JP7158790B1 - Biodegradable composite composition - Google Patents
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- JP7158790B1 JP7158790B1 JP2022048248A JP2022048248A JP7158790B1 JP 7158790 B1 JP7158790 B1 JP 7158790B1 JP 2022048248 A JP2022048248 A JP 2022048248A JP 2022048248 A JP2022048248 A JP 2022048248A JP 7158790 B1 JP7158790 B1 JP 7158790B1
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- 239000000203 mixture Substances 0.000 title claims abstract description 47
- 239000002131 composite material Substances 0.000 title claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 32
- 229920002472 Starch Polymers 0.000 claims abstract description 19
- 239000008107 starch Substances 0.000 claims abstract description 19
- 235000019698 starch Nutrition 0.000 claims abstract description 19
- 235000013312 flour Nutrition 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 12
- 239000011347 resin Substances 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 9
- 229920002988 biodegradable polymer Polymers 0.000 claims abstract description 8
- 239000004621 biodegradable polymer Substances 0.000 claims abstract description 8
- 240000007594 Oryza sativa Species 0.000 claims abstract description 4
- 235000007164 Oryza sativa Nutrition 0.000 claims abstract description 4
- 240000008042 Zea mays Species 0.000 claims abstract description 4
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 claims abstract description 4
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims abstract description 4
- 235000005822 corn Nutrition 0.000 claims abstract description 4
- 235000009566 rice Nutrition 0.000 claims abstract description 4
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 21
- 239000000155 melt Substances 0.000 claims description 8
- 229920000520 poly(3-hydroxybutyrate-co-3-hydroxyvalerate) Polymers 0.000 claims description 8
- 239000004626 polylactic acid Substances 0.000 claims description 8
- 239000012744 reinforcing agent Substances 0.000 claims description 7
- -1 polyethylene Polymers 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 2
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 2
- 229940063655 aluminum stearate Drugs 0.000 claims description 2
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 2
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 2
- 235000013539 calcium stearate Nutrition 0.000 claims description 2
- 239000008116 calcium stearate Substances 0.000 claims description 2
- 235000019359 magnesium stearate Nutrition 0.000 claims description 2
- 239000012188 paraffin wax Substances 0.000 claims description 2
- 229920000573 polyethylene Polymers 0.000 claims description 2
- 229920001897 terpolymer Polymers 0.000 claims description 2
- 239000001993 wax Substances 0.000 claims description 2
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 2
- 229920000704 biodegradable plastic Polymers 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 7
- 239000002689 soil Substances 0.000 abstract description 6
- 238000009933 burial Methods 0.000 abstract description 5
- 238000010137 moulding (plastic) Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000000704 physical effect Effects 0.000 description 9
- 239000002699 waste material Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 229920000747 poly(lactic acid) Polymers 0.000 description 7
- 239000000463 material Substances 0.000 description 6
- 244000005700 microbiome Species 0.000 description 6
- 239000003623 enhancer Substances 0.000 description 5
- 238000002347 injection Methods 0.000 description 5
- 239000007924 injection Substances 0.000 description 5
- 229920000331 Polyhydroxybutyrate Polymers 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 239000003570 air Substances 0.000 description 4
- 238000006065 biodegradation reaction Methods 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000005015 poly(hydroxybutyrate) Substances 0.000 description 4
- 238000003915 air pollution Methods 0.000 description 3
- 229920001222 biopolymer Polymers 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 238000001746 injection moulding Methods 0.000 description 3
- 229920003023 plastic Polymers 0.000 description 3
- 239000004033 plastic Substances 0.000 description 3
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 2
- 208000034530 PLAA-associated neurodevelopmental disease Diseases 0.000 description 2
- 241000533293 Sesbania emerus Species 0.000 description 2
- 239000002671 adjuvant Substances 0.000 description 2
- 229910002091 carbon monoxide Inorganic materials 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 229920001577 copolymer Polymers 0.000 description 2
- 239000007822 coupling agent Substances 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 229940117927 ethylene oxide Drugs 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- LHGVFZTZFXWLCP-UHFFFAOYSA-N guaiacol Chemical compound COC1=CC=CC=C1O LHGVFZTZFXWLCP-UHFFFAOYSA-N 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 239000011777 magnesium Substances 0.000 description 2
- 229910052749 magnesium Inorganic materials 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 239000002667 nucleating agent Substances 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 239000004629 polybutylene adipate terephthalate Substances 0.000 description 2
- 239000004631 polybutylene succinate Substances 0.000 description 2
- 229920002961 polybutylene succinate Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 229920002101 Chitin Polymers 0.000 description 1
