) having an oil absorption of 4.0 g / g or more,
- the resin composition of the present invention can be produced by melt-kneading at a relatively high temperature (for example, a temperature of 200°C or higher).
- a relatively high temperature for example, a temperature of 200°C or higher.
- the heat storage compound phase transition material
- the resin composition of the present invention is used, the heat storage compound (phase transition material) does not leak out from the resin (does not bleed out), it is possible to control the temperature sensation, and it is brittle resistant and lightweight. Excellent moldings can be produced.
- the resin composition according to the present invention is 100 parts by mass of a thermoplastic resin (A) that satisfies requirements (a-1) to (a-3) described later; 10 to 100 parts by mass of a heat storage compound (B) having a flash point of 200° C. or higher (different from the component (A)); 1.5 to 20 parts by mass of a porous inorganic compound (C) having an oil absorption of 4.0 g / g or more, When the content of the porous inorganic compound (C) is 100 parts by mass, the content of the heat storage compound (B) is less than 700 parts by mass.
- thermoplastic resin (A) used in the present invention satisfies the following requirements (a-1) to (a-3).
- (a-1) Density measured according to the method described in ASTM D 1505 is in the range of 0.80 to 1.0 g/cm 3 .
- (a-2) Melt flow rate (MFR) measured at 230° C. under a load of 10 kg according to the method described in ISO 1133 is in the range of 0.1 to 100 g/10 min.
- Durometer A hardness (instantaneous value) measured according to the method described in ISO 7619 is in the range of 30-100.
- the density in requirement (a-1) is preferably 0.81-0.97 g/cm 3 , more preferably 0.82-0.94 g/cm 3 .
- the MFR in requirement (a-2) is preferably 0.5-80 g/10 min, more preferably 1-50 g/10 min.
- the moldability of the obtained resin composition is excellent.
- the durometer A hardness (instantaneous value) in requirement (a-3) is preferably 40-90, more preferably 40-85, even more preferably 40-80.
- the durometer A hardness (instantaneous value) of the thermoplastic resin (A) is within the above range, embrittlement hardly occurs even when the porous inorganic compound (C) is added within the specified range.
- thermoplastic resin (A) as described above is not particularly limited as long as it is a thermoplastic resin that satisfies the above requirements (a-1) to (a-3).
- resins polyester resins, polyvinyl chloride resins, polyamide resins, polycarbonate resins, polylactic acid resins, polyimide resins, polysulfone resins, aromatic polyketone resins, and the like. These resins can be used singly or in combination of two or more, and commercially available products may be used.
- olefinic resins are preferred, and olefinic thermoplastic elastomers are more preferred.
- olefinic thermoplastic elastomers include ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] having 3 to 20 carbon atoms (hereinafter referred to as “ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I ]”) and a dynamically crosslinked product of polyolefin resin [II].
- the dynamically crosslinked product may be one obtained by dynamically crosslinking one type each of the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] and the polyolefin resin [II].
- a non-conjugated polyene copolymer [I] or a plurality of polyolefin resins [II] may be dynamically crosslinked.
- the dynamic cross-linking means at least ethylene/ ⁇ -olefin/nonconjugated It means that part of the carbon-carbon double bonds of the polyene copolymer [I] is subjected to a cross-linking reaction.
- the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] comprises an ethylene-derived structural unit (a), an ⁇ -olefin-derived structural unit (b) having 3 to 20 carbon atoms, and a non-conjugated polyene-derived and the structural unit (c) of
- the content molar ratio (a)/(b) of the structural unit (a) and the structural unit (b) in the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] is 50/50 to 95/5.
- 60/40 to 80/20 is more preferable, and 65/35 to 75/25 is even more preferable.
- the specific amount of the structural unit (c) derived from the non-conjugated polyene in the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] is the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I ] with respect to the total amount of 2 to 20% by mass.
