WO2023063915A1 - Application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials - Google Patents
Application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials Download PDFInfo
- Publication number
- WO2023063915A1 WO2023063915A1 PCT/TR2022/051127 TR2022051127W WO2023063915A1 WO 2023063915 A1 WO2023063915 A1 WO 2023063915A1 TR 2022051127 W TR2022051127 W TR 2022051127W WO 2023063915 A1 WO2023063915 A1 WO 2023063915A1
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- WO
- WIPO (PCT)
- Prior art keywords
- microcapsules
- essential oil
- eucalyptus essential
- textile
- application
- Prior art date
Links
- 239000003094 microcapsule Substances 0.000 title claims abstract description 117
- 239000004753 textile Substances 0.000 title claims abstract description 48
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 32
- 239000000341 volatile oil Substances 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 29
- 244000166124 Eucalyptus globulus Species 0.000 title claims abstract 12
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N glyoxal Chemical compound O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims abstract description 68
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- 229940015043 glyoxal Drugs 0.000 claims abstract description 34
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims abstract description 30
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 27
- 108010010803 Gelatin Proteins 0.000 claims abstract description 19
- 239000008273 gelatin Substances 0.000 claims abstract description 19
- 229920000159 gelatin Polymers 0.000 claims abstract description 19
- 235000019322 gelatine Nutrition 0.000 claims abstract description 19
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 19
- 239000004971 Cross linker Substances 0.000 claims abstract description 16
- 244000215068 Acacia senegal Species 0.000 claims abstract description 13
- 229920000084 Gum arabic Polymers 0.000 claims abstract description 13
- 239000000205 acacia gum Substances 0.000 claims abstract description 13
- 235000010489 acacia gum Nutrition 0.000 claims abstract description 13
- 239000003921 oil Substances 0.000 claims abstract description 7
- 241000283690 Bos taurus Species 0.000 claims abstract description 4
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 4
- 239000002861 polymer material Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 24
- 238000002156 mixing Methods 0.000 claims description 22
- 238000005354 coacervation Methods 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000002360 preparation method Methods 0.000 claims description 10
- 230000006641 stabilisation Effects 0.000 claims description 5
- 238000011105 stabilization Methods 0.000 claims description 5
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 238000005470 impregnation Methods 0.000 claims description 4
- -1 polypropylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 230000000284 resting effect Effects 0.000 claims description 4
- 231100000419 toxicity Toxicity 0.000 claims description 4
- 230000001988 toxicity Effects 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000004750 melt-blown nonwoven Substances 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- 239000008213 purified water Substances 0.000 claims 1
- 239000003814 drug Substances 0.000 abstract description 6
- 239000002537 cosmetic Substances 0.000 abstract description 4
- 235000013305 food Nutrition 0.000 abstract description 2
- 241000219927 Eucalyptus Species 0.000 description 21
- 239000002775 capsule Substances 0.000 description 21
- 238000012360 testing method Methods 0.000 description 14
- 239000011162 core material Substances 0.000 description 13
- 239000000126 substance Substances 0.000 description 12
- 239000000243 solution Substances 0.000 description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 9
- 239000000835 fiber Substances 0.000 description 9
- 239000011257 shell material Substances 0.000 description 9
- 238000000576 coating method Methods 0.000 description 7
- 238000007730 finishing process Methods 0.000 description 7
- 244000005700 microbiome Species 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 238000001878 scanning electron micrograph Methods 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 6
- 239000013543 active substance Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 5
- 239000011248 coating agent Substances 0.000 description 5
- 230000005764 inhibitory process Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000011156 evaluation Methods 0.000 description 4
- 230000036541 health Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000000879 optical micrograph Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 230000008821 health effect Effects 0.000 description 3
- 238000003921 particle size analysis Methods 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- NOOLISFMXDJSKH-UTLUCORTSA-N (+)-Neomenthol Chemical compound CC(C)[C@@H]1CC[C@@H](C)C[C@@H]1O NOOLISFMXDJSKH-UTLUCORTSA-N 0.000 description 2
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- NOOLISFMXDJSKH-UHFFFAOYSA-N DL-menthol Natural products CC(C)C1CCC(C)CC1O NOOLISFMXDJSKH-UHFFFAOYSA-N 0.000 description 2
- 239000001856 Ethyl cellulose Substances 0.000 description 2
- ZZSNKZQZMQGXPY-UHFFFAOYSA-N Ethyl cellulose Chemical compound CCOCC1OC(OC)C(OCC)C(OCC)C1OC1C(O)C(O)C(OC)C(CO)O1 ZZSNKZQZMQGXPY-UHFFFAOYSA-N 0.000 description 2
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 2
- 239000013011 aqueous formulation Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- RYYVLZVUVIJVGH-UHFFFAOYSA-N caffeine Chemical compound CN1C(=O)N(C)C(=O)C2=C1N=CN2C RYYVLZVUVIJVGH-UHFFFAOYSA-N 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000009918 complex formation Effects 0.000 description 2
- 238000013270 controlled release Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 238000005538 encapsulation Methods 0.000 description 2
- 235000019325 ethyl cellulose Nutrition 0.000 description 2
- 229920001249 ethyl cellulose Polymers 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 230000000873 masking effect Effects 0.000 description 2
- 229940041616 menthol Drugs 0.000 description 2
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- YYGNTYWPHWGJRM-UHFFFAOYSA-N (6E,10E,14E,18E)-2,6,10,15,19,23-hexamethyltetracosa-2,6,10,14,18,22-hexaene Chemical compound CC(C)=CCCC(C)=CCCC(C)=CCCC=C(C)CCC=C(C)CCC=C(C)C YYGNTYWPHWGJRM-UHFFFAOYSA-N 0.000 description 1
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- RAXXELZNTBOGNW-UHFFFAOYSA-N 1H-imidazole Chemical compound C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 description 1
- 241000517647 Balcis Species 0.000 description 1
- 208000025721 COVID-19 Diseases 0.000 description 1
- 101100361281 Caenorhabditis elegans rpm-1 gene Proteins 0.000 description 1
- 229920002134 Carboxymethyl cellulose Polymers 0.000 description 1
- 208000035484 Cellulite Diseases 0.000 description 1
- 229920001661 Chitosan Polymers 0.000 description 1
- 108010082495 Dietary Plant Proteins Proteins 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 238000012695 Interfacial polymerization Methods 0.000 description 1
- LPHGQDQBBGAPDZ-UHFFFAOYSA-N Isocaffeine Natural products CN1C(=O)N(C)C(=O)C2=C1N(C)C=N2 LPHGQDQBBGAPDZ-UHFFFAOYSA-N 0.000 description 1
- 241000588747 Klebsiella pneumoniae Species 0.000 description 1
- 206010049752 Peau d'orange Diseases 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- BHEOSNUKNHRBNM-UHFFFAOYSA-N Tetramethylsqualene Natural products CC(=C)C(C)CCC(=C)C(C)CCC(C)=CCCC=C(C)CCC(C)C(=C)CCC(C)C(C)=C BHEOSNUKNHRBNM-UHFFFAOYSA-N 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 229920001222 biopolymer Polymers 0.000 description 1
