CN114108316B - Preparation method of antibacterial textile and antibacterial textile - Google Patents
Preparation method of antibacterial textile and antibacterial textile Download PDFInfo
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- CN114108316B CN114108316B CN202111522797.8A CN202111522797A CN114108316B CN 114108316 B CN114108316 B CN 114108316B CN 202111522797 A CN202111522797 A CN 202111522797A CN 114108316 B CN114108316 B CN 114108316B
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- Prior art keywords
- essential oil
- plant essential
- preparing
- fabric
- emulsion
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 51
- 239000004753 textile Substances 0.000 title claims abstract description 47
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000341 volatile oil Substances 0.000 claims abstract description 140
- 239000000839 emulsion Substances 0.000 claims abstract description 58
- 239000004744 fabric Substances 0.000 claims abstract description 53
- 239000003094 microcapsule Substances 0.000 claims abstract description 44
- 238000000576 coating method Methods 0.000 claims abstract description 37
- 239000011248 coating agent Substances 0.000 claims abstract description 36
- 239000004814 polyurethane Substances 0.000 claims abstract description 35
- 229920002635 polyurethane Polymers 0.000 claims abstract description 35
- 125000002091 cationic group Chemical group 0.000 claims abstract description 30
- 238000002156 mixing Methods 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 238000000034 method Methods 0.000 claims abstract description 17
- 238000001694 spray drying Methods 0.000 claims abstract description 17
- 241000196324 Embryophyta Species 0.000 claims description 88
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 51
- 239000008367 deionised water Substances 0.000 claims description 43
- 229910021641 deionized water Inorganic materials 0.000 claims description 43
- 238000003756 stirring Methods 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 32
- 238000001035 drying Methods 0.000 claims description 31
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 28
- 238000005406 washing Methods 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 22
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 21
- 239000012948 isocyanate Substances 0.000 claims description 21
- 150000002513 isocyanates Chemical class 0.000 claims description 21
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 20
- 229920000742 Cotton Polymers 0.000 claims description 18
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 17
- 229920000053 polysorbate 80 Polymers 0.000 claims description 17
- 239000000243 solution Substances 0.000 claims description 16
- 239000007921 spray Substances 0.000 claims description 15
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 14
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 14
- 235000003261 Artemisia vulgaris Nutrition 0.000 claims description 13
- 240000006891 Artemisia vulgaris Species 0.000 claims description 13
- 241000246358 Thymus Species 0.000 claims description 13
- 235000007303 Thymus vulgaris Nutrition 0.000 claims description 13
- 239000004359 castor oil Substances 0.000 claims description 13
- 235000019438 castor oil Nutrition 0.000 claims description 13
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 13
- 239000001585 thymus vulgaris Substances 0.000 claims description 13
- 239000004970 Chain extender Substances 0.000 claims description 12
- 230000001804 emulsifying effect Effects 0.000 claims description 12
- OMIGHNLMNHATMP-UHFFFAOYSA-N 2-hydroxyethyl prop-2-enoate Chemical group OCCOC(=O)C=C OMIGHNLMNHATMP-UHFFFAOYSA-N 0.000 claims description 11
- 150000001875 compounds Chemical class 0.000 claims description 11
- CRVGTESFCCXCTH-UHFFFAOYSA-N methyl diethanolamine Chemical group OCCN(C)CCO CRVGTESFCCXCTH-UHFFFAOYSA-N 0.000 claims description 11
- 239000005057 Hexamethylene diisocyanate Substances 0.000 claims description 10
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 10
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical group CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 10
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 10
- RRAMGCGOFNQTLD-UHFFFAOYSA-N hexamethylene diisocyanate Chemical compound O=C=NCCCCCCN=C=O RRAMGCGOFNQTLD-UHFFFAOYSA-N 0.000 claims description 10
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 10
- 239000002562 thickening agent Substances 0.000 claims description 10
- 239000012875 nonionic emulsifier Substances 0.000 claims description 8
- 229960000583 acetic acid Drugs 0.000 claims description 7
- 239000012874 anionic emulsifier Substances 0.000 claims description 7
- FOCAUTSVDIKZOP-UHFFFAOYSA-N chloroacetic acid Chemical compound OC(=O)CCl FOCAUTSVDIKZOP-UHFFFAOYSA-N 0.000 claims description 7
- 229940106681 chloroacetic acid Drugs 0.000 claims description 7
- 239000012362 glacial acetic acid Substances 0.000 claims description 7
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 7
- 230000002572 peristaltic effect Effects 0.000 claims description 7
- 238000004321 preservation Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 7
- 239000002904 solvent Substances 0.000 claims description 7
- 239000002981 blocking agent Substances 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000003054 catalyst Substances 0.000 claims description 5
- 230000000845 anti-microbial effect Effects 0.000 claims description 4
- 239000004599 antimicrobial Substances 0.000 claims description 4
- 238000002347 injection Methods 0.000 claims description 4
- 239000007924 injection Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 125000000524 functional group Chemical group 0.000 claims description 3
- 238000010025 steaming Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 150000002009 diols Chemical class 0.000 claims 1
- 125000000129 anionic group Chemical group 0.000 abstract description 17
- 239000002131 composite material Substances 0.000 abstract description 13
- 239000003995 emulsifying agent Substances 0.000 abstract description 12
- 241000222122 Candida albicans Species 0.000 abstract description 4
- 241000588724 Escherichia coli Species 0.000 abstract description 4
- 241000191967 Staphylococcus aureus Species 0.000 abstract description 4
- 229940095731 candida albicans Drugs 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 description 20
- 230000000052 comparative effect Effects 0.000 description 18
- 239000011259 mixed solution Substances 0.000 description 10
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 238000004945 emulsification Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 238000006386 neutralization reaction Methods 0.000 description 4
- 238000002390 rotary evaporation Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 241000628997 Flos Species 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000003945 anionic surfactant Substances 0.000 description 3