- 229920003314 Elvaloy® Polymers 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical class OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000004594 Masterbatch (MB) Substances 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 235000003095 Vaccinium corymbosum Nutrition 0.000 description 1
- 240000000851 Vaccinium corymbosum Species 0.000 description 1
- 235000017537 Vaccinium myrtillus Nutrition 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000021014 blueberries Nutrition 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 235000013339 cereals Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- CWVRJTMFETXNAD-JUHZACGLSA-N chlorogenic acid Chemical compound O[C@@H]1[C@H](O)C[C@@](O)(C(O)=O)C[C@H]1OC(=O)\C=C\C1=CC=C(O)C(O)=C1 CWVRJTMFETXNAD-JUHZACGLSA-N 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000009264 composting Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 229920006238 degradable plastic Polymers 0.000 description 1
- 238000002845 discoloration Methods 0.000 description 1
- 241001233061 earthworms Species 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 229960001867 guaiacol Drugs 0.000 description 1
- 239000012760 heat stabilizer Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 239000002029 lignocellulosic biomass Substances 0.000 description 1
- 239000011785 micronutrient Substances 0.000 description 1
- 235000013369 micronutrients Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000005445 natural material Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000013502 plastic waste Substances 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
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- 239000003516 soil conditioner Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 238000010186 staining Methods 0.000 description 1
- 239000000326 ultraviolet stabilizing agent Substances 0.000 description 1
- 239000000341 volatile oil Substances 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
-
- 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
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- 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
- C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
- C08K5/098—Metal salts of carboxylic acids
-
- 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
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L67/00—Compositions of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Compositions of derivatives of such polymers
- C08L67/04—Polyesters derived from hydroxycarboxylic acids, e.g. lactones
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L91/00—Compositions of oils, fats or waxes; Compositions of derivatives thereof
- C08L91/06—Waxes
-
- 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
- C08L101/16—Compositions of unspecified macromolecular compounds the macromolecular compounds being biodegradable
Abstract
【課題】生分解性プラスチック使用時の埋設や焼却による土壌、大気、海洋汚染の問題を最小限にし、さらに製造コストを低減するプラスチック成形品用原料組成物を提供する。【解決手段】本実施形態における生分解性複合体組成物は、生分解性高分子マトリックス樹脂を１００重量部と、コーヒーかすの粉と、米粉、トウモロコシ粉およびそれらの混合物からなる群から選択されるデンプン粉とを５～２００重量部と、を含む。例えば、コーヒーかすの粉を４０～８０重量部、デンプン粉を１０～２０重量部含んでもよい。【選択図】 なしThe object of the present invention is to provide a raw material composition for plastic moldings that minimizes the problems of soil, air, and sea pollution caused by burial or incineration when biodegradable plastics are used, and further reduces manufacturing costs. The biodegradable composite composition in this embodiment is selected from the group consisting of 100 parts by weight of a biodegradable polymer matrix resin, coffee grounds powder, rice flour, corn flour and mixtures thereof. and 5 to 200 parts by weight of starch powder. For example, it may contain 40 to 80 parts by weight of ground coffee grounds and 10 to 20 parts by weight of starch powder. [Selection figure] None
Description
本発明は、バイオ系フィラー、合成フィラー、およびその他の添加剤などを含む生分解性複合体組成物に関するものである。 The present invention relates to biodegradable composite compositions containing bio-based fillers, synthetic fillers, other additives, and the like.
分解性プラスチックに関する技術は、光分解技術、生分解技術、光生分解技術の３つに分類される。さらに、光分解技術は、感光性官能基の導入と感光性試薬の添加の２種類に分類される。感光性官能基導入型は、エチレンと一酸化炭素の共重合体を商品化している製造者が開発したもので、感光性試薬添加型は、エチレンと一酸化炭素の共重合体を商品化している製造者が開発したものである。 Technologies related to degradable plastics are classified into three categories: photodegradation technology, biodegradation technology, and photobiodegradation technology. Further, photolysis techniques are classified into two types: introduction of photosensitive functional groups and addition of photosensitive reagents. The photosensitive functional group-introduced type was developed by a manufacturer that commercializes copolymers of ethylene and carbon monoxide, and the photosensitive reagent-added type is a copolymer of ethylene and carbon monoxide. Developed by a manufacturer.
また、金属錯体化合物を添加するタイプは、感光性試薬を添加するタイプの主流であった。しかし、これらの光分解性製品は製造コストが高く、土中に埋めると太陽光が遮断され光エネルギーを吸収できないため分解されないという問題があった。そのため、光分解技術だけではプラスチック廃棄物問題を解決することができず、生分解技術の研究が続けられている。 Moreover, the type in which a metal complex compound is added has been the mainstream of the type in which a photosensitive reagent is added. However, these photodegradable products are expensive to manufacture, and when buried in the ground, they block sunlight and cannot absorb light energy, so they do not decompose. Therefore, photodegradation technology alone cannot solve the plastic waste problem, and research into biodegradation technology continues.