- 238000009529 body temperature measurement Methods 0.000 description 1
- 229960001948 caffeine Drugs 0.000 description 1
- VJEONQKOZGKCAK-UHFFFAOYSA-N caffeine Natural products CN1C(=O)N(C)C(=O)C2=C1C=CN2C VJEONQKOZGKCAK-UHFFFAOYSA-N 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001746 carotenes Chemical class 0.000 description 1
- 235000005473 carotenes Nutrition 0.000 description 1
- 235000019993 champagne Nutrition 0.000 description 1
- 229940045110 chitosan Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 230000002354 daily effect Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- FPAFDBFIGPHWGO-UHFFFAOYSA-N dioxosilane;oxomagnesium;hydrate Chemical compound O.[Mg]=O.[Mg]=O.[Mg]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O FPAFDBFIGPHWGO-UHFFFAOYSA-N 0.000 description 1
- PRAKJMSDJKAYCZ-UHFFFAOYSA-N dodecahydrosqualene Natural products CC(C)CCCC(C)CCCC(C)CCCCC(C)CCCC(C)CCCC(C)C PRAKJMSDJKAYCZ-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000003974 emollient agent Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 239000010642 eucalyptus oil Substances 0.000 description 1
- 229940044949 eucalyptus oil Drugs 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000007380 fibre production Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- DDSRCCOGHFIQDX-UHFFFAOYSA-N furan-2,5-dione;methoxymethane Chemical compound COC.O=C1OC(=O)C=C1 DDSRCCOGHFIQDX-UHFFFAOYSA-N 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000000077 insect repellent Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229940119170 jojoba wax Drugs 0.000 description 1
- 230000005923 long-lasting effect Effects 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000004745 nonwoven fabric Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000001139 pH measurement Methods 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920002432 poly(vinyl methyl ether) polymer Polymers 0.000 description 1
- 229920000447 polyanionic polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 150000003140 primary amides Chemical class 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 239000001944 prunus armeniaca kernel oil Substances 0.000 description 1
- 229960003471 retinol Drugs 0.000 description 1
- 235000020944 retinol Nutrition 0.000 description 1
- 239000011607 retinol Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000004626 scanning electron microscopy Methods 0.000 description 1
- 150000003334 secondary amides Chemical class 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229940031439 squalene Drugs 0.000 description 1
- TUHBEKDERLKLEC-UHFFFAOYSA-N squalene Natural products CC(=CCCC(=CCCC(=CCCC=C(/C)CCC=C(/C)CC=C(C)C)C)C)C TUHBEKDERLKLEC-UHFFFAOYSA-N 0.000 description 1
- 238000009988 textile finishing Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 239000003440 toxic substance Substances 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/06—Making microcapsules or microballoons by phase separation
- B01J13/10—Complex coacervation, i.e. interaction of oppositely charged particles
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5052—Proteins, e.g. albumin
- A61K9/5057—Gelatin
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/02—Making microcapsules or microballoons
- B01J13/20—After-treatment of capsule walls, e.g. hardening
- B01J13/206—Hardening; drying
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/005—Compositions containing perfumes; Compositions containing deodorants
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M23/00—Treatment of fibres, threads, yarns, fabrics or fibrous goods made from such materials, characterised by the process
- D06M23/12—Processes in which the treating agent is incorporated in microcapsules
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/20—Polyalkenes, polymers or copolymers of compounds with alkenyl groups bonded to aromatic groups
Definitions
- the invention relates to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, which are widely used in many industries such as food, agriculture, medicine, pharmaceuticals, and cosmetics.
- textile industry started its studies in this field late compared to other sectors, it is currently producing innovative ideas and inventions in this field.
- microcapsules with antibacterial properties containing eucalyptus essential oil When applied to textile surfaces, they are used both on textile surfaces used in our daily lives and on all kinds of textile surfaces used in the health sector (stretcher cover, mask, surgical gown, etc.) makes life easier by using. In particular, it will provide antibacterial effectiveness if applied to protective masks, which in the Covid- 19 pandemic are now part of everyday life, rather than medical textiles.
- microcapsules can be spherical or irregularly shaped. They can be single-core, multi-core or matrix in structure. In singlecore microcapsules, the core material is continuously wrapped by a shell. In multicore microcapsules, the core material is collected in different parts of the microcapsule and surrounded by shell material. In matrix-type microcapsules, the core material is homogeneously distributed within the shell material. (Kut, 2011).
- the core material can be protected from reactive, corrosive and harmful environment, it can gain better workability (increase in solubility, fluidity, etc.), its shelf life is increased, dangerous and toxic materials can be safely transported, enzyme and microorganism immobilization can be performed, taste and odor can be hidden, liquid substances can be transported in solid form and their release can be kept under control (Nelson, 2002; Rosenberg et al., 1990; Anal and Singh, 2007; Krasaekoopt et al., 2003; Champagne and Fustier, 2007; KOQ et al., 2010). Many techniques are used in the production of microcapsules. In the selection of the microencapsulation technique, Type of core material, Desired particle size, Permeability of the shell material, etc. Features like this are important. Microencapsulation technique should be chosen according to the targeted effect. (Kut, 2011).
- ultrasonic Kerat et al., 2009
- microwave energy use Karl et al., 2003
- plasma application Karahan et al., 2009; Samanta et al., 2014
- foamed application Kut, 2011
- coating methods Perelshtein et al., 2013
- microcapsule applications Monllor et al., 2010; Yuan et al., 2009
- Microencapsulation technology is an important technique in terms of prolonging the effect of the functional finishing applied to the product (Re, 1998). It is seen as unrivaled, especially when effects such as controlled release are desired (Re, 1998).
- Microencapsulation can also be applied to other wet processes such as dyeing and printing.
- Environmental effects such as washing conditions and usage conditions limit the long-lasting use of many substances.
- Such substances are protected by a shell with the microencapsulation technique and their resistance to the environment is increased (Tan et al., 2003; Kim and Cho, 2002; Salatin et al., 2009; Huang and Yang, 2014; Martin et al., 2015; Ezhilarasi, 2013). Due to the long-term effect, it provides in textile finishing processes, the use of microencapsulation technique is frequently encountered in recent days (Li et al., 2013; Sathianarayanan et al., 2011).
- Microencapsulation is the encapsulation of various chemicals such as drugs, proteins, dyes or cosmetics in a liquid, gaseous or solid state in a suitable shell (Nesterenko et al., 2013; Nesterenko et al., 2014; Rajam and Anandharamakrishnan, 2015; Nunes et al., 2015).