- ⁇ -olefin having 3 to 20 carbon atoms constituting the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] include propylene, 1-butene, 4-methyl-1-pentene, 1- hexene, 1-heptene, 1-octene, 1-nonene, 1-decene, 1-undecene, 1-dodecene, 1-tridecene, 1-tetradecene, 1-pentadecene, 1-hexadecene, 1-heptadecene, 1-nonadecene, 1-eicosene, 9-methyl-1-decene, 11-methyl-1-dodecene, 12-ethyl-1-tetradecene and the like are included.
- the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] may contain only one type of ⁇ -olefin-derived structural unit (b), or may contain two or more types thereof.
- non-conjugated polyene constituting the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] may be a compound that does not have a conjugated structure and has two or more carbon-carbon double bonds.
- 1,4-hexadiene 3-methyl-1,4-hexadiene, 4-methyl-1,4-hexadiene, 5-methyl-1,4-hexadiene, 4,5-dimethyl-1, chain nonconjugated dienes such as 4-hexadiene, 7-methyl-1,6-octadiene, 8-methyl-4-ethylidene-1,7-nonadiene, 4-ethylidene-1,7-undecadiene; methyltetrahydroindene, 5 -ethylidene-2-norbornene, 5-methylene-2-norbornene, 5-isopropylidene-2-norbornene, 5-vinylidene-2-norbornene, 6-chloromethyl-5-isopropenyl-2-norbornene, 5-vinyl- Cyclic non-conjugated dienes such as 2-norbornene, 5-isopropenyl-2-norbornene
- the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] may contain only one kind of structural unit (c) derived from non-conjugated polyene, or may contain two or more kinds thereof.
- the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] may be a so-called oil-extended rubber in which a softening agent, preferably a mineral oil-based softening agent is blended during its production.
- a softening agent preferably a mineral oil-based softening agent is blended during its production.
- Mineral oil-based softeners can be conventionally known mineral oil-based softeners, examples of which include paraffinic process oils and the like.
- the ethylene/ ⁇ -olefin/non-conjugated polyene copolymer [I] can be produced by a conventionally known method.
- the polyolefin resin [II] may be any polyolefin-based resin having substantially no unsaturated bonds in its main chain. Specific examples thereof include homopolymers of ⁇ -olefins such as ethylene, propylene, 1-butene, 1-pentene, 1-hexene, 4-methyl-1-pentene, 1-octene, and 1-decene; polymer; When the polyolefin resin [II] is a copolymer, the content of any one kind of ⁇ -olefin is preferably 90 mol % or more.
- the polyolefin resin [II] is particularly preferably a propylene-based polymer (II-1) containing propylene as a main component or an ethylene-based polymer (II-2) containing ethylene as a main component.
- propylene-based polymer (II-1) examples include homopolymers of propylene; - pentene, etc.); block copolymers of propylene homopolymers and amorphous or low-crystalline propylene/ethylene random copolymers; and the like.
- the amount of structural units other than propylene is preferably 10 mol % or less with respect to the total amount of structural units.
- the propylene-based polymer (II-1) may be polymerized by a known polymerization method, or may be manufactured and sold as a polypropylene resin.
- the propylene-based polymer (II-1) preferably has an isotactic structure, but a syndiotactic structure, a mixture of these structures, or a partial atactic structure. can be anything.
- examples of the ethylene-based polymer (II-2) include homopolymers of ethylene; -1-pentene, etc.).
- the amount of structural units other than ethylene is preferably 10 mol % or less based on the total amount of structural units.
- the ethylene-based polymer (II-2) may be one polymerized by a known polymerization method, and is manufactured and sold as high-pressure low-density polyethylene, linear low-density polyethylene, high-density polyethylene, or the like. There may be.
- the dynamic crosslinked product comprises the above-described ethylene/ ⁇ -olefin/nonconjugated polyene copolymer [I] and polyolefin resin [II], and, if necessary, a known cross-linking agent, It can be prepared by adding a cross-linking aid and a softening agent and kneading (dynamic cross-linking). Moreover, you may use a commercial item.