生分解性プラスチックは、PLA（ポリ乳酸）やPHB（ポリヒドロキシブチレート）などの微生物による高分子生成物、微生物が生産する生化学物質から合成される高分子、キチンなどの天然高分子から構成されている。しかし、これらの生分解性プラスチックは製造コストが高く経済的に適していないため、一般のプラスチックにコーヒーかすなどを添加した生分解性複合材料が提案されている。 Biodegradable plastics consist of polymers produced by microorganisms such as PLA (polylactic acid) and PHB (polyhydroxybutyrate), polymers synthesized from biochemical substances produced by microorganisms, and natural polymers such as chitin. It is However, these biodegradable plastics are economically unsuitable due to their high production costs, so biodegradable composite materials have been proposed in which coffee grounds or the like is added to general plastics.
従来、コーヒーかすを生分解性天然素材の成分の一つの選択肢として「含有してもよい」とする技術は公知である。しかしながら、「コーヒーかす」を必須成分として含有する場合に、実用性のある生分解性複合組成物というものは存在しなかった。 Conventionally, there has been known a technology that "may contain" coffee grounds as one of the components of the biodegradable natural material. However, there has been no practical biodegradable composite composition containing "coffee grounds" as an essential ingredient.
したがって、本発明の目的は、コーヒー豆を使用するリサイクル工程から容易に得られる廃コーヒーかすの粉などの生分解性天然素材を用いて、簡単な工程で優れた物性と安全性を有する生分解性複合組成物を製造することにより、生分解性プラスチック使用時の埋設や焼却による土壌、大気、海洋汚染の問題を最小限にし、さらに製造コストを低減するプラスチック成形品用原料組成物を提供することにある。 Accordingly, an object of the present invention is to provide a biodegradable product with excellent physical properties and safety in a simple process using biodegradable natural materials such as waste coffee grounds powder that can be easily obtained from a recycling process using coffee beans. To provide a raw material composition for plastic molded articles that minimizes the problems of soil, air, and marine pollution caused by burial or incineration when biodegradable plastics are used, and further reduces manufacturing costs by producing a biodegradable composite composition. That's what it is.
本発明に係る生分解性複合体組成物は、上述した課題を解決するために、生分解性高分子マトリックス樹脂を１００重量部と、コーヒーかすの粉と、米粉、トウモロコシ粉およびそれらの混合物からなる群から選択されるデンプン粉とを５～２００重量部と、を含む。 In order to solve the above-described problems, the biodegradable composite composition according to the present invention comprises 100 parts by weight of a biodegradable polymer matrix resin, coffee grounds powder, rice flour, corn flour and a mixture thereof. 5 to 200 parts by weight of a starch powder selected from the group consisting of;
本発明はPLAとPHBVの混合物１００重量部およびコーヒーかすの粉およびデンプン粉からなる群から選択される穀物粉５～２００重量部を含む生分解性プラスチック組成物を提供する。 The present invention provides a biodegradable plastic composition comprising 100 parts by weight of a mixture of PLA and PHBV and 5-200 parts by weight of flour selected from the group consisting of coffee grounds flour and starch flour.
本発明による複合組成物は、組成物の分解性を向上させ、コーヒーかすまたはデンプン粉の添加による物性の低下を防止するために、生分解補助剤としてグリセロールを０.１～５重量部含有することが好ましい。そのほか、コーヒーかすの粉およびデンプン粉とマトリックス樹脂との相溶性を向上させ、組成物の物性と作業性を同時に向上させるために、補強剤０.１～５重量部、メルトフローエンハンサー０.１～５重量部を含んでもよい。 The composite composition according to the present invention contains 0.1 to 5 parts by weight of glycerol as a biodegradation adjuvant in order to improve the degradability of the composition and prevent deterioration of physical properties due to the addition of coffee grounds or starch powder. is preferred. In addition, 0.1 to 5 parts by weight of a reinforcing agent and 0.1 part of a melt flow enhancer are added to improve the compatibility between the coffee grounds powder and starch powder and the matrix resin, and simultaneously improve the physical properties and workability of the composition. ∼5 parts by weight.