- the encapsulated material is called the core (Istanbul Commerce University Journal of Science 15th Year Special Issue Spring 2016 11), and the coating material is called the wall, shell or wall material (Nesterenko et al., 2013).
- microencapsulation technique controlled/delayed release to textile surfaces (Kut, 2011), taste, odor (Fei et al., 2015) and color masking, UV (Xu et al., 2013), heat (Pomianowski et al., 2012), oxidation ( Gupta et al., 2015), protection against acids and bases and stabilization of volatile compounds, antibacterial (Qimen, 2007), anti-microbiality (Balci, 2006), anti-fungal (Park et al., 2009), long-term flame retardancy ( Giraud et al., 2001), insect repellent (Miller et al., 2011) and heat insulation (Hawlader et al., 2003) properties can be gained. After the textile materials are produced in the desired construction (structure), various functional properties are gained to the fabrics by finishing processes. In terms of microcapsule production, the commercial microcapsule in our country is produced and sold by the German Rudolph company within the scope of Rudalf Duraner partnership.
- microcapsules which have the feature of giving freshness and coolness, contain frescolate and menthol.
- TR2015/06062 “Seamless Bra with Microcapsule” the patent application titled Sun Textile’s patent in 2015 is related to three-dimensional honeycomb textured seamless bras containing microcapsules containing active ingredients of Dictyopterans unitednacea extract and apricot kernel oil.
- TR200505291 “Fibers and Non-Woven Textiles Finished with Micro Capsules” the patent application titled Fashion Chemicals received in 2002 concerns the application of microcapsules containing squalene, chitosan, retinol, caffeine, vegetable proteins and their hydrolysis products, carotenes and jojoba oil to fibers or non-woven textiles in finishing processes.
- This invention relates to a process for making films from nonwoven webs containing filaments, fibers by converting filaments, fibers or nonwoven webs into films.
- This invention relates to a filament-forming material and methods that can be used to prepare such filaments for nonwovens where yarns, and in particular one or more active substances, are filamented or used in filaments.
- This invention relates to forming a film layer on a filament, fiber or nonwoven surface containing an active agent to form a filament fiber or nonwoven surface that can disperse the active agent in its content.
- This invention relates to filaments, and more particularly to filaments comprising a filament forming material and an additive, particularly one or more active agents, non-woven webs using the filaments, and methods for making such filaments.
- Patent application numbered WO2019243425 Al entitled "Microcapsule Preparation Process” relates to a new process for the preparation of fill-shell microcapsules.
- Microcapsules are also an object of the invention.
- Consumer products containing said microcapsules, particularly perfumed consumer products or flavored consumer products, are also part of the invention.
- microcapsules Approximately 97% of these microcapsules have a size less than 100 and more characteristically having a particle size peak distribution of 30 to 40 microns (microcapsular diameter). These microcapsules contain less than approximately 3 wt. % free oil and more characteristically less than about 1 wt. % free oil (non-micro- encapsulated oil) and have less free (unreacted) formaldehyde which can be extracted with water, than do prior art microencapsulated emollient materials.
- the dry microcapsules of this invention are free-flowing and have a silky-smooth feeling similar to that of talcum powder.
- This invention eucalyptus and essential fatty featured antibacterial microcapsules applied to the textile material, and property; a property is high antibacterial, non-toxic biodegradable fact that the skin in lack.
- microcapsules consist of completely biodegradable ingredients, they do not contain any toxic substances for the human body and there is no toxicity for the environment.
- Microcapsules containing eucalyptus essential oil, which also has antibacterial properties, are not available in the literature.
- Glutaraldehyde has the code HE14 (Slight effects for eyes, nose, throat and skin) while glyoxal has the code HE 16 (Mild effects for eyes, nose, throat and skin). Based on these data, we think that it is more appropriate to use glyoxal on surfaces applied to textiles and in contact with human skin. In addition, the fact that the microcapsules contain less than 2% crosslinker prevents toxicity.
- Figure 1 It is a schematic representation of the production steps of the microcapsule.
- Figure 2 It is a schematic representation of the production steps of the microcapsule.
- Figure 3 Optical microscope image of the microcapsules in the coacervation stage. (lOOx magnification)
- Figure 5 It is an optical microscope image of microcapsules after the addition of glyoxal. (lOOx magnification ratio)
- Figure 6 They are optical microscope images of textile surfaces, a) meltblown surface b) glyoxalli microcapsule applied surface c) gluteraldehyde microcapsule applied surface (lOOx magnification ratio)
- Figure 7 Comparative FT-IR analysis of eucalyptus essential oil/gelatin/arabic, gum/glyoxal microcapsule/glutaraldehyde microcapsule.
- Figure 8 Comparative FT-IR spectrum of microencapsulated meltblown surfaces with glutaraldehyde and glyoxal.
- Figure 9 Glyoxal microcapsule applied meltblown surface SEM images.
- Figure 10 Glyoxal microcapsule applied meltblown surface SEM images.
- Figure 11 Glyoxal microcapsule applied meltblown surface SEM images.
- Figure 12 Glyoxal microcapsule applied meltblown surface SEM images.
- the invention consists of eucalyptus essential oil as oil, powdered gelatin (J) (bovine gelatin-type B) and gum arabic (A) as polymer material, glutaraldehyde (25%) and glyoxal (40%) as crosslinker, acetic acid as pH adjuster. (99.8%) and sodium hydroxide (99%).
- Microcapsules become usable by being applied on textile surfaces by absorbing 30 g/m2 meltblown nonwoven surface produced from 100% polypropylene and drying the samples at room temperature (20 C° ⁇ 2) for 8 hours.
- the invention as an oil eucalyptus essential oil, gelatin powder, a polymer material (J) (bovine gelatin Type B) and gum Arabic (A), cross-connector glutaraldehyde (25%) and glioksal (%40), acetic acid as a pH adjuster (%99,8) and sodium hydroxide (99%) it contains.
- aqueous solutions of eucalyptus essential oil which is the core material, were prepared at a ratio of 1 :1 (50-60°C) and aqueous solutions of gum arabic (A) and gelatin (J) were mixed at 400 rpm using a mechanical mixer.
- acetic acid the pH was adjusted to the range of 3.5-4 (pH where the polymers are electrolytes) and the polyanion (gum arabic) - polycation (gelatin) complex formation was started and the mixture was left to rest for the stabilization of the complexes.
- the pH was adjusted to 9 by adding sodium hydroxide and thus the complex formation (coacervation step) was stopped.
- microcapsules produced in the study were applied to the 30 g/m2 meltblown nonwoven surface made of 100% polypropylene by the impregnation method.
- the samples were dried at room temperature (20°C ⁇ 2) for 8 hours.