- a closed-type apparatus or an open-type apparatus may be used, but it is preferable to use a closed-type apparatus.
- Dynamic cross-linking is preferably carried out in an inert gas atmosphere such as nitrogen or carbon dioxide gas.
- the temperature for dynamic crosslinking is usually in the range from the melting point of the polyolefin resin [II] to 300°C, preferably 150 to 270°C, more preferably 170 to 250°C.
- the kneading time is preferably 1 to 20 minutes, more preferably 1 to 10 minutes.
- the shear rate at this time is preferably 10 to 50,000 sec -1 , more preferably 100 to 20,000 sec -1 .
- kneading devices used for dynamic cross-linking include mixing rolls, intensive mixers (e.g., Banbury mixers, kneaders), single-screw or twin-screw extruders, etc. Closed-type devices are preferred, and twin-screw extrusion machines are particularly preferred.
- the heat storage compound (B) used in the present invention is used as a phase transition material, and has a flash point of 200°C or higher, preferably 210°C or higher and 300°C or lower, more preferably 220°C or higher and 290°C or lower, further preferably 220°C or higher. °C or higher and 280 °C or lower (provided that they are compounds other than the component (A)).
- the flash point is within the above range, it can be contained in the resin composition without being thermally decomposed even when it is melt-kneaded with the component (A) at a high temperature of 200° C. or higher, and exhibits an excellent phase transition effect. be able to.
- the crystal melting heat amount ⁇ Hm of the heat storage compound (B) is preferably 150 J/g or more, more preferably 180 J/g or more and 300 J/g or less, still more preferably 210 J/g or more and 290 J/g or less, and particularly preferably 210 J/g. It is more than 280J/g or less. When the crystal melting heat quantity ⁇ Hm of the heat storage compound (B) is within the above range, the above effects are enhanced.
- Examples of the heat-storage compound (B) as described above include a chain structure that does not contain a cyclic or multiple bond and is not bulky, a structure that has a hydrocarbon, a structure that has a hydrogen bond unit such as a carbonyl group or a hydroxy group, and the like.
- a compound having More specifically, fatty acid esters, fatty alcohols, fatty acids, and the like can be mentioned. Of these, fatty acid esters are preferred, and fatty acid esters having chain-like substituents at both ends of the ester are more preferred.
- fatty acid esters examples include isocetyl myristate, octyldodecyl myristate, isocetyl isostearate, cetyl 2-ethylhexanoate, isocetyl stearate, 2-ethylhexyl palmitate, isotridecyl stearate, butyl stearate, dodecyl stearate, myristin
- the aliphatic alcohol preferably has 20 or more carbon atoms, such as behenyl alcohol, and the fatty acid preferably has 20 or more carbon atoms, such as behenic acid.
- the heat storage compound (B) can be appropriately selected depending on the desired phase transition temperature (heat retention temperature), and may be used singly or in combination of two or more.
- the oil absorption of the porous inorganic compound (C) used in the present invention is 4.0 g/g or more, preferably 4.5 g/g or more and 10.0 g/g or less, more preferably 5.0 g/g or more9. 5 g/g or less, more preferably 5.0 g/g or more and 9.0 g/g or less.
- a larger amount of the heat storage compound (B) can be retained. It is possible to suppress leaking bleed out.
- the average particle size of the porous inorganic compound (C) is preferably 1 ⁇ m or more and 100 ⁇ m or less. When the average particle size of the porous inorganic compound (C) is within the above range, the above effects are enhanced.
- the average particle size is a value measured by an apparatus and analysis method suitable for the particle size, for example, a value measured by a laser diffraction/scattering method.
