WO2019159804A1 - 粒状核剤、樹脂組成物、成形品およびその製造方法 - Google Patents
粒状核剤、樹脂組成物、成形品およびその製造方法 Download PDFInfo
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- WO2019159804A1 WO2019159804A1 PCT/JP2019/004405 JP2019004405W WO2019159804A1 WO 2019159804 A1 WO2019159804 A1 WO 2019159804A1 JP 2019004405 W JP2019004405 W JP 2019004405W WO 2019159804 A1 WO2019159804 A1 WO 2019159804A1
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- Prior art keywords
- nucleating agent
- granular nucleating
- resin composition
- particle size
- granular
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- 239000002280 amphoteric surfactant Substances 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 238000003287 bathing Methods 0.000 description 1
- 229910052790 beryllium Inorganic materials 0.000 description 1
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- SECPZKHBENQXJG-UHFFFAOYSA-N cis-palmitoleic acid Natural products CCCCCCC=CCCCCCCCC(O)=O SECPZKHBENQXJG-UHFFFAOYSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000000113 cyclohexyl group Chemical group [H]C1([H])C([H])([H])C([H])([H])C([H])(*)C([H])([H])C1([H])[H] 0.000 description 1
- 235000020669 docosahexaenoic acid Nutrition 0.000 description 1
- 229940090949 docosahexaenoic acid Drugs 0.000 description 1
- JAZBEHYOTPTENJ-UHFFFAOYSA-N eicosapentaenoic acid Natural products CCC=CCC=CCC=CCC=CCC=CCCCC(O)=O JAZBEHYOTPTENJ-UHFFFAOYSA-N 0.000 description 1
- 235000020673 eicosapentaenoic acid Nutrition 0.000 description 1
- 229960005135 eicosapentaenoic acid Drugs 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- FARYTWBWLZAXNK-WAYWQWQTSA-N ethyl (z)-3-(methylamino)but-2-enoate Chemical compound CCOC(=O)\C=C(\C)NC FARYTWBWLZAXNK-WAYWQWQTSA-N 0.000 description 1
- 229920001038 ethylene copolymer Polymers 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000009408 flooring Methods 0.000 description 1
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- 239000004088 foaming agent Substances 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- VZCCETWTMQHEPK-UHFFFAOYSA-N gamma-Linolensaeure Natural products CCCCCC=CCC=CCC=CCCCCC(O)=O VZCCETWTMQHEPK-UHFFFAOYSA-N 0.000 description 1
- VZCCETWTMQHEPK-QNEBEIHSSA-N gamma-linolenic acid Chemical compound CCCCC\C=C/C\C=C/C\C=C/CCCCC(O)=O VZCCETWTMQHEPK-QNEBEIHSSA-N 0.000 description 1
- 235000020664 gamma-linolenic acid Nutrition 0.000 description 1
- 229960002733 gamolenic acid Drugs 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 229910052735 hafnium Inorganic materials 0.000 description 1
- VBJZVLUMGGDVMO-UHFFFAOYSA-N hafnium atom Chemical compound [Hf] VBJZVLUMGGDVMO-UHFFFAOYSA-N 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002366 halogen compounds Chemical class 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000003505 heat denaturation Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 125000003187 heptyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000012770 industrial material Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 125000000959 isobutyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])* 0.000 description 1
- 125000001972 isopentyl group Chemical group [H]C([H])([H])C([H])(C([H])([H])[H])C([H])([H])C([H])([H])* 0.000 description 1
- 229920003049 isoprene rubber Polymers 0.000 description 1
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000004611 light stabiliser Substances 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229940127554 medical product Drugs 0.000 description 1
- 150000007974 melamines Chemical class 0.000 description 1
- 239000006078 metal deactivator Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 125000000740 n-pentyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 125000001196 nonadecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 235000021313 oleic acid Nutrition 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 239000004014 plasticizer Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920002857 polybutadiene Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920001610 polycaprolactone Polymers 0.000 description 1
- 239000004632 polycaprolactone Substances 0.000 description 1
- 229920005668 polycarbonate resin Polymers 0.000 description 1
- 239000004431 polycarbonate resin Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000004626 polylactic acid Substances 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920005672 polyolefin resin Polymers 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 229920001021 polysulfide Polymers 0.000 description 1
- 239000011118 polyvinyl acetate Substances 0.000 description 1
- 229920002689 polyvinyl acetate Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 229910052705 radium Inorganic materials 0.000 description 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 description 1
- 238000001175 rotational moulding Methods 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000007493 shaping process Methods 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 239000000344 soap Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- JIWBIWFOSCKQMA-UHFFFAOYSA-N stearidonic acid Natural products CCC=CCC=CCC=CCC=CCCCCC(O)=O JIWBIWFOSCKQMA-UHFFFAOYSA-N 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003856 thermoforming Methods 0.000 description 1
- 229920001169 thermoplastic Polymers 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 150000003568 thioethers Chemical class 0.000 description 1
- 150000003606 tin compounds Chemical class 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- XKZKQTCECFWKBN-UHFFFAOYSA-N trans-4-decenoic acid Natural products CCCCCC=CCCC(O)=O XKZKQTCECFWKBN-UHFFFAOYSA-N 0.000 description 1
- UWHZIFQPPBDJPM-BQYQJAHWSA-N trans-vaccenic acid Chemical compound CCCCCC\C=C\CCCCCCCCCC(O)=O UWHZIFQPPBDJPM-BQYQJAHWSA-N 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 125000002469 tricosyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/53—Phosphorus bound to oxygen bound to oxygen and to carbon only
- C08K5/5317—Phosphonic compounds, e.g. R—P(:O)(OR')2
- C08K5/5333—Esters of phosphonic acids
- C08K5/5357—Esters of phosphonic acids cyclic
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/6564—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms
- C07F9/6571—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having phosphorus atoms, with or without nitrogen, oxygen, sulfur, selenium or tellurium atoms, as ring hetero atoms having phosphorus and oxygen atoms as the only ring hetero atoms
- C07F9/6574—Esters of oxyacids of phosphorus
- C07F9/65744—Esters of oxyacids of phosphorus condensed with carbocyclic or heterocyclic rings or ring systems
-
- 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
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/003—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor characterised by the choice of material
-
- 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
- C08K5/49—Phosphorus-containing compounds
- C08K5/51—Phosphorus bound to oxygen
- C08K5/52—Phosphorus bound to oxygen only
- C08K5/527—Cyclic esters
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L101/00—Compositions of unspecified macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
-
- 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
- C08K2201/003—Additives being defined by their diameter
-
- 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
- C08K2201/016—Additives defined by their aspect ratio
-
- 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
- C08K5/0008—Organic ingredients according to more than one of the "one dot" groups of C08K5/01 - C08K5/59
- C08K5/0083—Nucleating agents promoting the crystallisation of the polymer matrix
Definitions
- the present invention relates to a granular nucleating agent, a resin composition, a molded product, and a method for producing the same.