- the size of the capsules in the coacervation stage ranged from 5.62 pm to 38.99 pm, while the average capsule size was 19.70 pm. While the size of the capsules using glutaraldehyde ranged from 5.46 pm to 36.31 pm, the average capsule size was determined as 17.10 pm. The size of the capsules using glyoxal ranged from 6.14 pm to 63.82 pm, while the average capsule size was measured as 18.37 pm.
- Eucalyptus essential oil as the core material used in the produced microcapsules, biopolymers as the wall material, gum arabic (A) and gelatin (J), FT-IR analysis for Microcapsule with Glutaraldehyde (GM) and Glyoxal Microcapsule (GIM) are presented in Figure 7.
- the characteristic bands for eucalyptus essential oil are the band showing C-H stresses at 2967 and the band showing C-N stresses at 1214. In Figure 8, these bands are seen for eucalyptus essential oil. In the structure of the microcapsules, the band at 2967 was not visible, but the band at 1214 showing the C-N tensions was observed.
- the characteristic bands for gum arabic (A) are bands showing N-H stretches at 3300 and negatively charged carboxyl groups at 2925.
- the characteristic bands for gelatin (J) are bands showing positively charged amine groups at 3400 and C-N stretches at 1078.
- the bands showing that gum arabic (A) and gelatin (J) react in the presence of the crosslinker and that new primary, secondary and tertiary amide bonds are formed in the medium are characteristic bands in 1636, 1545 and 1241.
- Figure 8 shows the FT-IR spectrum for Melt blown Surface with Glyoxal Microcapsule (Y) treated with microcapsules with glutaraldehyde and glyoxal.
- Bands showing the presence of eucalyptus essential oil in the structure in the surface spectra were observed at 2840 cm' 1 on the microcapsule with glutaraldehyde (GM) surface and at 2921 cm' 1 on the glyoxal microcapsules (GIM) surface.
- Bands showing the presence of gelatin (J) in the structure on the microencapsulated surfaces were observed at 1599 cm-1 on the microcapsule with glutaraldehyde (GM) surface and at 1634 cm-1 on the glyoxal microcapsules (GIM) surface.
- SEM images were taken from the surface on which the microcapsule was applied, and the morphology of the microcapsules, the capsule dimensions and the appearance on the polypropylene fibers were examined.
- SEM images at different magnifications taken from meltblown ( Figure 9, Figure 10, Figure 11, Figure 12) surfaces treated with glyoxal and microcapsule with glutaraldehyde (GM).
- GM glutaraldehyde
- the average capsule size was 5.56 pm in the microcapsule application using glutaraldehyde as the crosslinker
- the average capsule size was measured as 2.89 pm in the microcapsule application using glyoxal as the crosslinker. All the capsules displayed were found to be non-porous. In addition, it was determined from the images that the microcapsules were generally in smooth spherical morphology and attached to the fibers on the applied surfaces, but generally appeared embedded in the excess polymers, and the relatively large and dense capsules that could be seen in the optical microscope were deformed in the coating and vacuum processes for SEM imaging.
- AATCC 147 According to the 2016 standard, antibacterial activity test was applied to 6 sample surfaces. The results are given in the table above. According to the test results, microorganism growth has been observed on the surface that has not been treated with number 1, and the antibacterial activity test result is ineffective. No microorganism growth was observed in the surface test impregnated with eucalyptus essential oil Number 2, the inhibition zone was determined as 2.25 mm for Staphylococcus aureus gram (+) bacteria and for Klebsiella pneumoniae gram (-) bacteria, and the antibacterial activity test result was recorded as effective.
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Abstract
The invention is widely used in many sectors such as food, agriculture, medicine, medicine, cosmetics, textile, eucalyptus essential oil microcapsules with antibacterial properties and application to textile materials and its feature; eucalyptus essential oil as oil, powder gelatin (J) (bovine gelatin-type B) and gum arabic (A) as polymer material, glutaraldehyde (25%), and glyoxal (40%) as crosslinker, acetic acid (40%) as pH adjuster (99.8%), and sodium hydroxide (99%).
Description
APPLICATION OF EUCALYPTUS ESSENTIAL OIL TO MICROCAPSULES WITH ANTIBACTERIAL PROPERTIES AND TEXTILE MATERIALS
Technical Field:
The invention relates to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, which are widely used in many industries such as food, agriculture, medicine, pharmaceuticals, and cosmetics. Although the textile industry started its studies in this field late compared to other sectors, it is currently producing innovative ideas and inventions in this field.
When microcapsules with antibacterial properties containing eucalyptus essential oil are applied to textile surfaces, they are used both on textile surfaces used in our daily lives and on all kinds of textile surfaces used in the health sector (stretcher cover, mask, surgical gown, etc.) makes life easier by using. In particular, it will provide antibacterial effectiveness if applied to protective masks, which in the Covid- 19 pandemic are now part of everyday life, rather than medical textiles.
State of the Art:
The morphology (structure) of microcapsules varies mainly depending on the core material and the microencapsulation process. Microcapsules can be spherical or irregularly shaped. They can be single-core, multi-core or matrix in structure. In singlecore microcapsules, the core material is continuously wrapped by a shell. In multicore microcapsules, the core material is collected in different parts of the microcapsule and surrounded by shell material. In matrix-type microcapsules, the core material is homogeneously distributed within the shell material. (Kut, 2011).
Thanks to the microencapsulation technique, the core material can be protected from reactive, corrosive and harmful environment, it can gain better workability (increase in
solubility, fluidity, etc.), its shelf life is increased, dangerous and toxic materials can be safely transported, enzyme and microorganism immobilization can be performed, taste and odor can be hidden, liquid substances can be transported in solid form and their release can be kept under control (Nelson, 2002; Rosenberg et al., 1990; Anal and Singh, 2007; Krasaekoopt et al., 2003; Champagne and Fustier, 2007; KOQ et al., 2010). Many techniques are used in the production of microcapsules. In the selection of the microencapsulation technique, Type of core material, Desired particle size, Permeability of the shell material, etc. Features like this are important. Microencapsulation technique should be chosen according to the targeted effect. (Kut, 2011).
At the beginning of the techniques used in microcapsule production; extruder, spray drying, in-situ polymerization, interfacial polymerization, coacervation and fluidized bed microencapsulation methods.