- 239000002736 nonionic surfactant Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- -1 aldehyde ketone Chemical class 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000009257 reactivity Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 150000003505 terpenes Chemical class 0.000 description 2
- 235000007586 terpenes Nutrition 0.000 description 2
- PTBDIHRZYDMNKB-UHFFFAOYSA-N 2,2-Bis(hydroxymethyl)propionic acid Chemical compound OCC(C)(CO)C(O)=O PTBDIHRZYDMNKB-UHFFFAOYSA-N 0.000 description 1
- OZICRFXCUVKDRG-UHFFFAOYSA-N 2-[2-hydroxyethyl(propyl)amino]ethanol Chemical compound CCCN(CCO)CCO OZICRFXCUVKDRG-UHFFFAOYSA-N 0.000 description 1
- 240000005209 Canarium indicum Species 0.000 description 1
- 235000009024 Ceanothus sanguineus Nutrition 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 244000131522 Citrus pyriformis Species 0.000 description 1
- 239000004593 Epoxy Chemical class 0.000 description 1
- 244000178870 Lavandula angustifolia Species 0.000 description 1
- 235000010663 Lavandula angustifolia Nutrition 0.000 description 1
- 240000003553 Leptospermum scoparium Species 0.000 description 1
- 235000015459 Lycium barbarum Nutrition 0.000 description 1
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 1
- AKNUHUCEWALCOI-UHFFFAOYSA-N N-ethyldiethanolamine Chemical compound OCCN(CC)CCO AKNUHUCEWALCOI-UHFFFAOYSA-N 0.000 description 1
- 229920001214 Polysorbate 60 Polymers 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical compound C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Chemical class 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 150000001298 alcohols Chemical class 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 125000002057 carboxymethyl group Chemical group [H]OC(=O)C([H])([H])[*] 0.000 description 1
- 150000001768 cations Chemical group 0.000 description 1
- 229960002887 deanol Drugs 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000012972 dimethylethanolamine Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229930004069 diterpene Natural products 0.000 description 1
- 125000000567 diterpene group Chemical group 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000004862 elemi Substances 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000675 fabric finishing Substances 0.000 description 1
- 238000009962 finishing (textile) Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 150000002576 ketones Chemical class 0.000 description 1
- 239000001102 lavandula vera Substances 0.000 description 1
- 235000018219 lavender Nutrition 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229930003658 monoterpene Natural products 0.000 description 1
- 150000002773 monoterpene derivatives Chemical class 0.000 description 1
- 235000002577 monoterpenes Nutrition 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229940051841 polyoxyethylene ether Drugs 0.000 description 1
- 229920000056 polyoxyethylene ether Polymers 0.000 description 1
- 239000001267 polyvinylpyrrolidone Substances 0.000 description 1
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 description 1
- 229920000036 polyvinylpyrrolidone Polymers 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229930004725 sesquiterpene Natural products 0.000 description 1
- 150000004354 sesquiterpene derivatives Chemical class 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- WBHQBSYUUJJSRZ-UHFFFAOYSA-M sodium bisulfate Chemical compound [Na+].OS([O-])(=O)=O WBHQBSYUUJJSRZ-UHFFFAOYSA-M 0.000 description 1
- 229910000342 sodium bisulfate Inorganic materials 0.000 description 1
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 description 1
- 229940001584 sodium metabisulfite Drugs 0.000 description 1
- 235000010262 sodium metabisulphite Nutrition 0.000 description 1
- DAJSVUQLFFJUSX-UHFFFAOYSA-M sodium;dodecane-1-sulfonate Chemical compound [Na+].CCCCCCCCCCCCS([O-])(=O)=O DAJSVUQLFFJUSX-UHFFFAOYSA-M 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
-
- 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
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
-
- 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
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/184—Carboxylic acids; Anhydrides, halides or salts thereof
- D06M13/207—Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
- D06M13/21—Halogenated carboxylic acids; Anhydrides, halides or salts 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
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- 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
- D06M2101/02—Natural fibres, other than mineral fibres
- D06M2101/04—Vegetal fibres
- D06M2101/06—Vegetal fibres cellulosic
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Biochemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention belongs to the technical field of textile, and particularly relates to a preparation method of an antibacterial textile and the antibacterial textile. The preparation method of the invention comprises the following steps: preparing plant essential oil emulsion by adopting an anionic/nonionic composite emulsifier; preparing end-capped cationic aqueous polyurethane emulsion; mixing the plant essential oil emulsion and the polyurethane emulsion to prepare a plant essential oil microcapsule in a spray drying mode; and coating the coating finishing liquid prepared by the plant essential oil microcapsules on the fabric in a coating mode. The antibacterial textile prepared by the method has excellent broad-spectrum antibacterial property on staphylococcus aureus, escherichia coli, candida albicans and the like, and can still keep good antibacterial effect after being washed for a plurality of times.
Description
Technical Field
The invention relates to the technical field of textile, in particular to a preparation method of an antibacterial textile and the antibacterial textile.
Background
The plant essential oil is a general term for oily liquid substances with high volatility and small molecular weight extracted from flowers, leaves, bark, fruits, seeds, roots and other parts of plants by distillation, freezing and squeezing, extraction and other modes. The main components of the plant essential oil comprise: terpenes (monoterpenes, sesquiterpenes and diterpenes), alcohols, aldehydes, acids, esters, ketones, epoxy compounds, amines, sulfur compounds and the like. Research shows that the micromolecular phenols, terpenes and aldehyde ketone substances in the plant essential oil have obvious antibacterial activity. However, the essential oil has the characteristics of containing unsaturated bonds, being volatile and the like, so that the essential oil has the defects of short fragrance retention time, uncontrollable release and the like, is inconvenient to store, transport, diversify pharmaceutical dosage forms and the like, is easy to deteriorate due to the influence of factors such as light, heat, air and the like, and limits the action effect and the application range of the essential oil. Particularly, when the fabric is applied in the textile field, the problem of difficult application exists, and the fabric treated by the essential oil is repeatedly washed and dried in the use process, so that the fragrance loss is large, and the effect cannot last.