- Patent Document 1 discloses a crystal nucleating agent having an average particle size of 0.001 to 3.0 ⁇ m in crystalline polylactic acid (hereinafter, nucleating agents such as a crystal nucleating agent and a crystallization accelerator are collectively referred to as “nucleating agent”. (Referred to as claims 1 and 3 in Patent Document 1).
- a general nucleating agent is a granular material (granular nucleating agent) obtained by mixing (kneading) each raw material component, drying, and then pulverizing as necessary.
- the particulate nucleating agent is melt-kneaded with a thermoplastic resin such as a crystalline polymer, and used for thermoforming the thermoplastic resin.
- a thermoplastic resin such as a crystalline polymer
- Such dust workability is required not only in the process of manufacturing, transporting and storing granular nucleating agents, but also in the production of mixed products (compositions) and thermoplastic resins using such granular nucleating agents, and mass production of these. It is what is done.
- the present inventor conducted research based on such development circumstances.By controlling the dust characteristics of the granular nucleating agent under mild pulverization conditions, dust workability is improved, and coarse particles are cut by combing. It was found that the transparency can be improved. As a result of further intensive studies, it was possible to stably evaluate the dust workability and transparency by using the dispersion degree and maximum particle size of the granular nucleating agent as an index. It has been found that by controlling the upper limit of the diameter to a predetermined value or less, dust workability and transparency can be improved, and the present invention has been completed.
- a granular nucleating agent containing a compound represented by the following general formula (1) Using a laser diffraction particle size distribution measurement method, the particle size distribution of the granular nucleating agent is dry measured, and the maximum particle size of the granular nucleating agent is defined as Dmax , When the degree of dispersion of the granular nucleating agent is measured according to the following procedure was D p, A granular nucleating agent is provided in which D max satisfies the following formula (A) and D p satisfies the following formula (B).
- Formula (A) 1.0% ⁇ D p ⁇ 27.0%
- Formula (B) (procedure)
- a predetermined amount of granular nucleating agent is prepared as a sample.
- the sample is put into a cylinder from a height of 60 cm, and the sample is dropped in the vertical direction inside the cylinder. Then, the amount of the sample remaining on the watch glass installed at the dropping point is measured.
- the dispersity (%) is measured based on the following equation using the amount of sample charged and the amount of sample remaining in the watch glass.
- Dispersity (%) [(input sample amount (g) ⁇ sample amount remaining in watch glass (g)) / input sample amount (g)] ⁇ 100
- R 1 to R 4 each independently represents a hydrogen atom, a linear or branched alkyl group having 1 to 9 carbon atoms
- R 5 represents a hydrogen atom or carbon number 1 Represents an alkyl group of ⁇ 4
- m represents 1 or 2
- M 1 represents a hydrogen atom, Al (OH) 2 or an alkali metal atom
- M 1 is Represents a group II element, Al (OH) or Zn.
- the inventor conducted research based on such development circumstances, and found that the dust characteristics can be controlled by appropriately adjusting the particle size profile in the granular nucleating agent. As a result of further intensive studies, it is possible to improve the dust workability by appropriately controlling the upper limit and the lower limit of the maximum particle diameter Dmax within a predetermined range of the volume average particle diameter MV as a particle diameter profile. As a result, the inventors have found that the transparency can be obtained.
- a granular nucleating agent containing the compound represented by the general formula (1) Using the laser diffraction particle size distribution measurement method, the particle size distribution of the granular nucleating agent is dry measured, and the maximum particle size of the granular nucleating agent is D max and the volume average particle size is MV, A granular nucleating agent is provided in which D max satisfies the following formula (A) and MV satisfies the following formula (C). 80 ⁇ m ⁇ D max ⁇ 300 ⁇ m Formula (A) 5 ⁇ m ⁇ MV ⁇ 100 ⁇ m Formula (C)
- thermoplastic resin a resin composition comprising the above granular nucleating agent in a thermoplastic resin.
- a production method for producing a molded product using the resin composition is provided.
- a granular nucleating agent excellent in dust workability and transparency, a resin composition using the same, a molded article, and a method for producing the same are provided.
- the granular nucleating agent of this embodiment will be described.
- the particulate nucleating agent contains an aromatic phosphate metal salt.
- aromatic phosphate metal salt a compound represented by the following general formula (1) is used. These may be used alone or in combination of two or more.
- R 1 to R 4 each independently represents a hydrogen atom, a linear or branched alkyl group having 1 to 9 carbon atoms, and R 5 represents a hydrogen atom or 1 to carbon atoms.
- 4 represents an alkyl group, m represents 1 or 2, and when m is 1, M 1 represents a hydrogen atom, Al (OH) 2 or an alkali metal atom, and when m is 2, M 1 is Represents a group II element, Al (OH) or Zn.
- Examples of the alkyl group having 1 to 9 carbon atoms represented by R 1 , R 2 , R 3 and R 4 in the general formula (1) include, for example, a methyl group, an ethyl group, a propyl group, and an isopropyl group.
- examples of the alkali metal represented by M 1 include sodium (Na), potassium (K), and lithium (Li).