Developing technology has made functional product design a priority in the textile industry, as in every field. In addition to the aesthetic appearance of the products, their functionality, comfort features, not harming the health of the user and being economical are among the demands of the consumers. In addition, the fact that energy resources are becoming more expensive and limited, and the environmental awareness gradually develops, has made energy and water saving compulsory in the textile sector as in all areas of life. Functionality can be given to textile materials in fiber production, as well as mostly through finishing processes. Finishing processes, with the most general definition, are the processes applied to improve the attitude-appearance and usage properties of textile materials. There are many chemicals commonly used in finishing processes. The most distinctive feature of these chemicals is that they are not substantive (interest) in textile products. For this reason, applications made according to the impregnation method are frequently used in finishing applications in business environments. In addition, foamed application and coating methods have also been used in finishing processes in recent years. In the textile sector, the search for alternative methods to conventional methods has accelerated in order to maintain industrialization and protect the environment. Among these methods, ultrasonic (Kamel et al., 2009) and microwave
energy use (Kim et al., 2003), plasma application (Karahan et al., 2009; Samanta et al., 2014), foamed application (Kut, 2011), coating methods ( Perelshtein et al., 2013) and microcapsule applications (Monllor et al., 2010; Yuan et al., 2009) stand out from other methods especially in terms of environmental and economic advantages. Microencapsulation technology is an important technique in terms of prolonging the effect of the functional finishing applied to the product (Re, 1998). It is seen as unrivaled, especially when effects such as controlled release are desired (Re, 1998). Microencapsulation can also be applied to other wet processes such as dyeing and printing. Environmental effects such as washing conditions and usage conditions limit the long-lasting use of many substances. Such substances are protected by a shell with the microencapsulation technique and their resistance to the environment is increased (Tan et al., 2003; Kim and Cho, 2002; Salatin et al., 2009; Huang and Yang, 2014; Martin et al., 2015; Ezhilarasi, 2013). Due to the long-term effect, it provides in textile finishing processes, the use of microencapsulation technique is frequently encountered in recent days (Li et al., 2013; Sathianarayanan et al., 2011). Microencapsulation is the encapsulation of various chemicals such as drugs, proteins, dyes or cosmetics in a liquid, gaseous or solid state in a suitable shell (Nesterenko et al., 2013; Nesterenko et al., 2014; Rajam and Anandharamakrishnan, 2015; Nunes et al., 2015). The encapsulated material is called the core (Istanbul Commerce University Journal of Science 15th Year Special Issue Spring 2016 11), and the coating material is called the wall, shell or wall material (Nesterenko et al., 2013). With the use of microencapsulation technique, controlled/delayed release to textile surfaces (Kut, 2011), taste, odor (Fei et al., 2015) and color masking, UV (Xu et al., 2013), heat (Pomianowski et al., 2012), oxidation ( Gupta et al., 2015), protection against acids and bases and stabilization of volatile compounds, antibacterial (Qimen, 2007), anti-microbiality (Balci, 2006), anti-fungal (Park et al., 2009), long-term flame retardancy ( Giraud et al., 2001), insect repellent (Miller et al., 2011) and heat insulation (Hawlader et al., 2003) properties can be gained. After the textile materials are produced in the desired construction (structure), various functional properties are gained to the fabrics by finishing processes.
In terms of microcapsule production, the commercial microcapsule in our country is produced and sold by the German Rudolph company within the scope of Rudalf Duraner partnership.
Its microcapsules, which have the feature of giving freshness and coolness, contain frescolate and menthol.
TR201920466 "A Microcapsule Spraying System For the Production of Denim or NonDenim Products with Functional Properties And Its Working Method” the patent that Roteks Textile company received in 2019 is related to the use of a microcapsule spraying system for the production of denim and non-denim products with functional properties. The method described in this patent is the microencapsulation of cosmetic active substances with a spray system and their application to textiles. It has been stated that the spraying system causes less water, chemical and energy consumption compared to impregnation and extraction methods.
National patents related to the subject of invention:
TR2016/04040 “Using Microcapsules on Textile Surface in Apparel Industry” the patent application titled Defacto received in 2016 is related to the addition of different properties to textile products in the ready-made clothing sector by applying microcapsules in the finishing processes. In this method, microcapsule applied textiles; Microcapsules containing saltidine have anti-insect properties, capsules containing fresco late and menthol have cooling properties, capsules containing vitamin E have anti-aging properties, capsules containing brown seaweed have anti-cellulite properties, capsules containing some plant extracts have a thinning feature, capsules containing spice mixtures add fragrance.
TR2015/06062 “Seamless Bra with Microcapsule” the patent application titled Sun Textile’s patent in 2015 is related to three-dimensional honeycomb textured seamless bras containing microcapsules containing active ingredients of Dictyopterans membrenacea extract and apricot kernel oil.
TR200505291 “Fibers and Non-Woven Textiles Finished with Micro Capsules” the patent application titled Fashion Chemicals received in 2002 concerns the application of microcapsules containing squalene, chitosan, retinol, caffeine, vegetable proteins and their hydrolysis products, carotenes and jojoba oil to fibers or non-woven textiles in finishing processes.
TR200800889 “Microcapsules Produced by Coacervation, containing a Pharmaceutical in Ethyl Cellulose Coating” the patent application titled Adare Pharma obtained in 2004 relates to microcapsules produced by coacervation, containing a pharmaceutical in an ethyl cellulose coating. Capsules produced in this way have been noted to have excellent taste masking and extended active ingredient release properties.
International patents on the subject of invention:
[EP2588652B1, 2019]: This invention relates to the application of active agents with different functions to fibers and textile surfaces by coating them with polymers.
[US9163205B2, 2010]: This invention relates to a process for making films from nonwoven webs containing filaments, fibers by converting filaments, fibers or nonwoven webs into films.
[CA2803625C, 2010]: This invention relates to a filament-forming material and methods that can be used to prepare such filaments for nonwovens where yarns, and in particular one or more active substances, are filamented or used in filaments.
[US20180338890A1, 2010]: This invention relates to forming a film layer on a filament, fiber or nonwoven surface containing an active agent to form a filament fiber or nonwoven surface that can disperse the active agent in its content.
[CA2803629C, 2010]: This invention relates to filaments, and more particularly to filaments comprising a filament forming material and an additive, particularly one or
more active agents, non-woven webs using the filaments, and methods for making such filaments.
The applications most similar to the invention are as follows:
Patent application numbered WO2019243425 Al entitled "Microcapsule Preparation Process" relates to a new process for the preparation of fill-shell microcapsules. Microcapsules are also an object of the invention. Consumer products containing said microcapsules, particularly perfumed consumer products or flavored consumer products, are also part of the invention.
US5043161A “Small, oily, free-flowing, silky-smooth, talc-like, dry microcapsules and aqueous formulations containing them ” this disclosure is directed to the preparation of dry microencapsulated product, having an oily core material with microcapsule cell wall materials having a first cell wall of gelatin/polyvinyl methylether maleic anhydride copolymer (PVMMA)/carboxymethylcellulose (CMC) which is prehardened (crosslinked) with a material selected from the group consisting of formaldehyde, glyoxal and glutaraldehyde to which there is grafted formaldehyde and resorcinol which is then crosslinked with formaldehyde and urea, and aqueous formulations containing them. Approximately 97% of these microcapsules have a size less than 100 and more characteristically having a particle size peak distribution of 30 to 40 microns (microcapsular diameter). These microcapsules contain less than approximately 3 wt. % free oil and more characteristically less than about 1 wt. % free oil (non-micro- encapsulated oil) and have less free (unreacted) formaldehyde which can be extracted with water, than do prior art microencapsulated emollient materials. The dry microcapsules of this invention are free-flowing and have a silky-smooth feeling similar to that of talcum powder.