- the porous inorganic compound (C) is not particularly limited as long as it is a porous inorganic compound having the above oil absorption, but from the viewpoint of having excellent heat resistance, examples include silica, alumina and carbon. These may be used individually by 1 type, or may use 2 or more types. Silica is preferable among the above, and hydrophobic silica is more preferable from the viewpoint of being able to further enhance the oil absorption effect.
- the porous inorganic compound (C) when the heat storage compound (B) is held at a temperature equal to or higher than the melting point (melting peak temperature) of the heat storage compound (B), the heat storage compound (B) is a single substance. As compared with the case of (1), it is preferable to use one that is less likely to volatilize and is less likely to catch fire. Examples of such a preferable porous inorganic compound (C) include "AEROS" manufactured by THILIUM.
- the content of each component in the resin composition of the present invention is, relative to 100 parts by mass of the thermoplastic resin (A),
- the content of the heat storage compound (B) is 10 to 100 parts by mass, preferably 12 to 80 parts by mass, more preferably 15 to 50 parts by mass
- the content of the porous inorganic compound (C) is 1.5 to 20 parts by mass, preferably 2.0 to 18 parts by mass, more preferably 2.5 to 16 parts by mass.
- the content of the porous inorganic compound (C) can be 1.5 parts by mass or more and less than 14 parts by mass, 2.0 parts by mass or more and less than 14 parts by mass, or 2.5 parts by mass or more and less than 14 parts by mass. .
- the content of the porous inorganic compound (C) is 100 parts by mass
- the content of the heat storage compound (B) is less than 700 parts by mass, preferably 100 parts by mass or more and less than 700 parts by mass, more preferably It is 200 parts by mass or more and less than 700 parts by mass.
- the heat storage compound (B) does not leak out (bleed out) from the resin when formed into a molded body, and a sufficient phase transition effect can be obtained.
- a compact having excellent brittleness and lightness can be obtained.
- the resin composition of the present invention contains optional components such as a slip agent, a nucleating agent, a filler, an antioxidant, a weather stabilizer, and a coloring agent (thermochromic material). ), foaming agents, pigments, dyes, antistatic agents, flame retardants and the like may be contained within a range that does not impair the effects of the present invention.
- thermoplastic resin (A), the heat storage compound (B), the porous inorganic compound (C), and optionally optional components are heated at 200°C or higher, preferably at 210°C. It has a step of kneading at a temperature of 300° C. or higher, more preferably 220° C. or higher and 260° C. or lower.
- the kneading time is usually 1 to 20 minutes, preferably 1 to 10 minutes.
- a mixing roll As a kneading device, a mixing roll, an intensive mixer (eg, Banbury mixer, kneader), a single-screw or twin-screw extruder, etc. can be used, but a non-open type device is preferable.
- an intensive mixer eg, Banbury mixer, kneader
- a single-screw or twin-screw extruder etc.
- a non-open type device is preferable.
- the molded article of the present invention comprises the resin composition of the present invention described above.
- Various known methods can be employed as the molding method. Specific examples include extrusion molding, press molding, injection molding, calender molding, blow molding, and the like. Further, a molded article such as a sheet obtained by the above molding method can be subjected to secondary processing such as thermoforming, or laminated with another material to obtain a molded article.
- the use of the molded article of the present invention is not particularly limited, but it is suitable for various known uses such as automobile parts, civil engineering and building materials, electrical and electronic parts, sanitary products, films and sheets, and foams.
- it is useful as a material for steering wheels and instrument panels, wearable materials, apparel materials, shoes, various cold insulating materials, cold insulating containers, heat insulating materials, and heat insulating containers, which become hot in cars in the summer.