本発明は、生分解性プラスチック組成物に関するものである。特に良好な物性と安全性を有する各種製品に成形することができるばかりでなく、本発明材料は天然素材、すなわちコーヒーかすの粉とデンプン粉からなり、この組成物から製造された製品の廃棄物は一定期間経過後に自然界の微生物によって分解されるため、製品の廃棄物の埋設や焼却による土壌、大気、海洋汚染などの環境問題を最小限に抑えることができるプラスチック成形品用材料組成物に関するものである。 The present invention relates to biodegradable plastic compositions. In addition to being able to be molded into various products with particularly good physical properties and safety, the material of the present invention consists of natural materials, ie coffee grounds powder and starch powder, and waste products produced from this composition. is decomposed by microorganisms in the natural world after a certain period of time, so it is a material composition for plastic molded products that can minimize environmental problems such as soil, air, and marine pollution caused by burial or incineration of product waste. is.
本発明は、バイオポリマー（バクテリアによって自然に生成される生分解性プラスチック等の無毒性生分解性プラスチック）１００重量部、コーヒーかすの粉およびデンプン粉５～２００重量部からなることを特徴とする、コーヒーかすの粉を含む生分解性複合組成物に関するものである。 The present invention is characterized by comprising 100 parts by weight of biopolymer (non-toxic biodegradable plastic such as biodegradable plastic naturally produced by bacteria), 5 to 200 parts by weight of ground coffee grounds and starch powder. , relates to biodegradable composite compositions containing ground coffee grounds.
本発明による生分解性プラスチック組成物は、射出成形品、シート成形品、ブロー成形品など種々の形態で製造することができ、物性および製品安定性に優れるものである。本組成物に含まれるコーヒーかすの粉は、一定期間経過後に自然界の微生物によって分解されるため、本組成物を用いて製造された製品の廃棄物処理の効率を著しく向上させることができる。したがって、従来のプラスチック成形品の廃棄物の埋設や焼却による土壌汚染、大気汚染、海洋汚染の問題を最小限に抑えることができる。 The biodegradable plastic composition according to the present invention can be produced in various forms such as injection molded articles, sheet molded articles and blow molded articles, and has excellent physical properties and product stability. Since the coffee grounds contained in the present composition are decomposed by natural microorganisms after a certain period of time, the waste disposal efficiency of products manufactured using the present composition can be significantly improved. Therefore, it is possible to minimize the problems of soil pollution, air pollution, and marine pollution caused by the burial or incineration of the waste of conventional plastic moldings.
本発明による生分解性複合組成物について、以下詳細に説明する。本発明の生分解性複合組成物は、生分解性高分子マトリックス樹脂１００重量部を基準として、コーヒーかすの粉を５～２００重量部、好ましくは３０～８０重量部含有する。 The biodegradable composite composition according to the invention is described in detail below. The biodegradable composite composition of the present invention contains 5 to 200 parts by weight, preferably 30 to 80 parts by weight of coffee grounds powder based on 100 parts by weight of the biodegradable polymer matrix resin.
マトリックス樹脂には、PLA（ポリ乳酸）、PHB（ポリヒドロキシブチレート）、生分解性ランダムコポリマーであるPBAT（ポリブチレンアジペートテレフタレート）、いわゆるPHBV（Poly（３-hydroxybutyrate-co-３-hydroxyvalerate）、ポリ（３-ヒドロキシブチレート-コ-３-ヒドロキシバレレート））、ポリブチレンサクシネート（PBS）などの生分解性高分子樹脂が製品の成形性を考慮して使用可能である。 Matrix resins include PLA (polylactic acid), PHB (polyhydroxybutyrate), biodegradable random copolymer PBAT (polybutylene adipate terephthalate), so-called PHBV (Poly(3-hydroxybutyrate-co-3-hydroxyvalerate), Biodegradable polymer resins such as poly(3-hydroxybutyrate-co-3-hydroxyvalerate)) and polybutylene succinate (PBS) can be used in consideration of the moldability of the product.
本発明によるバイオポリマー組成物は、PLAとPBHVの混合物を含有するものである。
本発明の説明に用いる用語のうち、コーヒーかすの粉とデンプン粉とは、水分５%まで乾燥させた粉を意味する。 Among the terms used to describe the present invention, coffee grounds powder and starch powder refer to powders dried to 5% moisture content.