In the applications listed above, polymers are used as wall materials in the production of microcapsules and chemical binders are used to secure the capsules. This leads to toxicity.
Description of the Invention:
This invention, eucalyptus and essential fatty featured antibacterial microcapsules applied to the textile material, and property; a property is high antibacterial, non-toxic biodegradable fact that the skin in lack.
The meeting of microencapsulation technology and textile enables the production of technical or functional textile surfaces.
The produced microcapsules consist of completely biodegradable ingredients, they do not contain any toxic substances for the human body and there is no toxicity for the environment. Microcapsules containing eucalyptus essential oil, which also has antibacterial properties, are not available in the literature. The HE (Health effect) codes found in the toxicity reports found in Pubchem data, the National Library of Medicine institution affiliated to the US National Health Agency, analyze the effects of chemicals on the health of living things. Glutaraldehyde has the code HE14 (Slight effects for eyes, nose, throat and skin) while glyoxal has the code HE 16 (Mild effects for eyes, nose, throat and skin). Based on these data, we think that it is more appropriate to use glyoxal on surfaces applied to textiles and in contact with human skin. In addition, the fact that the microcapsules contain less than 2% crosslinker prevents toxicity.
Description of the Figures:
This invention is described in more detail by means of sampling only, with reference to the October drawings hereinafter, in these drawings;
Figure 1 It is a schematic representation of the production steps of the microcapsule.
Figure 2 It is a schematic representation of the production steps of the microcapsule.
Figure 3 Optical microscope image of the microcapsules in the coacervation stage. (lOOx magnification)
Figure 4 Optical microscope image of microcapsules after adding glutaraldehyde. (lOOx magnification)
Figure 5 It is an optical microscope image of microcapsules after the addition of glyoxal. (lOOx magnification ratio)
Figure 6 They are optical microscope images of textile surfaces, a) meltblown surface b) glyoxalli microcapsule applied surface c) gluteraldehyde microcapsule applied surface (lOOx magnification ratio)
Figure 7 Comparative FT-IR analysis of eucalyptus essential oil/gelatin/arabic, gum/glyoxal microcapsule/glutaraldehyde microcapsule.
Figure 8 Comparative FT-IR spectrum of microencapsulated meltblown surfaces with glutaraldehyde and glyoxal.
Figure 9 Glyoxal microcapsule applied meltblown surface SEM images.
Figure 10 Glyoxal microcapsule applied meltblown surface SEM images.
Figure 11 Glyoxal microcapsule applied meltblown surface SEM images.
Figure 12 Glyoxal microcapsule applied meltblown surface SEM images.
The figures to help understand the present invention are numbered as indicated in the attached image and are given below along with their names.
Description of References:
10. Heating
20. Preparation
30. Preparation of The Solution
40. Mixing 1
50. Mixing 2
60. Adjusting to pH 1
70. Mixing 3
80. Mixing 4
90. Adjusting to pH 2
100. 30 min. Mixing
110. Setting PH 3.5- 4
120. Stabilization
130. Termination of the Coacervation Phase
140. Lowering the Temperature
150. Hardening
160. Splitting the Mixture into 2
170. Addition
180. 120 Min. Mixing
190. Resting
GM. Microcapsule with Glutaraldehyde
GIM. Glyoxal Microcapsule
A. Gum Arabic
J. Gelatin
O. Eucalyptus Oil
X. Melt blown Surface with Glutaraldehyde Microcapsule Applied
Y. Melt blown Surface with Glyoxal Microcapsule
Description of The Invention:
The invention consists of eucalyptus essential oil as oil, powdered gelatin (J) (bovine gelatin-type B) and gum arabic (A) as polymer material, glutaraldehyde (25%) and glyoxal (40%) as crosslinker, acetic acid as pH adjuster. (99.8%) and sodium hydroxide (99%).
Invention; Heating (10) 1500 mL of pure water to 50-60°C, preparation of 1 M NaOH solution (20), Preparation of the solution (30), of 1 M acetic acid solution mixture and, Mixing 1 (40), 16 g gelatin and 400 ml distilled water at 50-60°C at 400 rpm for 30 minutes, mixing 3 (50), 160 ml of eucalyptus essential oil and 240 ml of pure water at 50-60°C for 30 minutes at 400 rpm 1 M NaOH solution of gelatin-pure water mixture adjusting to pH 7 1 (60) with mixing gelatin - pure water and eucalyptus essential oil - pure water mixture mixing 3 (70) at 50-60°C for 30 minutes at 400 rpm, 16 g gum arabic - 400 ml pure water mixture is prepared and 50 Mixing 4(80) at -60°C for 30 minutes at 400 rpm the gum arabic - water mixture adjusting to pH 72 (90) with 1 M NaOH solution, stabilization (120) of the complexes by mixing all the prepared materials together at 50- 60°C at 1000 rpm for 30 minutes mixing (100), setting pH to 3.5-4 (110) with 1 M acetic acid, resting for 90 minutes at room temperature, Termination of the coacervation phase (130) by adjusting the pH to 9.5-10 with 1 M NaOH solution leaving the ice bath to lower the temperature (140) to 5°C keeping the shells in an ice bath at 5°C for 60 minutes splitting the mixture into 2 (160), addition (170) of glutaraldehyde to the mixture at 5°C to one of the mixtures, glyoxal to the mixture at 5°C to the other mixing the mixtures at 1200-1500 rpm at room temperature for 120 minutes mixing (180), and resting (190) the mixtures at 4°C for 600 minutes (Figure 1, Figure 2).
Microcapsules become usable by being applied on textile surfaces by absorbing 30 g/m2 meltblown nonwoven surface produced from 100% polypropylene and drying the samples at room temperature (20 C° ± 2) for 8 hours.
Detailed Description of The Invention:
Chemicals Used
The invention as an oil eucalyptus essential oil, gelatin powder, a polymer material (J) (bovine gelatin Type B) and gum Arabic (A), cross-connector glutaraldehyde (25%) and glioksal (%40), acetic acid as a pH adjuster (%99,8) and sodium hydroxide (99%) it contains.