Disclosure of Invention
In view of the shortcomings of the prior art, the invention provides a preparation method of an antibacterial textile and the antibacterial textile, so that the textile has broad-spectrum antibacterial property on common staphylococcus aureus, escherichia coli, candida albicans and the like.
To achieve the above and other related objects, the present invention provides a method for preparing an antibacterial textile, comprising the steps of:
preparing plant essential oil emulsion by adopting an anionic/nonionic composite emulsifier;
preparing end-capped cationic aqueous polyurethane emulsion;
adding the plant essential oil emulsion into the blocked cationic aqueous polyurethane emulsion, uniformly dispersing, and preparing plant essential oil microcapsules by a spray drying method;
preparing a coating finishing liquid by adopting the plant essential oil microcapsule; and
And coating the coating finishing liquid on the fabric to obtain the antibacterial textile.
In one example of the invention, preparing a plant essential oil emulsion comprises: firstly, adding an anionic/nonionic composite emulsifier into deionized water, and stirring until the anionic/nonionic composite emulsifier is completely dissolved; and adding plant essential oil, emulsifying for 1h at a high speed at 40 ℃ to obtain stable O/W type plant essential oil emulsion, wherein the mass of the anionic/nonionic composite emulsifier is 5-10 wt% of the mass of the plant essential oil.
In an example of the present invention, the anionic/nonionic composite emulsifier includes Tween 80 (Tween-80) and sodium dodecyl sulfate, and the mass ratio of Tween 80 to sodium dodecyl sulfate is 1:1-3:1.
In an example of the invention, the plant essential oil is a compound plant essential oil comprising thyme essential oil and mugwort essential oil, and the mass ratio of thyme essential oil to mugwort essential oil is 1:1-1:3.
In one example of the invention, the step of preparing the capped cationic aqueous polyurethane emulsion comprises: the preparation method of the end-capped cationic aqueous polyurethane emulsion comprises the following steps: placing castor oil modified dihydric alcohol into a container, and decompressing and dehydrating for 1-2 h; adding hexamethylene diisocyanate, mixing and stirring uniformly at 40-50 ℃, adding a catalyst, and reacting for 60-120 min at 40-70 ℃; dripping 1, 4-butanediol and isophorone diisocyanate, mixing and stirring to react for 1-2 h at 70 ℃; dropwise adding a cationic chain extender to react for 1-2 h; acetone is used as a solvent, and reflux heat preservation is carried out until the NCO amount reaches a theoretical value; cooling to 40-50 ℃, adding a blocking agent, and reacting for 2-3 h; adding glacial acetic acid to neutralize until the PH is 6-7, adding deionized water to emulsify under strong stirring, and stirring for 60-90 min; and (5) rotary steaming and removing acetone.
In one example of the invention, the castor oil modified glycol has a hydroxyl number of 180mg KOH/g; the molar ratio of the functional group NCO in the hexamethylene diisocyanate and the isophorone diisocyanate to the functional group OH in the castor oil modified dihydric alcohol and the 1, 4-butanediol is 1.2-1.4.
In an example of the invention, the catalyst is dibutyl tin dilaurate, the cationic chain extender is N-methyldiethanolamine, the end capping agent is hydroxyethyl acrylate, and the addition amount of the dibutyl tin dilaurate is 0.5-1.0 wt% of the total mass of dihydric alcohol and isocyanate in the system; the addition amount of the N-methyldiethanolamine is 3-6wt% of the total mass of the dihydric alcohol and the isocyanate in the system; the adding amount of the hydroxyethyl acrylate is 1.0 to 1.5 weight percent of the total mass of the dihydric alcohol and the isocyanate in the system.
In an example of the invention, when preparing the plant essential oil microcapsule, the mass ratio of the blocked cationic aqueous polyurethane emulsion to the plant essential oil emulsion is 1:1-2:1, the inlet temperature during spray drying is 160-180 ℃, the peristaltic pump sample injection amount is set to 5-10 mL/min during spray drying, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h。
In an example of the invention, the plant essential oil microcapsule is firstly dispersed in deionized water when preparing the coating finishing liquid, and then the thickening agent is added and stirred uniformly, wherein the addition amount of the thickening agent accounts for 3-wt% of the total mass of the system, and the mass of the plant essential oil microcapsule accounts for 10-30wt% of the total mass of the system.
In one example of the invention, the fabric is a carboxymethylated cotton fabric.
In one example of the invention, the step of carboxymethylation treatment comprises: padding the fabric in caustic soda solution with the mass fraction of 25-30%, wherein the padding is carried out twice, and the padding residual rate is 80-90%; taking out the fabric, and drying the fabric in a 60 ℃ oven for 5-10 min; immersing the fabric subjected to alkali treatment into chloroacetic acid solution with the mass fraction of 15-25%, and reacting for 30-50 min at 60-70 ℃; and taking out the fabric, washing the fabric with deionized water for 3-5 times, and drying the fabric at 60-80 ℃.
The invention also provides an antibacterial textile prepared by the preparation method.