コーヒーかすの粉は、リグノセルロース系バイオマスであり、生命に必要な要素（C、H、O、N）を主成分とし、主にセルロース（５９．２～６２．９４wt%）、ヘミセルロース（５～１０wt%）、リグニン（１９．８～２６．５wt%）などを形成しているものである。さらに、これらの要素は、エッセンシャルオイルやフラボノイド、クエン酸、クロロゲン酸グアイアコールなどの回収可能な化合物の形で存在する。コーヒーかすに含まれるこれらの化合物は、PLAとの相性が良いという利点がある。また、この種の廃棄物には通常、カルシウム、マグネシウム、ナトリウムなどの無機微量栄養素とされる元素が含まれているが、その濃度は一般に乾燥重量で５．０%未満である。 Coffee grounds powder is a lignocellulosic biomass, mainly composed of the elements (C, H, O, N) necessary for life, mainly cellulose (59.2-62.94 wt%), hemicellulose (5- 10 wt%) and lignin (19.8-26.5 wt%). Furthermore, these elements are present in the form of recoverable compounds such as essential oils and flavonoids, citric acid and guaiacol chlorogenate. These compounds in coffee grounds have the advantage of being compatible with PLA. Also, this type of waste typically contains elements considered to be inorganic micronutrients, such as calcium, magnesium, sodium, etc., generally in concentrations of less than 5.0% by dry weight.
コーヒーかすは土壌にゆっくりと窒素を放出することが知られているので、庭ではコンポストやマルチングに使用することができる。乾燥したコーヒーかすには、カリウム、マグネシウム、リンが大量に含まれている。特に、ミミズや、ブルーベリーなどの酸を好む植物に好まれるが、使用中に酸が溶け出すため、一般的にpHは中性になる。 Coffee grounds are known to slowly release nitrogen into the soil, so they can be used in gardens for composting and mulching. Dried coffee grounds contain large amounts of potassium, magnesium and phosphorus. It is particularly preferred by earthworms and acid-loving plants such as blueberries, but since the acid dissolves during use, the pH generally becomes neutral.
使用済みのコーヒーかすは、土壌改良材として特に注目されている。スターバックスの「Ground for your Garden」プロジェクトなど、コーヒーショップの中には、コーヒー豆の廃棄を防ぐ取り組みを行っているところもあり、イギリスのケンブリッジシャー州の「Ground to Ground」や「Green Coffee Shop Scheme」など、地域主催の取り組みも存在する。 Spent coffee grounds are of particular interest as a soil conditioner. Some coffee shops, such as Starbucks' "Ground for your Garden" project, are working to prevent coffee bean wastage. There are also regionally sponsored initiatives such as
デンプン粉は、例えば米粉、トウモロコシ粉およびそれらの混合物からなる群から選択される。 Starch flour is for example selected from the group consisting of rice flour, corn flour and mixtures thereof.
このように、コーヒーかすの粉を含む複合組成物を用いて成形品を製造すれば、一定期間経過後に微生物によって生分解されるため、土壌、大気、水の汚染問題を最小限に抑えることができ、廃棄物処理の効率も向上させることができる。 Thus, if a composite composition containing ground coffee grounds is used to manufacture an article, it will be biodegraded by microorganisms after a certain period of time, thus minimizing the problem of soil, air and water pollution. It can also improve the efficiency of waste disposal.
本発明の組成物によれば、生分解補助剤としてのグリセロールを０．１～５重量部添加すると、生分解性だけでなく、その親水性グリセロールの水酸基と水との反応により、樹脂組成物からなる成形品の物性が向上するだけでなく、コーヒーかすの粉やデンプン粉の添加による物性の低下も防止することが可能である。 According to the composition of the present invention, when 0.1 to 5 parts by weight of glycerol is added as a biodegradation adjuvant, not only biodegradability but also the reaction between the hydroxyl group of the hydrophilic glycerol and water results in a resin composition. It is possible not only to improve the physical properties of the molded product composed of this, but also to prevent the deterioration of the physical properties due to the addition of coffee grounds powder and starch powder.
また、成形品の一般的な物性とバイオポリマー樹脂とコーヒーかすの粉やデンプン粉との相溶性を共に向上させるために、さらに補強剤０．１～５重量部、溶融流動性向上剤０．１～５重量部を添加してもよい。 In addition, in order to improve both the general physical properties of the molded product and the compatibility between the biopolymer resin and the coffee grounds powder or starch powder, 0.1 to 5 parts by weight of a reinforcing agent and 0.1 part by weight of a melt fluidity improver are added. 1 to 5 parts by weight may be added.
成形品の剛性を高めるために補強剤が使用される。補強剤の一例として、カップリング剤としてのELVALOY PTW（Dow Corning Corp.、登録商標）のようなエチレンターポリマー合成品が挙げられる。カップリング剤は、過酸化水素化合物からなる群から選択される１つを含む。その他の潜在的な成分は、主に加工性を向上させるために含まれるもので、溶融流動性向上剤や核剤などがある。 Reinforcing agents are used to increase the stiffness of the molded article. One example of a reinforcing agent is an ethylene terpolymer synthetic such as ELVALOY PTW (Dow Corning Corp.®) as a coupling agent. The coupling agent includes one selected from the group consisting of hydrogen peroxide compounds. Other latent ingredients are included primarily to improve processability, such as melt flow improvers and nucleating agents.