- Be beryllium
- Mg magnesium
- Ca calcium
- strontium Sr
- Ba barium
- Ra radium
- those which are magnesium and calcium are preferred because the nucleating agent effect of the nucleating agent component is remarkable.
- a compound in which m is 1 is preferable.
- a compound in which R 1 , R 2 , R 3 and R 4 have a single group selected from the group consisting of a methyl group, an ethyl group, a sec-butyl group and a tert-butyl group is preferable.
- a compound in which R 5 is a hydrogen atom or a methyl group is particularly preferable.
- the compound represented by the general formula (1) preferably includes one or more compounds represented by any one of the following chemical formulas (2) to (15).
- a compound represented by any one of the chemical formulas (2) to (6) is preferable.
- a compound represented by any one of the chemical formulas (7) to (15) is preferable.
- phosphorus trichloride or phosphorus oxychloride
- 2,2′-alkylidenephenol is hydrolyzed as necessary.
- a cyclic acidic phosphate ester is reacted with a metal hydroxide such as sodium hydroxide or potassium hydroxide, and the resulting reaction product is appropriately purified (filtered, etc.) and dried to obtain the above compound.
- Aromatic phosphate metal salt may be synthesized by a conventionally known method and used as the above compound.
- the obtained compound is dissolved in a solvent and reacted with another metal hydroxide such as lithium hydroxide, or reacted with a salt of any one of aluminum, magnesium and group II elements, and the obtained reaction product. Is purified and dried to obtain another compound described above.
- another metal hydroxide such as lithium hydroxide
- a salt of any one of aluminum, magnesium and group II elements Is purified and dried to obtain another compound described above.
- the granular nucleating agent of the present embodiment can be obtained by pulverizing the obtained compound with an appropriate pulverizing means, if necessary.
- coarse particles may be excluded by sieving with a sieve having a predetermined mesh size.
- the said granular nucleating agent can contain 1 type, or 2 or more types of powdery compounds.
- the above-mentioned granular nucleating agent may be obtained by blending two or more compounds having different particle size distributions or two or more classified compounds in combination at an appropriate ratio.
- Examples of the pulverizing means include, for example, a mortar, ball mill, rod mill, tube mill, conical mill, vibration ball mill, high swing ball mill, roller mill, pin mill, hammer mill, attrition mill, jet mill, jet mizer, micronizer, nanomizer, Examples include a Macjack mill, a micro atomizer, a colloid mill, a premier colloid mill, a micron mill, a Charlotte colloid mill, a rotary cutter, and a dry medium agitation mill. These pulverizers can be used alone or in combination of two or more, and are appropriately selected depending on the type of raw material powder to be pulverized, the pulverization time, and the like.
- the granular nucleating agent of the present embodiment may be composed only of the compound represented by the general formula (1), and may contain other components within the scope of achieving the object of the present invention.
- the other components include aromatic phosphate metal salts, fatty acid metal salts, silicic acid-based inorganic additive components, hydrotalcites, and the like other than the compound represented by the general formula (1). These may be used alone or in combination of two or more.
- the fatty acid metal salt preferably contains a compound represented by the following general formula (16).
- R 6 represents a linear or branched aliphatic group having 9 to 30 carbon atoms
- M represents a metal atom
- n represents an integer of 1 to 4
- It represents an integer corresponding to the valence of the metal atom.
- R 6 represents a linear or branched aliphatic group having 9 to 30 carbon atoms, such as an alkyl group or alkenyl group having 9 to 30 carbon atoms, which is a hydroxyl group. May be substituted.
- Examples of the aliphatic group having 9 to 30 carbon atoms include capric acid, 2-ethylhexanoic acid, undecyl acid, lauric acid, tridecylic acid, myristic acid, pentadecylic acid, palmitic acid, margaric acid, stearic acid, and nonadecyl.
- Acids arachidic acid, heicosyl acid, behenic acid, tricosyl acid, lignoceric acid, serotic acid, montanic acid, melicic acid and other saturated fatty acids, 4-decenoic acid, 4-dodecenoic acid, palmitoleic acid, ⁇ -linolenic acid, linoleic acid , Linear unsaturated fatty acids such as ⁇ -linolenic acid, stearidonic acid, petrothelic acid, oleic acid, elaidic acid, vaccenic acid, eicosapentaenoic acid, docosapentaenoic acid and docosahexaenoic acid.
- the fatty acid metal salt preferably has an aliphatic group represented by R 6 having 10 to 21 carbon atoms, and in particular, lauric acid, myristic acid, palmitic acid, stearic acid, behenic acid, oleic acid, 12 -Hydroxystearic acid is preferred.
- Examples of the metal atom represented by M include alkali metal, magnesium, calcium, strontium, barium, titanium, manganese, iron, zinc, silicon, zirconium, yttrium, barium or hafnium.
- alkali metals such as sodium, lithium and potassium are preferable, and sodium and lithium are particularly preferably used since the crystallization temperature becomes high.
- silicate-based inorganic additive component examples include fumed silica, fine particle silica, silica, diatomaceous earth, clay, kaolin, silica gel, calcium silicate, sericite, kaolinite, flint, feldspar powder, meteorite, attapulgite, Examples include talc, mica, minnesite, and pyrophyllite. Among them, those having a particle structure of a layered structure and those having a silicon content of 15% by mass or more are preferable. Examples of these preferable inorganic additives include sericite, kaolinite, talc, mica, minnesotite, and pyrophyllite, and talc and mica are more preferable.
- the hydrotalcites may be, for example, natural products or synthetic products, and can be used regardless of the presence or absence of surface treatment or the presence or absence of crystal water.
- the basic carbonate represented by the following general formula is mentioned.