The invention adopts an anionic/nonionic emulsifier to prepare O/W plant essential oil emulsion, then utilizes the electrostatic action between the end-capped cationic aqueous polyurethane and the plant essential oil emulsion to enable the aqueous polyurethane to be adsorbed on the surface of the plant essential oil emulsion, and then adopts a spray drying mode to prepare plant essential oil microcapsules; the plant essential oil microcapsules are treated on the textile in a coating finishing mode, and the excellent washing fastness of the antibacterial textile is endowed by utilizing the electrostatic effect between part of carboxymethylated cotton fabrics and the plant essential oil microcapsules and the reactivity of the end-capped cationic aqueous polyurethane in the high-temperature baking process, so that the antibacterial textile has a long-term effect.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described, it being obvious that the drawings in the following description are only some embodiments of the invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a flow chart of a method of making an antimicrobial textile of the present invention;
Detailed Description
Other advantages and effects of the present invention will become apparent to those skilled in the art from the following disclosure, which describes the embodiments of the present invention with reference to specific examples. The invention may be practiced or carried out in other embodiments that depart from the specific details, and the details of the present description may be modified or varied from the spirit and scope of the present invention. It should be noted that the following embodiments and features in the embodiments may be combined with each other without conflict. It is also to be understood that the terminology used in the examples of the invention is for the purpose of describing particular embodiments only, and is not intended to limit the scope of the invention. The test methods in the following examples, in which specific conditions are not noted, are generally conducted under conventional conditions or under conditions recommended by the respective manufacturers.
It should be understood that the terms such as "upper," "lower," "left," "right," "middle," and "a" and the like are used in this specification for descriptive purposes only and not for purposes of limitation, and that the invention may be practiced without materially departing from the novel teachings and without departing from the scope of the invention.
Referring to fig. 1, the present invention provides a method for preparing an antibacterial textile, which has excellent broad-spectrum antibacterial properties against staphylococcus aureus, escherichia coli, candida albicans, etc.
Referring to fig. 1, the present invention provides a method for preparing an antibacterial textile, comprising the following steps:
s1, preparing a plant essential oil emulsion by adopting an anionic/nonionic composite emulsifier;
s2, preparing end-capped cationic aqueous polyurethane emulsion;
s3, adding the plant essential oil emulsion into the end-capped cationic aqueous polyurethane emulsion, uniformly dispersing, and preparing a plant essential oil microcapsule in a spray drying mode;
s4, preparing a coating finishing liquid by adopting plant essential oil microcapsules;
s5, coating the coating finishing liquid on the fabric to obtain the antibacterial textile.
Referring to fig. 1, the preparation of the plant essential oil emulsion in step S1 specifically includes the following steps: adding the anionic/nonionic composite emulsifier into deionized water, and stirring until the anionic/nonionic composite emulsifier is completely dissolved to form a water phase; adding plant essential oil, and emulsifying at 40 deg.C for 1 hr to obtain stable O/W emulsion. Wherein the mass of the anionic/nonionic composite emulsifier is 5-10wt% of the mass of the plant essential oil. The anionic/nonionic composite emulsifier comprises an anionic surfactant and a nonionic surfactant, wherein the anionic surfactant can be sodium dodecyl sulfonate, sodium alkyl polyoxyethylene ether sulfate and the like, and the nonionic surfactant can be Tween 80, tween 60, polyvinylpyrrolidone and the like, wherein the mass ratio of the nonionic surfactant to the anionic surfactant is 1:1-3:1. In some embodiments, the anionic/nonionic composite emulsifier is a combination of Tween 80 and sodium dodecyl sulfate, wherein the mass ratio of Tween 80 to sodium dodecyl sulfate is 1:1 to 3:1, for example, 1:1, 2:1, or 3:1, etc. can be selected. The plant essential oil can be selected from one or more of flos Matricariae Chamomillae essential oil, flos Lonicerae essential oil, tea tree essential oil, lavender essential oil, herba Menthae essential oil, colophonium essential oil, herba Pogostemonis essential oil, thyme essential oil, mugwort essential oil, lemon essential oil, fructus Amomi rotundus essential oil, fructus Foeniculi essential oil, flos Caryophylli essential oil, and elemi essential oil. Preferably, the plant essential oil is compound plant essential oil composed of thyme essential oil and mugwort essential oil, wherein the mass ratio of thyme essential oil to mugwort essential oil is 1:1-1:3, for example, 1:1, 1:2 or 1:3 can be selected.
Referring to fig. 1, the preparation of the end-capping cationic aqueous polyurethane emulsion in step S2 specifically includes: placing castor oil modified dihydric alcohol into a three-neck flask with a temperature control, stirring and condensing device, and decompressing and dehydrating for 1-2 h at 110 ℃; cooling to 40 ℃, adding hexamethylene diisocyanate, stirring and mixing for 20min, adding dibutyltin dilaurate serving as a catalyst, heating to 50 ℃ for reaction for 30-60 min, and continuously heating to 70 ℃ for reaction for 30-60 min; cooling to 40 ℃, dropwise adding 1, 4-butanediol and isophorone diisocyanate, uniformly mixing after the dropwise adding, and heating to 70 ℃ for reacting for 1-2 hours; then cooling to 40 ℃, dropwise adding a cationic chain extender, after the dropwise adding is completed, uniformly mixing, heating to 80 ℃ for reaction for 1-2 h, taking acetone as a solvent, and refluxing at 60 ℃ for heat preservation until the NCO value is theoretical; cooling to 40 ℃, adding a blocking agent, reacting for 2-3 hours, and adding glacial acetic acid to neutralize until the PH value is 6-7; then adding deionized water under strong stirring, emulsifying and stirring for 60-90 min, wherein the mass ratio of the deionized water to the mixed materials is 4:1; finally, spin steaming is carried out, and acetone is removed, thus obtaining the polyurethane emulsion.