- Thermoplastic resin> A-1 "Milastomer 6010NST” manufactured by Mitsui Chemicals, Inc. (crosslinked thermoplastic elastomer mainly composed of olefinic rubber (EPT) and olefinic resin (PP), density: 0.88 g/cm 3 , MFR (230°C, 10kg load): 12g/10min, durometer A hardness (instantaneous value): 70)
- A'-2 Polyvinyl chloride (density: 1.2 g/cm 3 , durometer A hardness (instantaneous value): 70)
- Examples 1 to 6 and Comparative Examples 1 to 14 Thermoplastic resin, heat storage compound (phase transition material) and porous inorganic material in the amounts (parts by mass) shown in Table 1 were heated to 240 using Laboplastomill ("80C100" manufactured by Toyo Seiki Seisakusho Co., Ltd.). °C and a torque rotation speed of 30 rpm for 5 minutes. After kneading, the kneaded material was quickly collected. The resulting kneaded product was finely cut with scissors to a size of about 0.5 cm ⁇ 0.5 cm ⁇ 0.5 cm.
- a Teflon (registered trademark) sheet and a mold were placed in this order on a stainless steel plate (hereinafter also referred to as "SUS plate"), and the cut material obtained above was spread over the holes of the mold. After spreading the cut material, the Teflon (registered trademark) sheet and the SUS plate were stacked in this order.
- the Teflon (registered trademark) sheet was used to prevent the kneaded material from sticking to the SUS plate during hot pressing.
- the mold used had a length of 6.5 cm, a width of 6.5 cm, and three thicknesses (1 mm, 2 mm, and 5 mm).
- the obtained laminate was hot-pressed for 5 minutes at a temperature of 240°C and a pressure of 10 MPa using a compression molding machine ("ASF-10" manufactured by Shindo Kinzoku Kogyo Co., Ltd.). After that, while sandwiched between SUS plates, it was quickly transferred to a compression molding machine (“NSF-37” manufactured by Shindo Kinzoku Kogyo Co., Ltd.) and cooled for 5 minutes at a pressure of 10 MPa. After cooling, the SUS plate and the Teflon (registered trademark) sheet were removed from the mold to obtain a heat-pressed sheet sample having the thickness shown in Table 1.