- M x Mg y Al z CO 3 (OH) xp + 2y + 3z-2 ⁇ nH 2 O (In the above general formula, M represents an alkali metal or zinc, X represents a number from 0 to 6, y represents a number from 0 to 6, z represents a number from 0.1 to 4, and p represents M Where n represents the number of water of crystallization from 0 to 100)
- the granular nucleating agent containing the other component is a granular nucleating agent composition containing the compound represented by the general formula (1), and other aromatic phosphate metal salt, fatty acid metal salt, silicic acid type One or more selected from the group consisting of inorganic additive components and hydrotalcites, preferably one or more selected from the group consisting of fatty acid metal salts, talc, mica and hydrotalcites .
- Such a granular nucleating agent can be obtained, for example, by pulverizing by appropriately combining the above pulverizing means in the presence of the compound represented by the general formula (1) and other components.
- pulverization means, sieving, the blending method, etc. can also be used.
- the granular nucleating agent of the present embodiment functions as a nucleating agent / translucent agent added at the time of molding a thermoplastic resin such as a crystalline polymer.
- a thermoplastic resin such as a crystalline polymer.
- improvement (modification effect) such as crystallization temperature, heat denaturation temperature, flexural modulus, hardness, and transparency can be realized. Further, the molding cycle property can be improved and the productivity can be improved.
- the granular nucleating agent of the first embodiment includes the compound represented by the general formula (1), and the particle size distribution of the granular nucleating agent is measured by dry measurement using a laser diffraction particle size distribution measuring method.
- D max the maximum particle diameter of the granular nucleating agent
- D p the degree of dispersion of the granular nucleating agent measured according to the following procedure
- D max satisfies the following formula (A)
- Formula (A) 1.0% ⁇ D p ⁇ 27.0%
- Formula (B) (procedure)
- a predetermined amount of granular nucleating agent is prepared as a sample.
- the sample is put into a cylinder from a height of 60 cm, and the sample is dropped in the vertical direction inside the cylinder. Then, the amount of the sample remaining on the watch glass installed at the dropping point is measured.
- the dispersity (%) is measured based on the following equation using the amount of sample charged and the amount of sample remaining in the watch glass.
- the predetermined amount may be about 5 g
- the degree of dispersion may be an average value of three measurement values.
- Dispersity (%) [(input sample amount (g) ⁇ sample amount remaining in watch glass (g)) / input sample amount (g)] ⁇ 100
- the particle size of the granular nucleating agent be smaller.
- dust workability may be deteriorated. Therefore, the pulverization conditions were changed to relatively mild conditions in the process of reducing the particle size of the granular nucleating agent.
- dust workability is improved, large particles may be mixed into the granular nucleating agent, which may reduce transparency.
- the explosion index is usually an index for evaluating the dust explosibility of the powder. Even when the explosion index is low enough for practical use, it has been found that there is room for improvement in workability such as handling of the granular nucleating agent during scale-up. And it was found that by using such an explosion index and maximum explosion pressure as a guideline and lowering it, the dust characteristics at the time of scale-up can be suppressed, and the workability of the granular nucleating agent can be improved.
- measurement stability can be improved because there are no problems such as bubbles compared to wet conditions.
- the upper limit of the maximum particle diameter Dmax is 300 ⁇ m or less, preferably 295 ⁇ m or less, more preferably 290 ⁇ m or less. Thereby, the transparency of a granular nucleating agent can be improved.
- the lower limit of D max is, for example, 80 ⁇ m or more, preferably 83 ⁇ m or more, and more preferably 85 ⁇ m or more. Thereby, various physical properties can be balanced.
- the upper limit of the degree of dispersion D p for example 27.0% or less, preferably 26.8% or less, more preferably less 26.5%.
- operativity such as the dust workability
- the lower limit of D p is, for example, 1.0% or more, preferably 3.0% or more, more preferably 5.0% or more. It is possible to balance various physical properties.
- the granular nucleating agent of the second embodiment contains the compound represented by the general formula (1), and the particle size distribution of the granular nucleating agent is determined using a laser diffraction particle size distribution measuring method.
- D max satisfies the following formula (A)
- MV satisfies the following formula (C). . 80 ⁇ m ⁇ D max ⁇ 300 ⁇ m Formula (A) 5 ⁇ m ⁇ MV ⁇ 100 ⁇ m Formula (C)
- the volume average particle diameter MV is, for example, 5 ⁇ m to 100 ⁇ m, preferably 6 ⁇ m to 95 ⁇ m, more preferably 7 ⁇ m to 90 ⁇ m.
- ⁇ means that an upper limit value and a lower limit value are included unless otherwise specified.
- the upper limit of the maximum particle diameter Dmax is 300 ⁇ m or less, preferably 295 ⁇ m or less, more preferably 290 ⁇ m or less.
- the lower limit of D max is, for example, 80 ⁇ m or more, preferably 83 ⁇ m or more, and more preferably 85 ⁇ m or more.
- the transparency of the granular nucleating agent can be improved by keeping the volume average particle size MV within the above range and setting the upper limit of the maximum particle size D max to the above or below.
- the workability such as the dust workability of the granular nucleating agent and the handling property of the granular nucleating agent at the time of scale-up can be improved.
- the granular nucleating agent is preferably acicular particles.
- the aspect ratio of the granular nucleating agent at this time is, for example, 1.5 or more and 10 or less, preferably 2.0 or more and 8 or less, more preferably 2.5 or more and 6 or less.
- the aspect ratio of the granular nucleating agent is calculated from the average of the major axis / minor axis by measuring the lengths of the major axis and the minor axis of 100 crystals randomly from a micrograph.
- the pulverization conditions such as the pulverization method and the pulverization time, the classification conditions such as the cutting of coarse particles, and the like, the maximum particle size, dispersity, volume average particle of the above-mentioned granular nucleating agent It is mentioned as an element for making a diameter and an aspect ratio into a desired numerical range.
- the resin composition of this embodiment contains the above-described granular nucleating agent in a thermoplastic resin.
- the method of adding the granular nucleating agent to the thermoplastic resin is not particularly limited, and a generally used method can be applied as it is. For example, a method of dry blending a powder or pellets of a thermoplastic resin and a powder of the granular nucleating agent can be used.