Wherein, the cation chain extender can be selected from one or a combination of a plurality of N-methyl diethanol amine, triethanolamine, N-ethyl diethanol amine, N-propyl diethanol amine and dimethyl ethanol amine, and the end capping agent can be selected from one or a combination of a plurality of hydroxyethyl acrylate, sodium bisulfate, ammonium bisulfate, sodium metabisulfite and hydroxyethyl caprolactone acrylate. The hydroxyl value of the castor oil modified dihydric alcohol is 180mg KOH/g; the molar ratio of functional groups NCO in hexamethylene diisocyanate and isophorone diisocyanate to functional groups OH in castor oil modified dihydric alcohol and 1, 4-butanediol is 1.2-1.4. The addition amount of the dibutyl tin dilaurate is 0.5-1.0% of the total mass of the dihydric alcohol and the isocyanate in the system; the addition amount of the N-methyl diethanolamine is 3-6% of the total mass of the dihydric alcohol and the isocyanate in the system; the adding amount of the end capping agent hydroxyethyl acrylate is 1.0 to 1.5 percent of the total mass of the dihydric alcohol and the isocyanate in the system.
Referring to fig. 1, the preparation of the plant essential oil microcapsule in step S3 specifically includes the following steps: adding the plant essential oil emulsion prepared in the step S1 into the blocked cationic aqueous polyurethane emulsion prepared in the step S2, and dispersing at a high speed for 1h to obtain a mixed solution; and then will beInjecting the mixed solution into a spray dryer for spray drying, collecting spray dried powder, washing with deionized water for 3-5 times, and drying at 40-60 ℃ to obtain the plant essential oil microcapsule. Wherein the mass ratio of the blocked cationic aqueous polyurethane emulsion to the plant essential oil emulsion is 1:1-2:1, the inlet temperature of spray drying is 160-180 ℃, the peristaltic pump sample injection amount of spray drying is set to 5-10 mL/min, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h。
Referring to fig. 1, the preparation of the coating finishing liquid in step S4 specifically includes: and (3) adding the plant essential oil microcapsule prepared in the step (S3) into deionized water for uniform dispersion, and then adding a thickening agent for uniform mixing and stirring to obtain the coating finishing liquid. Wherein, the content of the plant essential oil microcapsule in the coating finishing liquid is 10 to 30 weight percent, and the addition amount of the thickener is 3 weight percent of the total mass of the system.
Referring to FIG. 1, step S5 is to uniformly coat the coating finishing liquid prepared in step S4 on a fabric by adopting a dry coating method, pre-bake for 5-10 min at 70-80 ℃, and then bake for 3-5 min at 110-120 ℃; washing with deionized water for 3-5 times, and drying at 60-80 ℃ to obtain the antibacterial textile. Preferably, the fabric in step S5 is a cotton fabric subjected to a partial carboxymethylation treatment, and the specific steps of the carboxymethylation treatment include: firstly padding cotton fabrics in caustic soda solution with the mass fraction of 25-30%, wherein the padding is carried out two by two, the padding residual rate is 80-90%, taking out the fabrics, and drying in a 60 ℃ oven for 5-10 min; and immersing the fabric subjected to alkali treatment into chloroacetic acid solution with the mass fraction of 15-25%, reacting for 30-50 min at 60-70 ℃, taking out, washing with deionized water for 3-5 times, and drying at 60-80 ℃.
The invention is illustrated in detail below by means of several specific examples. The drugs used in the following examples are all commercially available.
Example 1
(1) Adding Tween 80 and sodium dodecyl sulfate into deionized water according to a mass ratio of 1:1, stirring and dissolving to form a water phase, adding compound plant essential oil consisting of thyme essential oil and mugwort essential oil according to a mass ratio of 1:1, and emulsifying at a high speed by adopting a high-shear dispersing emulsifying machine for 1h at 40 ℃ to obtain stable O/W type emulsion, wherein the sum of the masses of Tween 80 and sodium dodecyl sulfate accounts for 5% of the quality of the compound plant essential oil;
(2) Placing 0.5mol of castor oil modified dihydric alcohol with a hydroxyl value of 180mg KOH/g into a three-neck flask with a temperature control, stirring and condensing device, decompressing and dehydrating for 1h at 110 ℃, cooling to 40 ℃, adding 0.6mol of hexamethylene diisocyanate, stirring and mixing for 20min, adding 0.5wt% (relative to the total mass of dihydric alcohol and isocyanate in the system) of dibutyltin dilaurate, heating to 50 ℃ for reacting for 30min, continuously heating to 70 ℃ for reacting for 30min, cooling to 40 ℃, slowly dropwise adding 0.5mol of 1, 4-butanediol and 0.6mol of isophorone diisocyanate, and heating to 70 ℃ for reacting for 1h after the dropwise adding is completed and mixing is uniform; then cooling to 40 ℃, slowly dripping 3wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of cationic chain extender N-methyldiethanolamine, uniformly mixing, heating to 80 ℃ for reaction for 1h, taking acetone as a solvent, refluxing at 60 ℃ for heat preservation until the NCO amount is close to a theoretical value, cooling to 40 ℃, adding 1.0wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of blocking agent hydroxyethyl acrylate, reacting for 2h, adding glacial acetic acid for neutralization for 5min, adding deionized water for emulsification (the mass ratio of deionized water to the mixture is 4:1) under strong stirring, stirring for 60min, and finally performing rotary evaporation to remove acetone to obtain polyurethane emulsion;
(3) Mixing the plant essential oil emulsion obtained in the step (1) with the aqueous polyurethane emulsion obtained in the step (2) in a mass ratio of 1:1, and dispersing at a high speed for 1h to obtain a mixed solution; after the inlet temperature of a spray dryer reaches 160 ℃, spray drying the mixed solution, collecting the obtained spray dried powder, washing with deionized water for 3 times, and drying at 40 ℃ to obtain plant essential oil microcapsule, wherein the feeding amount of a peristaltic pump is 5mL/min, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h；
(4) Weighing the plant essential oil microcapsule obtained in the step (3), dispersing the plant essential oil microcapsule by deionized water, adding 3wt% of thickener (relative to the total mass of the system), stirring and mixing uniformly by using a glass rod, and preparing coating finishing liquid with the mass fraction of 10wt% of the essential oil microcapsule; then uniformly coating the coating finishing liquid on the cotton fabric subjected to carboxymethylation treatment by adopting a dry coating mode, pre-baking for 10min at 70 ℃, baking for 5min at 110 ℃, washing for 3 times by using deionized water, and drying at 60 ℃ to obtain the antibacterial textile;
wherein, the specific steps of the carboxymethylation treatment of cotton fabric are as follows: padding cotton fabrics with caustic soda solution with the mass fraction of 25%, padding two by two, wherein the padding residual rate is 80%, taking out the fabrics, and drying in a 60 ℃ oven for 5min; immersing in 15% chloroacetic acid solution, reacting at 60 ℃ for 50min, taking out, washing with deionized water for 3 times, and drying at 60 ℃.