- the heat-pressed sheet samples produced were evaluated as follows.
- ⁇ Temperature rise rate and temperature drop rate both 3°C/min
- ⁇ Lightweight> The weight of the heat-pressed sheet sample obtained above was measured with a precision balance, and the density was obtained by dividing the weight by the volume of the obtained heat-pressed sheet. Based on the obtained density value, evaluation was made according to the following criteria. ⁇ : Less than 0.9 g/cm 3 ⁇ : 0.9 g/cm 3 or more and less than 1 g/cm 3 ⁇ : 1 g/cm 3 or more
- Examples 1 to 6 received a comprehensive evaluation of " ⁇ ", but all of the comparative examples received a result of "X”.
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Abstract
Description
引火点が200℃以上である蓄熱性化合物(B)(前記成分(A)とは異なる。)10~100質量部と、
吸油量が4.0g/g以上である多孔質無機化合物(C)1.5~20質量部と
を含み、
前記多孔質無機化合物(C)の含有量を100質量部とした場合、前記蓄熱性化合物(B)の含有量が700質量部未満である、樹脂組成物:
(a-1)ASTM D 1505に記載の方法に準拠して測定した密度が、0.80~1.0g/cm3の範囲である;
(a-2)ISO 1133に記載の方法に準拠して、230℃、10kg荷重で測定したメルトフローレート(MFR)が、0.1~100g/10minの範囲である;
(a-3)ISO 7619に記載の方法に準拠して測定したデュロメーターA硬度(瞬間値)が、30~100の範囲である。
[3] 前記多孔質無機化合物(C)が、シリカ、アルミナ、およびカーボンからなる群より選ばれる少なくとも1種の化合物である、項[1]または[2]に記載の樹脂組成物。
[5] 前記多孔質無機化合物(C)が疎水性シリカである、項[1]~[4]のいずれか1項に記載の樹脂組成物。
[7] 前記多孔質無機化合物(C)の含有量が1.5質量部以上14質量部未満である、項[1]~[6]のいずれか1項に記載の樹脂組成物。
[9] 項[1]~[7]のいずれか1項に記載の樹脂組成物の製造方法であって、熱可塑性樹脂(A)、蓄熱性化合物(B)および多孔質無機化合物(C)を、200℃以上の温度で混練する工程を有する、樹脂組成物の製造方法。
[樹脂組成物]
本発明に係る樹脂組成物は、
後述する要件(a-1)~(a-3)を満たす熱可塑性樹脂(A)100質量部と、
引火点が200℃以上である蓄熱性化合物(B)(前記成分(A)とは異なる。)10~100質量部と、
吸油量が4.0g/g以上である多孔質無機化合物(C)1.5~20質量部と
を含み、
前記多孔質無機化合物(C)の含有量を100質量部とした場合、前記蓄熱性化合物(B)の含有量が700質量部未満であることを特徴とする。
本発明で用いられる熱可塑性樹脂(A)は、下記要件(a-1)~(a-3)を満たす。
(a-1)ASTM D 1505に記載の方法に準拠して測定した密度が、0.80~1.0g/cm3の範囲である。
(a-2)ISO 1133に記載の方法に準拠して、230℃、10kg荷重で測定したメルトフローレート(MFR)が、0.1~100g/10minの範囲である。
(a-3)ISO 7619に記載の方法に準拠して測定したデュロメーターA硬度(瞬間値)が、30~100の範囲である。
エチレン・α-オレフィン・非共役ポリエン共重合体[I]は、エチレン由来の構成単位(a)と、炭素原子数3~20のα-オレフィン由来の構成単位(b)と、非共役ポリエン由来の構成単位(c)とを含む。