- the resin composition can be used in various forms.
- the resin composition may be in the form of pellets, granules, or powders. From the viewpoint of handleability, a pellet shape is preferable.
- thermoplastic resin examples include polyolefin resins, styrene resins, polyester resins, polyether resins, polycarbonate resins, polyamide resins, and halogen-containing resins. Among these, it is preferable to use a crystalline polymer.
- thermoplastic resin examples include, for example, petroleum resin, coumarone resin, polyvinyl acetate, acrylic resin, polymethyl methacrylate, polyvinyl alcohol, polyvinyl formal, polyvinyl butyral, polyphenylene sulfide, polyurethane, fiber-based resin, polyimide Resins, polysulfone, thermoplastic resins such as liquid crystal polymers, and blends thereof can be used.
- thermoplastic resins include isoprene rubber, butadiene rubber, acrylonitrile-butadiene copolymer rubber, styrene-butadiene copolymer rubber, polyester elastomer, nitrile elastomer, nylon elastomer, vinyl chloride elastomer, polyamide elastomer, polyurethane. May be a thermoplastic elastomer such as a base elastomer, or may be used in combination.
- the crystalline polymer is not particularly limited, but for example, polypropylene, high density polyethylene, low density polyethylene, linear low density polyethylene, polybutene-1, poly-3-methylpentene, poly-4-methylpentene, ethylene / propylene block Or polyolefin polymers such as ⁇ -olefin polymers such as random copolymers; thermoplastic linear polyester polymers such as polyethylene terephthalate, polybutylene terephthalate, polyhexamethylene terephthalate; polysulfide polymers such as polyphenylene sulfide; Examples thereof include polylactic acid polymers such as polycaprolactone; linear polyamide polymers such as polyhexamethylene adipamide; crystalline polystyrene polymers such as syndiotactic polystyrene.
- polyolefin-based polymers in which the effect of using the nucleating agent of the present invention is remarkably exhibited are preferable.
- Polypropylene resins such as a mixture of these propylene polymers and other ⁇ -olefin polymers are particularly preferable.
- a crystalline ⁇ -olefin polymer particularly polypropylene resin such as polypropylene, ethylene / propylene copolymer and a mixture of these propylene polymer and other ⁇ -olefin polymer is used as the crystalline polymer.
- polypropylene resin such as polypropylene, ethylene / propylene copolymer and a mixture of these propylene polymer and other ⁇ -olefin polymer is used as the crystalline polymer.
- polypropylene resins can be used regardless of their intrinsic viscosity, isometatic pentad fraction, density, molecular weight distribution, melt flow rate, rigidity, etc., for example, JP-A-63-37148, 63-37152, 63-90552, 63-210152, 63-213547, 63-243150, 63-243152, 63-260943, 63-260944, 63-264650, JP-A-1-178541, 2-49047, 2-102242, 2-251548, 2-279746, Polypropylene resins such as those described in Kaihei 3-195551 are also suitable. That.
- the content of the particulate nucleating agent is usually 0.001 to 10 parts by weight, preferably 0.005 to 8 parts by weight, with respect to 100 parts by weight of the thermoplastic resin (eg, crystalline polymer). More preferably, it can be in the range of 0.01 to 5 parts by weight. Thereby, the modification effect of the thermoplastic resin, particularly the crystalline polymer can be sufficiently obtained.
- the thermoplastic resin eg, crystalline polymer
- the resin composition of the present embodiment includes an antioxidant, a light stabilizer, an ultraviolet absorber, a pigment, a filler, an organic tin compound, a plasticizer, an epoxy compound, a foaming agent, an antistatic agent, a difficult agent.
- Additives such as flame retardants, lubricants, heavy metal deactivators, hydrotalcites, organic carboxylic acids, colorants, silicic acid-based additives and processing aids can be included. These may be used alone or in combination of two or more.
- the antioxidant include phosphorus antioxidants, phenol antioxidants, and thioether antioxidants.
- Examples of the antistatic agent include a cationic surfactant, an anionic surfactant, a nonionic surfactant, and an amphoteric surfactant.
- Examples of the flame retardant include halogen compounds, phosphate ester compounds, phosphate amide compounds, melamine compounds, melamine salt compounds of polyphosphoric acid, fluororesins or metal oxides.
- Examples of the lubricant include hydrocarbons, fatty acids, aliphatic alcohols, aliphatic esters, aliphatic amides, metal soaps, and the like.
- Fumed silica fine particle silica, silica, diatomaceous earth, clay, kaolin, silica gel, calcium silicate, sericite, kaolinite, flint, feldspar powder, meteorite, attapulgite, talc, mica, minnesota And pyrophyllite.
- the content of the additive in the resin composition is preferably 0.001 to 10 parts by weight with respect to 100 parts by weight of the crystalline polymer. By setting it as such a numerical range, the improvement of the effect of an additive is acquired.
- the resin composition is an injection molded product, fiber, flat yarn, biaxially stretched film, uniaxially stretched film, unstretched film, sheet, thermoformed product, extrusion blow molded product, injection blow molded product, injection stretch blow molded product, It can be used for molded products such as profile extrusion molded products and rotational molded products.
- a molded product an injection molded product, a film, a sheet, and a thermoformed product are preferable.
- the manufacturing method of the molded article of this embodiment includes the process of shape
- the molding method is not particularly limited, and is an injection molding method, extrusion molding method, blow molding method, rotational molding, vacuum molding method, inflation molding method, calendar molding method, slush molding method, dip molding method, foam molding method. Law. Among these, the injection molding method, the extrusion molding method, and the blow molding method are preferable.
- the resin composition can be used for various applications such as building materials, agricultural materials, automobile parts, trains, ships, aircrafts and other vehicle parts, packaging materials, sundries, toys, home appliances, and medical products.