Devices Used
In the experimental study, laboratory type heater (hot&stirrer, Tepe MS300HS) to adjust the temperature of the solutions in microencapsulation and to keep it constant, digital thermometer (Loyka) for temperature measurements of solutions, digital pHmeter (Hanna HI2211-02 Table type pHmeter, Germany) for pH measurements of solutions, in microencapsulation experiment setup, mechanical stirrer (0-2200 rpm Isolab Laborgerate Gmbh, Germany) in the mixing stages, examination of the morphology of the produced microcapsules, particle size analysis and optical microscope to detect the presence of microcapsules on microcapsule applied textile surfaces (BAB Bs200Doc, Turkey), molecular structure of microcapsules and microcapsule applied textile surfaces FT-IR Spectroscopy (Perkin Elmer Frontier FT-IR Spectrophotometer Spectrum 400, USA) for high level chemical structure analysis, SEM Scan for detecting the presence of microcapsules on microcapsule applied textile surfaces, examining microcapsule morphology and particle size analysis. All-electron microscope (Zeiss Evo® LS10, Germany) instruments were used. In order to determine the antibacterial activity of microcapsules, the antibacterial activity test (AATCC 147- 2016) was carried out in an accredited laboratory, Ekoteks Laboratory and Gbzetim A.§.
Microencapsulation of Eucalyptus Essential Oil with Complex Coacervation Method
In the first step of microencapsulation, aqueous solutions of eucalyptus essential oil, which is the core material, were prepared at a ratio of 1 :1 (50-60°C) and aqueous
solutions of gum arabic (A) and gelatin (J) were mixed at 400 rpm using a mechanical mixer. With the addition of acetic acid, the pH was adjusted to the range of 3.5-4 (pH where the polymers are electrolytes) and the polyanion (gum arabic) - polycation (gelatin) complex formation was started and the mixture was left to rest for the stabilization of the complexes. Then, the pH was adjusted to 9 by adding sodium hydroxide and thus the complex formation (coacervation step) was stopped. The mixture was cooled to 5°C in an ice bath and the mixture was left at this temperature for 1 hour to harden the microcapsule shell structures. Since two different crosslinkers will be used, after the mixture is divided into 2, the crosslinker glutaraldehyde and crosslinker glyoxal are added to stabilize the microcapsules. Microcapsules were rested at 4°C for 6 hours. The wall/core ratio of 1 :5 was applied in the microcapsules. In Figures 1 and 2, the production of eucalyptus essential oil microcapsules by the complex coacervation method is shown with all its steps.
Application of Microcapsules to Textile Surfaces
The microcapsules produced in the study were applied to the 30 g/m2 meltblown nonwoven surface made of 100% polypropylene by the impregnation method. The samples were dried at room temperature (20°C±2) for 8 hours.
According to the particle/size analysis given in the table above, the size of the capsules in the coacervation stage ranged from 5.62 pm to 38.99 pm, while the average capsule size was 19.70 pm. While the size of the capsules using glutaraldehyde ranged from
5.46 pm to 36.31 pm, the average capsule size was determined as 17.10 pm. The size of the capsules using glyoxal ranged from 6.14 pm to 63.82 pm, while the average capsule size was measured as 18.37 pm. When the images and dimensions of the microcapsules at the coacervation stage and the images examined after the crosslinker addition were compared, it was determined that the deviation in particle sizes in the use of glutaraldehyde was less than the use of glyoxal and a more regular distribution was achieved. In addition, the surface images of melt blown (Figure 6) applied microcapsules with the addition of glutaraldehyde and glyoxal crosslinker, which were not applied microcapsules, were examined under an optical microscope and the presence of microcapsules on the surfaces was determined.
Evaluation of FT-IR Analysis
Eucalyptus essential oil as the core material used in the produced microcapsules, biopolymers as the wall material, gum arabic (A) and gelatin (J), FT-IR analysis for Microcapsule with Glutaraldehyde (GM) and Glyoxal Microcapsule (GIM) are presented in Figure 7. The characteristic bands for eucalyptus essential oil are the band showing C-H stresses at 2967 and the band showing C-N stresses at 1214. In Figure 8, these bands are seen for eucalyptus essential oil. In the structure of the microcapsules, the band at 2967 was not visible, but the band at 1214 showing the C-N tensions was observed. The characteristic bands for gum arabic (A) are bands showing N-H stretches at 3300 and negatively charged carboxyl groups at 2925. The characteristic bands for gelatin (J) are bands showing positively charged amine groups at 3400 and C-N stretches at 1078. The bands showing that gum arabic (A) and gelatin (J) react in the presence of the crosslinker and that new primary, secondary and tertiary amide bonds are formed in the medium are characteristic bands in 1636, 1545 and 1241. These bands were seen in glutaraldehyde microcapsules in 1636, 1468 and 1297, in glyoxal microcapsules (GIM) in 1638, 1375, and their application to microcapsules with antibacterial properties and textile materials with eucalyptus essential oil.
Figure 8 shows the FT-IR spectrum for Melt blown Surface with Glyoxal Microcapsule (Y) treated with microcapsules with glutaraldehyde and glyoxal. Bands showing the presence of eucalyptus essential oil in the structure in the surface spectra were observed
at 2840 cm'1 on the microcapsule with glutaraldehyde (GM) surface and at 2921 cm'1 on the glyoxal microcapsules (GIM) surface. Bands showing the presence of gelatin (J) in the structure on the microencapsulated surfaces were observed at 1599 cm-1 on the microcapsule with glutaraldehyde (GM) surface and at 1634 cm-1 on the glyoxal microcapsules (GIM) surface. These results show that both glutaraldehyde and glyoxal microcapsules (GIM) have been successfully applied to textile surfaces.
Evaluation of SEM Analysis
SEM images were taken from the surface on which the microcapsule was applied, and the morphology of the microcapsules, the capsule dimensions and the appearance on the polypropylene fibers were examined. Above are SEM images at different magnifications taken from meltblown (Figure 9, Figure 10, Figure 11, Figure 12) surfaces treated with glyoxal and microcapsule with glutaraldehyde (GM). According to the particle size analysis performed on the SEM images taken from the microcapsule- applied surfaces, it was determined that the size of the microcapsules varied between 1.00 pm and 17.96 pm. While the average capsule size was 5.56 pm in the microcapsule application using glutaraldehyde as the crosslinker, the average capsule size was measured as 2.89 pm in the microcapsule application using glyoxal as the crosslinker. All the capsules displayed were found to be non-porous. In addition, it was determined from the images that the microcapsules were generally in smooth spherical morphology and attached to the fibers on the applied surfaces, but generally appeared embedded in the excess polymers, and the relatively large and dense capsules that could be seen in the optical microscope were deformed in the coating and vacuum processes for SEM imaging.