ポリオレフィン樹脂[II]は、実質的に主鎖に不飽和結合を有さないポリオレフィン系の樹脂であればよい。その具体例には、エチレン、プロピレン、1-ブテン、1-ペンテン、1-ヘキセン、4-メチル-1-ペンテン、1-オクテン、1-デセン等のα-オレフィンの単独重合体;これらの共重合体;が含まれる。なお、ポリオレフィン樹脂[II]が共重合体である場合、いずれか一種のα-オレフィンの含有量が90モル%以上であることが好ましい。
前記動的架橋体は、上述のエチレン・α-オレフィン・非共役ポリエン共重合体[I]およびポリオレフィン樹脂[II]と、必要に応じて、公知の架橋剤、架橋助剤および軟化剤を加え、混練(動的架橋)することにより調製することができる。また、市販品を用いてもよい。動的架橋する際には、非開放型の装置、開放型の装置のいずれを用いてもよいが、非開放型の装置を用いることが好ましい。
本発明で用いられる蓄熱性化合物(B)は、相転移材として用いられ、引火点が200℃以上、好ましくは210℃以上300℃以下、より好ましくは220℃以上290℃以下、さらに好ましくは220℃以上280℃以下の化合物である(ただし、前記成分(A)以外の化合物である。)。引火点が前記範囲であることにより、200℃以上の高温で成分(A)等とともに溶融混練しても熱分解することなく樹脂組成物に含有させることができ、優れた相転移効果を発揮することができる。
本発明で用いられる多孔質無機化合物(C)の吸油量は、4.0g/g以上、好ましくは4.5g/g以上10.0g/g以下、より好ましくは5.0g/g以上9.5g/g以下、さらに好ましくは5.0g/g以上9.0g/g以下である。多孔質無機化合物(C)の吸油量が前記範囲内であることにより、蓄熱性化合物(B)をより多く保持することができるため、成形体とした際に蓄熱性化合物(B)が樹脂から漏れだすブリードアウトを抑制することができる。
本発明の樹脂組成物における各成分の含有量は、熱可塑性樹脂(A)100質量部に対して、
蓄熱性化合物(B)の含有量は10~100質量部、好ましくは12~80質量部、より好ましくは15~50質量部であり、
多孔質無機化合物(C)の含有量は1.5~20質量部、好ましくは2.0~18質量部、より好ましくは2.5~16質量部である。また、多孔質無機化合物(C)の含有量を1.5質量部以上14質量部未満、2.0質量部以上14質量部未満または2.5質量部以上14質量部未満とすることもできる。
本発明の樹脂組成物は、上述した成分(A)~(C)以外に、任意成分として、スリップ剤、核剤、充填剤、酸化防止剤、耐候安定剤、着色剤(サーモクロミック材を含む)、発泡剤、顔料、染料、帯電防止剤、難燃剤等の添加剤を、本発明の効果を損なわない範囲で含有してもよい。
本発明の樹脂組成物の製造方法は、熱可塑性樹脂(A)、蓄熱性化合物(B)、多孔質無機化合物(C)、および必要に応じて任意成分を、200℃以上、好ましくは210℃以上300℃以下、より好ましくは220℃以上260℃以下の温度で混練する工程を有する。混練時間は、通常1~20分間、好ましくは1~10分間である。
本発明の成形体は、上述した本発明の樹脂組成物からなる。成形方法としては、種々公知の方法を採用することができる。具体的には、押出成形、プレス成形、射出成形、カレンダー成形、中空成形等が挙げられる。また、前記成形方法で得られたシートなどの成形体を熱成形などで二次加工、あるいは、他の材料と積層して成形体とすることもできる。
実施例および比較例で製造した樹脂組成物の各成分は以下のとおりである。
<熱可塑性樹脂>
・A-1:三井化学(株)製「ミラストマー6010NST」(オレフィン系ゴム(EPT)、オレフィン系樹脂(PP)を主成分とした架橋タイプの熱可塑性エラストマー、密度:0.88g/cm3、MFR(230℃、10kg荷重):12g/10min、デュロメーターA硬度(瞬間値):70)
・A’-2:ポリ塩化ビニル(密度:1.2g/cm3、デュロメーターA硬度(瞬間値):70)
・B-1:花王(株)製「エキセパールSS」(ステアリン酸ステアリル、引火点:258℃、ΔHm:234J/g)
・B-2:花王(株)製「エキセパールMY-M」(ミリスチン酸ミリスチル、引火点:239℃、ΔHm:229J/g)
・B-3:日油(株)製「スパームアセチ」(ミリスチン酸セチル、引火点:228℃、ΔHm:241J/g)
・B-4:日油(株)製「ユニスターM-2222SL」(ドコサン酸ドコシル、引火点:270℃、ΔHm:224J/g)
・B’-5:富士フイルム和光純薬(株)製「オクタデカン」(引火点:154℃)
・B’-6:三木理研工業(株)製メラミンカプセル「PMCD-28SP」(引火点:160℃)
・C-1:疎水性シリカ(THILIUM社製「AEROS」、吸油量:7g/g)