- automotive parts such as bumpers, dashboards, instrument panels, battery cases, luggage cases, door panels, door trims, fender liners; resin parts for household appliances such as refrigerators, washing machines, vacuum cleaners; tableware, bottles Household goods such as caps, buckets, bathing goods, etc .; resin parts for connection such as connectors; miscellaneous goods such as toys, storage containers, synthetic papers; medical packs, syringes, catheters, medical tubes, syringe preparations, infusion bags, reagents Medical molded products such as containers, pill containers, and individual pill packaging; building materials such as walls, flooring, window frames, wallpaper, and windows; wire covering materials; agricultural materials such as houses, tunnels, and flat yarn mesh bags Pallets, pail cans, back grind tapes, LCD protective tapes, pipes, modified silicone polymers for sealing materials
- low temperature plasma after molding to improve surface properties such as application for various post-treatments, for example, medical applications, food packaging applications, sterilization by radiation, or paintability. It can be used for purposes such as processing. Among these, it is preferable to use for automobile parts, household goods, and food packaging materials.
- a granular nucleating agent comprising a compound represented by the following general formula (1),
- R 1 to R 4 each independently represents a hydrogen atom, a linear or branched alkyl group having 1 to 9 carbon atoms, and R 5 represents a hydrogen atom or carbon number 1 Represents an alkyl group of ⁇ 4, m represents 1 or 2, when m is 1, M 1 represents a hydrogen atom or an alkali metal atom, and when m is 2, M 1 represents a group 2 element, Al ( OH) or Zn.) 2.
- a granular nucleating agent according to claim 1 The granular nucleating agent has an aspect ratio of 1.5 or more and 10 or less. 3.
- a granular nucleating agent according to claim 1 The compound is represented by the following formula No. 1 to formula no.
- a granular nucleating agent comprising one or more compounds represented by any one of 12 above. 4).
- a crystalline polymer composition comprising the granular nucleating agent according to any one of the above in a crystalline polymer. 5. 4).
- a crystalline polymer composition according to claim 1, A crystalline polymer composition, wherein the crystalline polymer comprises a polyolefin polymer. 6). 4).
- a crystalline polymer composition according to claim 1, A crystalline polymer composition, wherein the content of the granular nucleating agent is 0.001 part by weight or more and 10 parts by weight or less with respect to 100 parts by weight of the crystalline polymer. 7). 4).
- Test Example 1 The obtained Compound No. 1 was sieved with a sieve having a mesh size of 355 ⁇ m without pulverization to obtain a granular nucleating agent A.
- Test Example 2 The obtained Compound No. 1 was pulverized with a ball mill for 30 minutes and sieved with a sieve having a mesh size of 355 ⁇ m to obtain a granular nucleating agent B.
- volume average particle diameter, maximum particle diameter The volume average particle size MV and the maximum particle size D max were measured using a laser diffraction particle size distribution analyzer (Microtrac MT3000II) under dry conditions.
- the degree of dispersion (%) of the obtained granular nucleating agent was measured using a powder property evaluation apparatus (manufactured by Seishin Enterprise Co., Ltd., Multitester MT-02). Specifically, it measured as follows. First, about 5 g of the obtained granular nucleating agent was prepared as a sample, and a charging container having an inner diameter of 3 cm, a cylinder having an inner diameter of 10 cm, a height of 50.5 cm, and a watch glass having a diameter of 10 cm were provided. . Subsequently, the sample was placed in a charging container, and the charging container was set so that the bottom had a height of 60 cm.
- Dispersity (%) [(input sample amount (g) ⁇ sample amount remaining in watch glass (g)) / input sample amount (g)] ⁇ 100
- the aspect ratio was determined by measuring the lengths of the major axis and minor axis of 100 crystals randomly from a micrograph, and calculating the average of the major axis / minor axis.
- the granular nucleating agent of each example and comparative example was evaluated based on the following evaluation items. The evaluation results are shown in Table 2.
- K st (Maximum explosion pressure, explosion index)
- the explosion index (K st ) and the maximum explosion pressure were measured according to JIS Z 8817: 2002.
- K st [10 2 kPa ⁇ m / s] (dp / dt) max ⁇ V 1/3 (Dp / dt) max : Maximum pressure increase rate, V: Measurement container volume
- ⁇ Haze 100 parts by weight of polypropylene and 0.1 parts by weight of the obtained granular nucleating agent were mixed with a Henschel mixer for 1 minute, and extruded to produce pellets at 230 ° C. and 150 rpm. did.
- a haze (haze value:%) was measured according to JIS K7105 for a test piece having a thickness of 1 mm obtained by injection molding at 200 ° C.
- the granular nucleating agents of Examples 1 to 3 have a smaller haze value within a practically practical range than the granular nucleating agent of Comparative Example 2, and can improve the transparency of the crystalline polymer. It turned out that it can utilize suitably as an agent.