流動性向上剤は、押出成形や射出成形の工程で摩擦を低減するために使用される。流動性向上剤は、メルトフローレートを増加させ、加工温度を下げ、生産性を向上させる。流動性向上剤は、射出圧力を下げ、薄肉成形の工具への充填を容易にするために使用することができる。溶融流動性向上剤は、ステアリン酸カルシウム、ステアリン酸亜鉛、ステアリン酸バリウム、ステアリン酸アルミニウム、ステアリン酸マグネシウム、パラフィンワックスおよびポリエチレンワックスからなる群より選ばれる少なくとも１つを含む。溶融流動性向上剤の一例として、AP00157 EU Flow Enhancer （CRPP） MB （Tosaf Group、登録商標）がある。 Flow improvers are used to reduce friction in extrusion and injection molding processes. Flow improvers increase melt flow rate, lower processing temperatures, and improve productivity. Flow improvers can be used to reduce injection pressure and facilitate filling of thin-walled mold tools. The melt fluidity improver contains at least one selected from the group consisting of calcium stearate, zinc stearate, barium stearate, aluminum stearate, magnesium stearate, paraffin wax and polyethylene wax. An example of a melt flow enhancer is AP00157 EU Flow Enhancer (CRPP) MB (Tosaf Group®).
核剤の一例として、PLAマスターバッチCM-L01（Polyvel Inc.、登録商標）が挙げられる。その他、紫外線／熱安定剤、着色剤などの添加剤を加えてもよい。 An example of a nucleating agent is PLA masterbatch CM-L01 (Polyvel Inc., registered trademark). In addition, additives such as ultraviolet/heat stabilizers and colorants may be added.
上記の生分解性複合材料組成物は、射出成形品、シート成形品、ブロー成形品に使用することができる。例えば、生分解性高分子樹脂、コーヒーかすの粉、デンプン粉、グリセロール、化学強化剤、メルトフローエンハンサーを所定の割合で混合し、溶融した後、二軸押出機で押出成形を行う。ペレタイザーで造粒し、射出成形機やシートキャスティング押出機で射出成形品やシート成形品を製造する。このとき、次のような配合パラメータが維持された。 The above biodegradable composite material composition can be used for injection molded articles, sheet molded articles and blow molded articles. For example, a biodegradable polymer resin, coffee grounds powder, starch powder, glycerol, a chemical reinforcing agent, and a melt flow enhancer are mixed in a predetermined ratio, melted, and then extruded using a twin-screw extruder. Granulate with a pelletizer and manufacture injection molded products and sheet molded products with an injection molding machine or sheet casting extruder. At this time, the following formulation parameters were maintained.
回転数：１２５rpm
スループット：４０kg/hr
脱ガス：真空ゾーン７
Throughput: 40kg/hr
Degassing: vacuum zone 7
GER120型二軸押出機（スクリュー径３０mm、L/D=４５）で溶融し、粒状化した。
そのために、以下のような射出工程のパラメータを設定した。
It was melted and granulated in a GER120 twin-screw extruder (screw diameter 30 mm, L/D=45).
For this purpose, the parameters of the injection process were set as follows.
環状空間：１．４５mm
ノズル出口での溶融温度：１７０度
Annular space: 1.45mm
Melt temperature at nozzle exit: 170 degrees
［実施例］
以下、実施形態に言及した本発明の詳細を説明する。ただし、本発明による実施形態は様々な変更が可能であり、以下に説明する実施形態に限定されると理解されるべきではない。本発明の実施形態は当該技術分野において標準的な知識を有する者に対して、本発明をより明確に説明するために提供されるものである。
[Example]
The invention will now be described in detail with reference to embodiments. However, the embodiments according to the present invention are capable of various modifications and should not be understood to be limited to the embodiments described below. Embodiments of the present invention are provided in order to more clearly explain the present invention to those of ordinary skill in the art.
［第１実施例］
PHBV添加PLA（PLA with PHBV）を９０:１０の割合で混合してなる生分解性高分子マトリックス樹脂（メルトインデックス：１８）を１００重量部、８０：２０の割合のコーヒーかすの粉とデンプン粉を１００重量部、グリセロールを５重量部、補強剤を１重量部、メルトフローエンハンサーを１重量部混合し、混合しながら３～４分間１７０℃にて溶融し、１７０℃で押出成形しペレット状に形成させた。
[First embodiment]
100 parts by weight of biodegradable polymer matrix resin (melt index: 18) obtained by mixing PLA with PHBV at a ratio of 90:10, coffee grounds powder and starch powder at a ratio of 80:20 100 parts by weight of glycerol, 5 parts by weight of glycerol, 1 part by weight of a reinforcing agent, and 1 part by weight of a melt flow enhancer are mixed, melted at 170 ° C. for 3 to 4 minutes while mixing, and extruded at 170 ° C. to form pellets. was formed.