Example 2
(1) Adding Tween 80 and sodium dodecyl sulfate into deionized water according to a mass ratio of 3:1, stirring and dissolving to form a water phase, adding compound plant essential oil consisting of thyme essential oil and mugwort essential oil according to a mass ratio of 1:3, and emulsifying at a high speed by adopting a high-shear dispersing emulsifying machine for 1h at 40 ℃ to obtain stable O/W type emulsion, wherein the sum of the masses of Tween 80 and sodium dodecyl sulfate accounts for 10% of the quality of the compound plant essential oil;
(2) Placing 0.5mol of castor oil modified dihydric alcohol with a hydroxyl value of 180mg KOH/g into a three-neck flask with a temperature control, stirring and condensing device, decompressing and dehydrating for 2h at 110 ℃, cooling to 40 ℃, adding 0.7mol of hexamethylene diisocyanate, stirring and mixing for 20min, adding 1wt% (relative to the total mass of dihydric alcohol and isocyanate in the system) of dibutyltin dilaurate, heating to 50 ℃ for reacting for 60min, continuously heating to 70 ℃ for reacting for 60min, cooling to 40 ℃, slowly dropwise adding 0.5mol of 1, 4-butanediol and 0.7mol of isophorone diisocyanate, uniformly mixing, and heating to 70 ℃ for reacting for 2h; then cooling to 40 ℃, slowly dripping 6wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of cationic chain extender N-methyldiethanolamine, uniformly mixing, heating to 80 ℃ for reaction for 2 hours, taking acetone as a solvent, refluxing at 60 ℃ for heat preservation until the NCO amount is close to a theoretical value, cooling to 40 ℃, adding 1.5wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of blocking agent hydroxyethyl acrylate, reacting for 3 hours, adding glacial acetic acid for neutralization for 10 minutes, adding deionized water for emulsification (the mass ratio of deionized water to the mixture is 4:1) under strong stirring, stirring for 90 minutes, and finally performing rotary evaporation to remove acetone to obtain polyurethane emulsion;
(3) Mixing the plant essential oil emulsion obtained in the step (1) with the aqueous polyurethane emulsion obtained in the step (2) in a mass ratio of 1:2, and dispersing at a high speed for 1h to obtain a mixed solution; after the inlet temperature of a spray dryer reaches 180 ℃, spray drying the mixed solution, collecting the obtained spray dried powder, washing with deionized water for 5 times, and drying at 60 ℃ to obtain plant essential oil microcapsule, wherein the feeding amount of a peristaltic pump is 10mL/min, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h；
(4) Weighing the plant essential oil microcapsule obtained in the step (3), dispersing the plant essential oil microcapsule by deionized water, adding 3wt% of thickener (relative to the total mass of the system), stirring and mixing uniformly by using a glass rod, and preparing a coating finishing liquid with the mass fraction of 30wt% of the essential oil microcapsule; then uniformly coating the coating finishing liquid on the cotton fabric subjected to carboxymethylation treatment by adopting a dry coating mode, pre-baking for 5min at 80 ℃, baking for 3min at 130 ℃, washing for 5 times by using deionized water, and drying at 80 ℃ to obtain the antibacterial textile;
wherein, the specific steps of the carboxymethylation treatment of cotton fabric are as follows: padding cotton fabrics with caustic soda solution with the mass fraction of 30%, padding two by two, wherein the padding residual rate is 90%, taking out the fabrics, and drying in a 60 ℃ oven for 10min; immersing in 25% chloroacetic acid solution, reacting at 70 ℃ for 30min, taking out, washing with deionized water for 5 times, and drying at 80 ℃.