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Abstract
Description
一般的な核剤は、各原料成分を混合(混練)し乾燥させた後、必要に応じて粉砕することで得られた粉粒体(粒状核剤)である。粒状核剤は、結晶性高分子等の熱可塑性樹脂と溶融混練され、熱可塑性樹脂の加熱成形加工に使用される。
粒状核剤の量産化において、ラボスケールからのスケールアップを検討した場合、粒状核剤において、搬送・混練・保管時などの各種の使用環境におけるハンドリング性等の、粉塵作業性の向上がさらに要求されることが判明した。このような粉塵作業性は、粒状核剤の製造・搬送・保管過程のみならず、当該粒状核剤を用いた混合品(組成物)や熱可塑性樹脂の製造過程、これらの量産化においても要求されるものである。
下記一般式(1)で表される化合物を含む粒状核剤であって、
レーザー回折式粒度分布測定法を用いて、当該粒状核剤の粒子径分布を乾式測定し、その粒状核剤の最大粒子径をDmaxとし、
下記の手順に従って測定される当該粒状核剤の分散度をDpとしたとき、
Dmaxが下記式(A)を満たし、かつDpが下記式(B)を満たす、粒状核剤が提供される。
80μm≦Dmax≦300μm ・・・式(A)
1.0%≦Dp≦27.0% ・・・式(B)
(手順)
所定量の粒状核剤をサンプルとして準備する。当該サンプルを60cmの高さから円筒内に投入し、円筒内部を上下方向に当該サンプルを落下させる。そして、その落下地点に設置してある時計皿上に残ったサンプルの量を測定する。投入したサンプル量および時計皿に残ったサンプル量を用いて、下記の式に基づいて分散度(%)を測定する。
分散度(%)=[(投入サンプル量(g)-時計皿に残ったサンプル量(g))/投入サンプル量(g)]×100
上記一般式(1)で表される化合物を含む粒状核剤であって、
レーザー回折式粒度分布測定法を用いて、当該粒状核剤の粒子径分布を乾式測定し、その粒状核剤の最大粒子径をDmax、体積平均粒子径をMVとしたとき、
Dmaxが下記式(A)を満たし、かつMVが下記式(C)を満たす、粒状核剤が提供される。
80μm≦Dmax≦300μm ・・・式(A)
5μm≦MV≦100μm ・・・式(C)
上記粒状核剤は、芳香族リン酸エステル金属塩を含有するものである。当該芳香族リン酸エステル金属塩は、下記一般式(1)によって表される化合物が用いられる。これらを単独で用いても2種以上を組み合わせて用いてもよい。
また得られた化合物を、溶剤に溶解し、水酸化リチウム等の他の金属水酸化物と反応させ、またはアルミニウム・マグネシウム・第二族元素のいずれかの塩と反応させ、得られた反応物を精製、乾燥することにより、別の上記化合物が得られる。
上記脂肪酸金属塩は、R6で表される脂肪族基が、炭素原子数10~21であるものが好ましく、特に、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、ベヘン酸、オレイン酸、12-ヒドロキシステアリン酸が好ましい。
MxMgyAlzCO3(OH)xp+2y+3z-2・nH2O
(上記一般式中、Mはアルカリ金属または亜鉛を表し、Xは0~6の数を表し、yは0~6の数を表し、zは0.1~4の数を表し、pはMの価数を表し、nは0~100の結晶水の数を表す)
このような粒状核剤のとしては、例えば、上記一般式(1)で表される化合物および他の成分の共存下、上記の粉砕手段を適切に組み合わせることにより粉砕処理することにより得られる。また、上述の粉砕手段、篩い分け、ブレンド方法などを用いることもできる。
80μm≦Dmax≦300μm ・・・式(A)
1.0%≦Dp≦27.0% ・・・式(B)
(手順)
所定量の粒状核剤をサンプルとして準備する。当該サンプルを60cmの高さから円筒内に投入し、円筒内部を上下方向に当該サンプルを落下させる。そして、その落下地点に設置してある時計皿上に残ったサンプルの量を測定する。投入したサンプル量および時計皿に残ったサンプル量を用いて、下記の式に基づいて分散度(%)を測定する。ここで、所定量は約5g、分散度は、3回の測定値の平均値としてもよい。
分散度(%)=[(投入サンプル量(g)-時計皿に残ったサンプル量(g))/投入サンプル量(g)]×100
さらには、粒状核剤の分散度および最大粒子径を指標とすることで、粉塵作業性および透明化性を安定的に評価することが可能となり、指標である分散度の上限、および最大粒子径の上限を所定値以下に制御することで、粉塵作業性および透明化性を向上できることが見出された。
そして、このような爆発指数や最大爆発圧力を指針とし、それをより低くすることで、スケールアップ時における粉塵特性を抑制でき、粒状核剤の作業性を向上できることが見出された。
80μm≦Dmax≦300μm ・・・式(A)
5μm≦MV≦100μm ・・・式(C)
本明細書中、「~」は、特に明示しない限り、上限値と下限値を含むことを表す。
上記抗酸化剤として、リン系抗酸化剤、フェノール系抗酸化剤、チオエーテル系抗酸化剤等が挙げられる。
上記帯電防止剤として、カチオン系界面活性剤、アニオン系界面活性剤、ノニオン系界面活性剤、両性界面活性剤等が挙げられる。
上記難燃剤として、ハロゲン系化合物、リン酸エステル系化合物、リン酸アミド系化合物、メラミン系化合物、ポリリン酸のメラミン塩化合物、フッ素樹脂又は金属酸化物等が挙げられる。
上記滑剤として、炭化水素系、脂肪酸系、脂肪族アルコール系、脂肪族エステル系、脂肪族アマイド系、金属石けん系等が挙げられる。
上記珪酸系添加剤として、フュームドシリカ、微粒子シリカ、けい石、珪藻土類、クレー、カオリン、シリカゲル、珪酸カルシウム、セリサイト、カオリナイト、フリント、長石粉、蛭石、アタパルジャイト、タルク、マイカ、ミネソタイト、パイロフィライト等が挙げられる。
成形方法としては、特に限定されるものではなく、射出成形法、押出成形法、ブロー成形法、回転成形、真空成形法、インフレーション成形法、カレンダー成形法、スラッシュ成形法、ディップ成形法、発泡成形法等が挙げられる。この中でも、射出成形法、押出成形法、ブロー成型法が好ましい。
1. 下記一般式(1)によって表される化合物を含む粒状核剤であって、
レーザー回折式粒度分布測定法による当該粒状核剤の、体積平均粒子径をMV、最大粒子径をDmaxとしたとき、
当該粒状核剤の粒子径プロファイルが、以下の式(A)および式(B)を満たす、粒状核剤。