［第２～９実施例］
用いた成分およびその含有量が以下の表３に示す通りであること以外は、第１実施例と同様にして組成物を製造した。
以下の表３において、成分の含有量の単位は重量部である。
[Second to ninth embodiments]
A composition was produced in the same manner as in Example 1, except that the components used and their contents were as shown in Table 3 below.
In Table 3 below, the unit of content of the components is parts by weight.
上記実施形態による生分解性複合材料組成物を、射出成形機を用いて１７０～１７５℃、５００～６００psiの条件で射出し、その厚さが３．２６mmの試料を得た。この試料の引張強度、引張伸び、および形状を測定し、その結果を以下の表４に示す。 The biodegradable composite material composition according to the above embodiment was injected using an injection molding machine under conditions of 170-175° C. and 500-600 psi to obtain a sample with a thickness of 3.26 mm. The tensile strength, tensile elongation, and shape of this sample were measured and the results are shown in Table 4 below.
外観の色や汚れの程度を考慮し、以下の基準で形状を「良い」「普通」「悪い」の３段階に分けて評価した。また、１００×１００×５mmの大きさのチップおよび実験試料を作製し、チップおよび実験試料の表面に水を噴霧した後、以下の基準に基づいて分解の程度を考慮し、生分解性を良好、正常、不良の３段階に分けて評価した。 Considering the color of the appearance and the degree of staining, the shape was evaluated by dividing it into three grades of "good", "normal" and "bad" according to the following criteria. In addition, a chip with a size of 100 x 100 x 5 mm and an experimental sample were prepared, and after spraying water on the surface of the chip and experimental sample, the degree of decomposition was considered based on the following criteria, and biodegradability was determined to be good. , Normal and Poor.
（１）形状の推定基準
良好：組成物をサンプルに成形することができ、添加物の混入などによる変形がないこと。
普通：組成物をサンプルに成形することができるが、添加物の混入などによる変形がある。
不良：組成物のサンプルへの成形が不良である。
（２）生分解性の推定基準
良好：サンプル全体の５０%以上が分解している。
正常：サンプル全体の３０%以上が分解している。
不良：サンプル全体の１０%未満が分解している。
(1) Estimation Criteria for Shape Good: The composition can be molded into a sample, and there is no deformation due to contamination of additives.
Normal: The composition can be molded into a sample, but there is deformation due to inclusion of additives, etc.
Poor: Poor molding of the composition into the sample.
(2) Estimation criteria for biodegradability Good: 50% or more of the entire sample is degraded.
Normal: 30% or more of the entire sample is degraded.
Poor: Less than 10% of the total sample is degraded.
表４を参照すると、本発明による生分解性プラスチック組成物を用いて製造したサンプルは、形状、引張強度、引張伸びなどの物性が良好であり、様々な製品に使用できることが良く理解できる。さらに、本発明の材料は優れた生分解性を示すため、製品の廃棄物を埋設または焼却することによって生じる土壌汚染、大気汚染、海洋汚染などの環境問題を最小限に抑えることができる組成物である。 With reference to Table 4, the samples produced using the biodegradable plastic composition according to the present invention have good physical properties such as shape, tensile strength and tensile elongation, and can be used for various products. Furthermore, since the material of the present invention exhibits excellent biodegradability, the composition can minimize environmental problems such as soil pollution, air pollution, and marine pollution caused by burying or incinerating product waste. is.
以上のように、本発明による生分解性プラスチック複合体は、生分解性製品の製造工程をより簡素化し、費用対効果の高いものとすることができる。特に、コーヒーかすの粉およびデンプン粉は、PLA-PHBVマトリックス樹脂とより優れた相溶性を示し、変色に対する安定性および吸水に対する安定性に優れているので、バイオポリマー樹脂と配合されて製造された組成物の成形品は他の種類の穀物のそれよりも有用に使用することができる。 As described above, the biodegradable plastic composite according to the present invention can make the manufacturing process of biodegradable products simpler and more cost-effective. In particular, coffee grounds powder and starch powder show better compatibility with PLA-PHBV matrix resin, and have excellent stability against discoloration and water absorption. Formed articles of the composition can be used more usefully than those of other types of cereals.