Example 3
(1) Adding Tween 80 and sodium dodecyl sulfate into deionized water according to a mass ratio of 2:1, stirring and dissolving to form a water phase, adding compound plant essential oil consisting of thyme essential oil and mugwort essential oil according to a mass ratio of 1:2, and emulsifying at a high speed by adopting a high-shear dispersing emulsifying machine for 1h at 40 ℃ to obtain stable O/W type emulsion, wherein the sum of the masses of Tween 80 and sodium dodecyl sulfate accounts for 6% of the mass of the plant essential oil;
(2) Placing 0.5mol of castor oil modified dihydric alcohol with a hydroxyl value of 180mg KOH/g into a three-neck flask with a temperature control, stirring and condensing device, decompressing and dehydrating at 110 ℃ for 1.5h, cooling to 40 ℃, adding 0.65mol of hexamethylene diisocyanate, stirring and mixing for 20min, adding 0.6wt% (relative to the total mass of dihydric alcohol and isocyanate in the system) of dibutyltin dilaurate, heating to 50 ℃ for reacting for 45min, continuously heating to 70 ℃ for reacting for 45min, cooling to 40 ℃, slowly dropwise adding 0.5mol of 1, 4-butanediol and 0.65mol of isophorone diisocyanate, uniformly mixing, and heating to 70 ℃ for reacting for 1.5h; then cooling to 40 ℃, slowly dripping 4wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of cationic chain extender N-methyldiethanolamine, uniformly mixing, heating to 80 ℃ for reaction for 1.5 hours, taking acetone as a solvent, refluxing at 60 ℃ for heat preservation until the NCO amount is close to a theoretical value, cooling to 40 ℃, adding 1.2wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of end-capping agent hydroxyethyl acrylate, reacting for 2 hours, adding glacial acetic acid for neutralization for 5 minutes, adding deionized water for emulsification (the mass ratio of the deionized water to the mixture is 4:1) under strong stirring, stirring for 75 minutes, and finally performing rotary evaporation and acetone removal to obtain polyurethane emulsion;
(3) Mixing the plant essential oil emulsion obtained in the step (1) with the aqueous polyurethane emulsion obtained in the step (2) in a mass ratio of 1:1.5, and dispersing at a high speed for 1h to obtain a mixed solution; after the inlet temperature of a spray dryer reaches 170 ℃, spray-drying the mixed solution, collecting the obtained spray-dried powder, washing the powder with deionized water for 4 times, and drying at 50 ℃ to obtain plant essential oil microcapsules, wherein the sample injection amount of a peristaltic pump is 6mL/min, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h；
(4) Weighing the plant essential oil microcapsule obtained in the step (3), dispersing the plant essential oil microcapsule by deionized water, adding 3wt% of thickener (relative to the total mass of the system), stirring and mixing uniformly by using a glass rod, and preparing a coating finishing liquid with the mass fraction of 20wt% of the essential oil microcapsule; then uniformly coating the coating finishing liquid on the cotton fabric subjected to carboxymethylation treatment by adopting a dry coating mode, pre-baking for 6min at 75 ℃, baking for 4min at 120 ℃, washing for 4 times by using deionized water, and drying at 70 ℃ to obtain the antibacterial textile;
wherein, the specific steps of the carboxymethylation treatment of cotton fabric are as follows: padding cotton fabrics with 28% caustic soda solution by mass fraction, padding two by two, wherein the padding residual rate is 85%, taking out the fabrics, and drying in a 60 ℃ oven for 6min; immersing in 20% chloroacetic acid solution, reacting at 65 ℃ for 40min, taking out, washing with deionized water for 4 times, and drying at 70 ℃.
Example 4
(1) Adding Tween 80 and sodium dodecyl sulfate into deionized water according to the mass ratio of 2.5:1, stirring and dissolving to form a water phase, adding compound plant essential oil consisting of thyme essential oil and mugwort essential oil according to the mass ratio of 1:2.5, and emulsifying at a high speed by adopting a high-shear dispersing emulsifying machine for 1h at 40 ℃ to obtain stable O/W type emulsion, wherein the sum of the masses of Tween 80 and sodium dodecyl sulfate accounts for 8% of the mass of the compound plant essential oil;
(2) Placing 0.5mol of castor oil modified dihydric alcohol with a hydroxyl value of 180mg KOH/g into a three-neck flask with a temperature control, stirring and condensing device, decompressing and dehydrating for 2h at 110 ℃, cooling to 40 ℃, adding 0.6mol of hexamethylene diisocyanate, stirring and mixing for 20min, adding 0.8wt% (relative to the total mass of dihydric alcohol and isocyanate in the system) of dibutyltin dilaurate, heating to 50 ℃ for reacting for 40min, continuously heating to 70 ℃ for reacting for 40min, cooling to 40 ℃, slowly dropwise adding 0.5mol of 1, 4-butanediol and 0.65mol of isophorone diisocyanate, uniformly mixing, and heating to 70 ℃ for reacting for 2h; then cooling to 40 ℃, slowly dripping 5wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of cationic chain extender N-methyldiethanolamine, uniformly mixing, heating to 80 ℃ for reaction for 1h, taking acetone as a solvent, refluxing at 60 ℃ for heat preservation until the NCO amount is close to a theoretical value, cooling to 40 ℃, adding 1.4wt% (relative to the total mass of the dihydric alcohol and the isocyanate in the system) of blocking agent hydroxyethyl acrylate, reacting for 3h, adding glacial acetic acid for neutralization for 8min, adding deionized water for emulsification (the mass ratio of deionized water to the mixture is 4:1) under strong stirring, stirring for 70min, and finally performing rotary evaporation to remove acetone to obtain polyurethane emulsion;
(3) Mixing the plant essential oil emulsion obtained in the step (1) with the aqueous polyurethane emulsion obtained in the step (2) in a mass ratio of 1:1.2, and dispersing at a high speed for 1h to obtain a mixed solution; in spray dryingAfter the inlet temperature of the machine reaches 165 ℃, spray-drying the mixed solution, collecting the obtained spray-dried powder, washing the powder with deionized water for 3 times, and drying at 40 ℃ to obtain the plant essential oil microcapsule, wherein the feeding amount of a peristaltic pump is 8mL/min, the spray air pressure is 0.1MPa, and the drying air flow is 100m 3 /h；
(4) Weighing the plant essential oil microcapsule obtained in the step (3), dispersing the plant essential oil microcapsule by deionized water, adding 3wt% of thickener (relative to the total mass of the system), stirring and mixing uniformly by using a glass rod, and preparing a coating finishing liquid with the mass fraction of 25wt% of the essential oil microcapsule; then uniformly coating the coating finishing liquid on the cotton fabric subjected to carboxymethylation treatment by adopting a dry coating mode, pre-baking for 8min at 70 ℃, baking for 3.5min at 125 ℃, washing for 3 times by deionized water, and drying at 65 ℃ to obtain the antibacterial textile;
wherein, the specific steps of the carboxymethylation treatment of cotton fabric are as follows: padding cotton fabrics with 28% caustic soda solution by mass fraction, padding two by two, taking out the fabrics, and drying in a 60 ℃ oven for 8min; immersing in 18% chloroacetic acid solution, reacting at 68 ℃ for 45min, taking out, washing with deionized water for 3 times, and drying at 65 ℃.