・C’-2:活性炭化物(谷口商会(株)製「スミレイ」、吸油量:3.4g/g)
表1に示す量(質量部)の熱可塑性樹脂、蓄熱性化合物(相転移材)および多孔質無機材料を、ラボプラストミル((株)東洋精機製作所製「80C100」)を用いて、温度240℃およびトルク回転数30rpmの条件で5分間混練した。混練後、速やかに混練物を回収した。得られた混練物を、ハサミで約0.5cm×0.5cm×0.5cmのサイズを目安に、細かく裁断した。
上記で得られた熱プレスシートサンプルの上下を、クリーンペーパーで、6.5cm×6.5cmの面とクリーンペーパーが平行になるように挟み、その上下をSUS板でさらに挟んだ後、圧縮成型機((株)神藤金属工業所製「ASF-10」)で、温度100℃および圧力10MPaの条件で5分間熱プレスを行った。熱プレス後、熱プレスシートサンプルを速やかにクリーンペーパーから剥がした。クリーンペーパーの状態を確認し、シートを置いたエリアに跡が無い場合は「〇:漏れなし」、跡がある場合は「×:漏れあり」と評価した。
上記で得られた熱プレスシートサンプルを、長さ1.0cm、幅6.5cmのサイズにカットして引張試験用の試験片とし、テンシロン万能試験機(形式:RTG-1225)を用いて、引張速度300mm/分およびチャック間距離50mmの条件で、試験片の引張伸びを測定した。試験片が破断した時の引張伸びの値に対して、伸び率(%)=伸び値(mm)/チャック間距離(mm)とし、測定された伸び率に基づいて、以下の基準で評価した。
〇:10%より大きい
△:5~10%
×:5%未満
上記で得られた熱プレスシートサンプルから約5mgを切り取り、示差走査熱量計(DSC)を用いて以下の条件で測定を行った。
・測定装置:X-DSC7000(SII製)
・温度:-40℃からスタートし、100℃まで昇温した後、100℃で1分間保持し、その後-40℃まで降温
・昇温速度および降温速度:いずれも3℃/分
・測定雰囲気:窒素
・前処理:無し
・パン:簡易密封パン
〇:50J/gより大きい
△:25~50J/g
×:25J/g未満
上記で得られた熱プレスシートサンプルの重量を精密天秤で測定し、得られた熱プレスシートの体積で割った値を密度とした。得られた密度の値に基づいて、以下の基準で評価した。
〇:0.9g/cm3未満
△:0.9g/cm3以上1g/cm3未満
×:1g/cm3以上
上記評価で、少なくとも1つ×があるものは総合評価を×(適さない)とした。
Claims (9)
- 下記要件(a-1)~(a-3)を満たす熱可塑性樹脂(A)100質量部と、
引火点が200℃以上である蓄熱性化合物(B)(前記成分(A)とは異なる。)10~100質量部と、
吸油量が4.0g/g以上である多孔質無機化合物(C)1.5~20質量部と
を含み、
前記多孔質無機化合物(C)の含有量を100質量部とした場合、前記蓄熱性化合物(B)の含有量が700質量部未満である、樹脂組成物:
(a-1)ASTM D 1505に記載の方法に準拠して測定した密度が、0.80~1.0g/cm3の範囲である;
(a-2)ISO 1133に記載の方法に準拠して、230℃、10kg荷重で測定したメルトフローレート(MFR)が、0.1~100g/10minの範囲である;
(a-3)ISO 7619に記載の方法に準拠して測定したデュロメーターA硬度(瞬間値)が、30~100の範囲である。 - 前記蓄熱性化合物(B)が脂肪酸エステルである、請求項1に記載の樹脂組成物。
- 前記多孔質無機化合物(C)が、シリカ、アルミナ、およびカーボンからなる群より選ばれる少なくとも1種の化合物である、請求項1または2に記載の樹脂組成物。
- 前記多孔質無機化合物(C)の吸油量が4.5g/g以上10.0g/g以下である、請求項1~3のいずれか1項に記載の樹脂組成物。
- 前記多孔質無機化合物(C)が疎水性シリカである、請求項1~4のいずれか1項に記載の樹脂組成物。
- 前記蓄熱性化合物(B)の結晶融解熱量ΔHmが150J/g以上である、請求項1~5のいずれか1項に記載の樹脂組成物。
- 前記多孔質無機化合物(C)の含有量が1.5質量部以上14質量部未満である、請求項1~6のいずれか1項に記載の樹脂組成物。
- 請求項1~7のいずれか1項に記載の樹脂組成物からなる成形体。
- 請求項1~7のいずれか1項に記載の樹脂組成物の製造方法であって、熱可塑性樹脂(A)、蓄熱性化合物(B)および多孔質無機化合物(C)を、200℃以上の温度で混練する工程を有する、樹脂組成物の製造方法。
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