Evaluation of Antibacterial Efficacy Analysis
AATCC 147: According to the 2016 standard, antibacterial activity test was applied to 6 sample surfaces. The results are given in the table above. According to the test results, microorganism growth has been observed on the surface that has not been treated with
number 1, and the antibacterial activity test result is ineffective. No microorganism growth was observed in the surface test impregnated with eucalyptus essential oil Number 2, the inhibition zone was determined as 2.25 mm for Staphylococcus aureus gram (+) bacteria and for Klebsiella pneumoniae gram (-) bacteria, and the antibacterial activity test result was recorded as effective. No microorganism growth was observed in the melt blown surface (X) test, on which microcapsules with glutaraldehyde number 3 were applied, and the inhibition zone of gram (+) and gram (-) bacteria was determined as 2.2 mm, and the antibacterial activity test result was recorded as effective. Number 4 glioksalli meltblown microcapsules applied to the surface (Y) of the test microorganism unprecedented growth of gram (+) 2.1 mm inhibition zone for bacteria, gram(-) bacteria for antibacterial activity and 2.2 mm inhibition zone were recorded as the test result has been determined to be effective. Number 5 microorganism growth was observed on the meltblown surface (X) where 50% concentration of gluteraldehyde microcapsule was applied and antibacterial activity was ineffective as a result of the test.No microorganism growth was observed in the meltblown surface (Y) test, on which glyoxal microcapsule number 6 was applied at 50% concentration, the inhibition zone of gram(+) and gram(-) bacteria was determined as 2.2 mm, and the antibacterial activity test result was recorded as effective. These results confirmed the antibacterial activity of eucalyptus essential oil in the literature. At the same time, the antibacterial activity of the surfaces on which the microcapsules produced using both glutaraldehyde crosslinker and glyoxal crosslinker were applied was determined. These tests were carried out 40 days after the production of the capsules and this shows us that the eucalyptus essential oil is protected by encapsulation and has a controlled release on the surface. The fact that the capsule with glutaraldehyde is ineffective and the capsule with glyoxal is effective on the surfaces where 50% concentration is applied shows that the antibacterial activity of the microcapsules produced by using the glyoxal crosslinker is higher.
Claims
1- The invention is related to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, and its feature; eucalyptus essential oil as oil, powder gelatin (J) (bovine gelatin-type B) and gum arabic (A) as polymer material, glutaraldehyde (25%), and glyoxal (40%) as crosslinker, acetic acid (40%) as pH adjuster ( 99.8%), and sodium hydroxide (99%).
2- As mentioned in Claim 1, It is related to the application of eucalyptus essential oil to antibacterial microcapsules and textile materials, eucalyptus essential oil is related to the application of microcapsules with antibacterial properties and textile materials, and its feature;
Heating (10) 1500 mL of pure water to 50-60°C,
- Preparation (20) of 1 M NaOH solution,
- Preparation of solution (30) 1 M acetic acid,
Mixing 1 (40), a mixture of 16 g gelatin with 400 ml purified water at 50- 60°C at 400 rpm for 30 min
- Mixing 2 (50) 160 ml of eucalyptus essential oil and 240 ml of distilled water at 50-60°C at 400 rpm for 30 minutes,
Adjusting the pH 1 (60) of gelatin - pure water mixture to 1 M NaOH solution (60), mixing 3 (70) gelatin - pure water with eucalyptus essential oil - pure water mixture at 50-60°C for 30 minutes at 400 rpm,
- Preparation of 16 gr gum arabic - 400 ml distilled water mixture and mixing 4 (80) at 50-60°C for 30 minutes at 400 rpm, adjusting pH 7 2 (90) with the gum arabic - water mixture 1 M NaOH solution,
30 minutes mixing (100) all the prepared materials together at 50-60°C at 1000 rpm,
Adjusting pH 3,5-4 (100) with 1 M acetic acid,
stabilization (120) of the complexes by resting at room temperature for 90 minutes,
Termination of the coacervation phase (130) by adjusting the pH to 9.5-10 with 1 M NaOH solution, lowering the temperature (140) to 5°C by leaving it in an ice bath,
60 min in an ice bath at 5°C. hardening (150) of the shells by waiting, Since two different crosslinkers are used, Splitting the Mixture into 2 Addition (170) of glutaraldehyde to one of the mixtures at 5°C and glyoxal to the other mixture at 5 °C,
120 minutes mixing (180), the mixtures at 1200-1500 rpm at room temperature and, it is the production of the mixtures at 4°C for 600 minutes with 6+ steps. - The invention is related to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, and its feature; impregnation of microcapsules on a 30 g/m2 melt blown nonwoven surface made of 100% polypropylene and it is the drying of the samples at room temperature (20 C° ± 2) for 8 hours and making them usable by applying them on textile surfaces. - The invention is related to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, and its feature; it is the fact that the textile surfaces on which it is applied have glyoxal-used microcapsules with a low level of toxicity, which ensures a higher antibacterial activity. - The invention is related to the application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials, and its feature; it has microcapsules produced from biodegradable natural materials by complex coacervation method, which provides a permanent antibacterial effect when applied to textile surfaces.
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TR2021/015962A TR2021015962A2 (en) | 2021-10-13 | 2021-10-13 | APPLICATION TO MICROCAPSULES AND TEXTILE MATERIALS WITH ANTIBACTERIAL PROPERTIES WITH EVOLUTIVE OIL OF EUCALYPTUS |
TR2021/015962 | 2021-10-13 |
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PCT/TR2022/051127 WO2023063915A1 (en) | 2021-10-13 | 2022-10-13 | Application of eucalyptus essential oil to microcapsules with antibacterial properties and textile materials |
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WO (1) | WO2023063915A1 (en) |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5043161A (en) * | 1989-08-31 | 1991-08-27 | Eurand America, Inc. | Small, oily, free-flowing, silky-smooth, talc-like, dry microcapsules and aqueous formulations containing them |
KR20030022542A (en) * | 2001-09-11 | 2003-03-17 | 주식회사 마이크로폴 | The preparation and it's application of antibacterial, deorder and fragrant microcapsules |
WO2019243425A1 (en) * | 2018-06-21 | 2019-12-26 | Firmenich Sa | Process for preparing microcapsules |
-
2021
- 2021-10-13 TR TR2021/015962A patent/TR2021015962A2/en unknown
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2022
- 2022-10-13 WO PCT/TR2022/051127 patent/WO2023063915A1/en unknown
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5043161A (en) * | 1989-08-31 | 1991-08-27 | Eurand America, Inc. | Small, oily, free-flowing, silky-smooth, talc-like, dry microcapsules and aqueous formulations containing them |
KR20030022542A (en) * | 2001-09-11 | 2003-03-17 | 주식회사 마이크로폴 | The preparation and it's application of antibacterial, deorder and fragrant microcapsules |
WO2019243425A1 (en) * | 2018-06-21 | 2019-12-26 | Firmenich Sa | Process for preparing microcapsules |
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