5μm<MV<100μm ・・・式(A)
80μm<Dmax<300μm ・・・式(B)
2. 1.に記載の粒状核剤であって、
当該粒状核剤のアスペクト比は、1.5以上10以下である、粒状核剤。
3. 1.または2.に記載の粒状核剤であって、
前記化合物が、下記の式No.1から式No.12のいずれかで表される一または二以上の化合物を含む、粒状核剤。
5. 4.に記載の結晶性高分子組成物であって、
前記結晶性高分子がポリオレフィン系高分子を含む、結晶性高分子組成物。
6. 4.または5.に記載の結晶性高分子組成物であって、
結晶性高分子100重量部に対して、前記粒状核剤の含有量が0.001重量部以上10重量部以下である、結晶性高分子組成物。
7. 4.から6.のいずれか1つに記載の結晶性高分子組成物であって、
ペレット状である、結晶性高分子組成物。
2,2’-メチレンビス(4,6-ジ-t-ブチルフェニル)ホスフェート486g(1モル)、水酸化ナトリウム42g(1.05モル)と水100gの溶液およびメタノール97gをニーダー中に仕込み、室温で一時間混練した。減圧下に乾燥した後粉砕し、421gの白色粉末の化合物No.1を得た。
得られた化合物No.1を、粉砕処理なく、メッシュサイズ:355μmの篩で篩別して粒状核剤Aを得た。
得られた化合物No.1に対して、ボールミルで30分間粉砕し、メッシュサイズ:355μmの篩で篩別して粒状核剤Bを得た。
得られた化合物No.1に対して、ボールミルで4時間粉砕し、メッシュサイズ:355μmの篩で篩別して粒状核剤Cを得た。
得られた化合物No.1に対して、ボールミルで4時間粉砕し、さらにジェットミルで粉砕し、メッシュサイズ:355μmの篩で篩別して粒状核剤Dを得た。
・体積平均粒子径MV、および最大粒子径Dmaxは、乾式条件下、レーザー回折式粒度分布測定器(Microtrac MT3000II)を用いて測定した。
粉体特性評価装置(セイシン企業社製、マルチテスター MT-02)を用いて、得られた粒状核剤の分散度(%)を測定した。
具体的には、次のようにして測定した。
まず、サンプルとして、得られた粒状核剤を約5g、底に開閉自在のシャッターを備える、内径3cmの投入容器、内径10cm、高さ50.5cmの円筒、および直径10cmの時計皿を準備した。
続いて、サンプルを投入容器に入れ、底が高さ60cmとなるように投入容器を設置した。
続いて、円筒の上に、投入容器を設置し、円筒の下に、時計皿を設置した。円筒の下端と時計皿の表面との距離は約9cmであった。
続いて、投入容器の底のシャッターを開放することで、サンプルを円筒内に投入し、円筒内部の上下方向(鉛直方向)にサンプルを一気に落下させた。
その後、サンプルの落下地点に設置した時計皿に、飛散せず残ったサンプルの量を計量し、下記の式から分散度(%)を算出した。それぞれの粒状核剤について、分散度の測定を3回行い、その値の平均値を表1に示す。
分散度(%)=[(投入サンプル量(g)-時計皿に残ったサンプル量(g))/投入サンプル量(g)]×100
・アスペクト比は、顕微鏡写真からランダムに100個の結晶について長軸及び短軸の長さを測定し、長軸/短軸の平均を求めた。
・爆発指数(Kst)、及び最大爆発圧力は、JIS Z 8817:2002に準拠して測定した。
Kst[102kPa・m/s]=(dp/dt)max×V1/3
(dp/dt)max:最大圧力上昇速度、V:測定容器容積
篩別を行わないで、最大粒子径Dmaxが355μm超であり、化合物No.1で表される粒状核剤Eを準備した。
この粒状核剤Eを用いて、上述の方法でHazeを測定したところ、実施例1~3の場合と比べて、ヘイズ値が高い値を示すことが分かった。
Claims (11)
- 下記一般式(1)で表される化合物を含む粒状核剤であって、
レーザー回折式粒度分布測定法を用いて、当該粒状核剤の粒子径分布を乾式測定し、その粒状核剤の最大粒子径をDmaxとし、
下記の手順に従って測定される当該粒状核剤の分散度をDpとしたとき、
Dmaxが下記式(A)を満たし、かつDpが下記式(B)を満たす、粒状核剤。
80μm≦Dmax≦300μm ・・・式(A)
1.0%≦Dp≦27.0% ・・・式(B)
(手順)
所定量の粒状核剤をサンプルとして準備する。当該サンプルを60cmの高さから円筒内に投入し、円筒内部を上下方向に当該サンプルを落下させる。そして、その落下地点に設置してある時計皿上に残ったサンプルの量を測定する。投入したサンプル量および時計皿に残ったサンプル量を用いて、下記の式に基づいて分散度(%)を測定する。
分散度(%)=[(投入サンプル量(g)-時計皿に残ったサンプル量(g))/投入サンプル量(g)]×100
- 下記一般式(1)で表される化合物を含む粒状核剤であって、
レーザー回折式粒度分布測定法を用いて、当該粒状核剤の粒子径分布を乾式測定し、その粒状核剤の最大粒子径をDmax、体積平均粒子径をMVとしたとき、
Dmaxが下記式(A)を満たし、かつMVが下記式(C)を満たす、粒状核剤。
80μm≦Dmax≦300μm ・・・式(A)
5μm≦MV≦100μm ・・・式(C)
- 請求項1または2に記載の粒状核剤であって、
当該粒状核剤のアスペクト比は、1.5以上10以下である、粒状核剤。 - 請求項1~4のいずれか一項に記載の粒状核剤を熱可塑性樹脂中に含有する、樹脂組成物。
- 請求項5に記載の樹脂組成物であって、
前記熱可塑性樹脂が結晶性高分子を含む、樹脂組成物。 - 請求項6に記載の樹脂組成物であって、
前記結晶性高分子がポリオレフィン系高分子を含む、樹脂組成物。 - 請求項5~7のいずれか一項に記載の樹脂組成物であって、
前記熱可塑性樹脂100重量部に対して、前記粒状核剤の含有量が0.001重量部以上10重量部以下である、樹脂組成物。 - 請求項5~8のいずれか一項に記載の樹脂組成物であって、
ペレット状である、樹脂組成物。 - 請求項5~9のいずれか一項に記載の樹脂組成物を用いてなる成形品。
- 請求項5~9のいずれか一項に記載の樹脂組成物を用いて成形品を製造する製造方法。
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EP3753979B1 (en) | 2022-12-28 |
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