また、本発明材料は一定期間経過後に自然界の微生物によって分解されるため、製品の廃棄物の埋設や焼却による土壌、大気、海洋の汚染といった環境問題を最小限に抑えることができる。 In addition, since the material of the present invention is decomposed by natural microorganisms after a certain period of time, it is possible to minimize environmental problems such as contamination of soil, air, and sea due to burial or incineration of product waste.
Claims (7)
コーヒーかすの粉を５２～８０重量部と、
米粉、トウモロコシ粉およびそれらの混合物からなる群から選択されるデンプン粉を１４～２０重量部と、
を含み、
前記生分解性高分子マトリックス樹脂は、
ポリ乳酸（PLA）を９０重量部、
ポリ（３-ヒドロキシブチレート-コ-３-ヒドロキシバレレート）（PHBV）を１０重量部含む、生分解性複合体組成物。 100 parts by weight of a biodegradable polymer matrix resin,
52 to 80 parts by weight of coffee grounds powder,
14-20 parts by weight of starch flour selected from the group consisting of rice flour, corn flour and mixtures thereof;
including
The biodegradable polymer matrix resin is
90 parts by weight of polylactic acid (PLA),
A biodegradable composite composition comprising 10 parts by weight of poly(3-hydroxybutyrate-co-3-hydroxyvalerate) (PHBV) .
溶融流動性向上剤を３～５重量部と、
をさらに含む、請求項１または２に記載の生分解性複合体組成物。 3 to 5 parts by weight of an ethylene terpolymer synthetic product as a reinforcing agent,
3 to 5 parts by weight of a melt fluidity improver,
3. The biodegradable composite composition of claim 1 or 2 , further comprising:
前記デンプン粉を１４重量部含む、請求項１に記載の生分解性複合体組成物。 2. The biodegradable composite composition of claim 1, comprising 14 parts by weight of said starch powder.
前記デンプン粉を２０重量部含む、請求項１に記載の生分解性複合体組成物。 2. The biodegradable composite composition of claim 1, comprising 20 parts by weight of said starch powder.
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| US20060194900A1 (en) * | 2005-02-26 | 2006-08-31 | Chow David C | Articles of manufacture made from coffee bean residue, and methods for making such articles |
| KR20110098224A (en) * | 2010-02-26 | 2011-09-01 | 동국대학교 산학협력단 | Biodegradable resin composition |
| CN109593333A (en) * | 2018-12-26 | 2019-04-09 | 广东聚航新材料研究院有限公司 | A kind of high strength, biodegradable PLA/PHBV composite material and preparation method and film |
| CN110452512A (en) * | 2019-09-18 | 2019-11-15 | 南京博方生物科技有限公司 | A kind of amyloid biomass imitative rattan material and preparation method thereof |
| KR102058394B1 (en) * | 2018-06-14 | 2020-01-22 | 김용동 | Eco-Friendly Bio Bag Manufacture Method and Bag Obtained by using Method |
| CN112341766A (en) * | 2020-10-30 | 2021-02-09 | 辽宁幸福人科技有限公司 | Fully-degradable bio-based composite material product and preparation method thereof |
| CN113201172A (en) * | 2021-05-31 | 2021-08-03 | 咖法科技(上海)有限公司 | Coffee grounds degradable cold drink straw and preparation method thereof |
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2022
- 2022-03-24 JP JP2022048248A patent/JP7158790B1/en active Active
- 2022-11-30 WO PCT/JP2022/044139 patent/WO2023181504A1/en unknown
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060194900A1 (en) * | 2005-02-26 | 2006-08-31 | Chow David C | Articles of manufacture made from coffee bean residue, and methods for making such articles |
| KR20110098224A (en) * | 2010-02-26 | 2011-09-01 | 동국대학교 산학협력단 | Biodegradable resin composition |
| KR102058394B1 (en) * | 2018-06-14 | 2020-01-22 | 김용동 | Eco-Friendly Bio Bag Manufacture Method and Bag Obtained by using Method |
| CN109593333A (en) * | 2018-12-26 | 2019-04-09 | 广东聚航新材料研究院有限公司 | A kind of high strength, biodegradable PLA/PHBV composite material and preparation method and film |
| CN110452512A (en) * | 2019-09-18 | 2019-11-15 | 南京博方生物科技有限公司 | A kind of amyloid biomass imitative rattan material and preparation method thereof |
| CN112341766A (en) * | 2020-10-30 | 2021-02-09 | 辽宁幸福人科技有限公司 | Fully-degradable bio-based composite material product and preparation method thereof |
| CN113201172A (en) * | 2021-05-31 | 2021-08-03 | 咖法科技(上海)有限公司 | Coffee grounds degradable cold drink straw and preparation method thereof |
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| JP2023141764A (en) | 2023-10-05 |
| WO2023181504A1 (en) | 2023-09-28 |
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