Comparative example 1
The difference between this comparative example and example 1 is that: the cationic chain extender N-methyldiethanolamine from step (2) of example 1 was replaced with the anionic chain extender dimethylolpropionic acid.
Comparative example 2
The difference between this comparative example and example 1 is that: and (3) no end-capping agent hydroxyethyl acrylate is added in the step (2).
Comparative example 3
The difference between this comparative example and example 1 is that: the plant essential oil in the step (1) is thyme essential oil.
Comparative example 4
The difference between this comparative example and example 1 is that: the plant essential oil in the step (1) is mugwort essential oil.
Comparative example 5
The difference between this comparative example and example 1 is that: in step (1), only Tween 80 was used for emulsification.
Comparative example 6
The difference between this comparative example and example 1 is that: the fabric in step (4) is not carboxymethylated.
Antibacterial property test and antibacterial effect wash resistance test were performed on examples 1 to 4 and comparative examples 1 to 6, in which antibacterial property test: the antibacterial property of the finished fabric is measured according to GB/T20944.2-2007 evaluation of antibacterial property of textiles part 2 absorption method; antibacterial effect wash resistance test: washing was carried out according to test conditions A1M in GB/T12490-1990 using ECE standard detergents, the end of the washing being taken as 5 washes (corresponding to the specific operating conditions and steps of 5 washes: 40 ℃,150mL of solution, 10 beads, 45min, after washing, the sample was taken out and washed 2 times in 100mL of water at 40 ℃ for 1min each time). After the prescribed number of washing times was reached, the sample was thoroughly washed with water and dried. The results of the measurements are shown in Table 1.
Table 1: antibacterial property test
As can be seen from Table 1, the antibacterial textile obtained by the invention has excellent antibacterial property to Escherichia coli, staphylococcus aureus and Candida albicans, and has excellent washing fastness. In the comparative example 1, the anionic aqueous polyurethane is adopted to coat the plant essential oil, and the encapsulation rate of the microcapsule is not high due to the repulsive force between the essential oil emulsion and the anionic aqueous polyurethane, so that the fabric finishing effect is affected; in comparative example 2, the cationic aqueous polyurethane was not blocked, and the wash fastness of the finished fabric was slightly poor; comparative examples 3 and 4 prepared microcapsules with thyme essential oil and mugwort essential oil, respectively, the antibacterial effect of the finished textile was inferior to that of the composite essential oil microcapsules; in the comparative example 5, only a nonionic emulsifier is used when the essential oil is emulsified, the plant essential oil and the aqueous polyurethane are combined only by intermolecular force, and more empty capsules can appear when the microcapsule is formed, so that the antibacterial property of the final finished fabric is poor; the fabric of comparative example 6 was not subjected to carboxymethylation treatment, resulting in poor antibacterial effect and water wash resistance of the finished fabric.
The invention adopts an anionic/nonionic emulsifier to prepare O/W type plant essential oil emulsion, utilizes the electrostatic action between end-capped cationic aqueous polyurethane and the plant essential oil emulsion to adsorb the aqueous polyurethane on the surface of the plant essential oil emulsion, and then adopts a spray drying mode to prepare plant essential oil microcapsules; the plant essential oil microcapsules are treated on the textile in a coating finishing mode, and excellent washing fastness is provided for the antibacterial textile by utilizing the electrostatic effect between the carboxymethyl cotton fabric and the plant essential oil microcapsules and the reactivity of the end-capped cationic aqueous polyurethane in the high-temperature baking process. Therefore, the invention effectively overcomes some practical problems in the prior art, thereby having high utilization value and use significance.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (10)
1. A method for preparing an antibacterial textile, which is characterized by comprising at least the following steps:
preparing plant essential oil emulsion by adopting an anionic emulsifier and a nonionic emulsifier;
preparing end-capped cationic aqueous polyurethane emulsion;
adding the plant essential oil emulsion into the blocked cationic aqueous polyurethane emulsion, uniformly dispersing, and preparing plant essential oil microcapsules in a spray drying mode;
preparing a coating finishing liquid by adopting the plant essential oil microcapsule;
coating the coating finishing liquid on a fabric to obtain an antibacterial textile;
wherein, the preparation of the end-capped cationic aqueous polyurethane emulsion comprises the following steps: placing castor oil modified dihydric alcohol into a container, and decompressing and dehydrating for 1-2 h; adding hexamethylene diisocyanate, mixing and stirring uniformly at 40-50 ℃, adding a catalyst, and reacting for 60-120 min at 40-70 ℃; dripping 1, 4-butanediol and isophorone diisocyanate, mixing and stirring to react for 1-2 hours at 70 ℃; dropwise adding a cationic chain extender to react for 1-2 hours; acetone is used as a solvent, and reflux heat preservation is carried out until the NCO amount reaches a theoretical value; cooling to 40-50 ℃, adding a blocking agent, and reacting for 2-3 hours; adding glacial acetic acid to neutralize until the pH value is 6-7, adding deionized water to emulsify under strong stirring, and stirring for 60-90 min; rotary steaming to remove acetone;
the end capping agent is hydroxyethyl acrylate; the fabric is cotton fabric subjected to carboxymethylation treatment.
2. The method of preparing an antimicrobial textile according to claim 1, wherein preparing a plant essential oil emulsion comprises: adding an anionic emulsifier and a nonionic emulsifier into deionized water, and stirring until the anionic emulsifier and the nonionic emulsifier are completely dissolved; and adding plant essential oil, and emulsifying for 1h at a high speed at 40 ℃ to obtain stable O/W type plant essential oil emulsion, wherein the mass of the anionic emulsifier and the nonionic emulsifier is 5-10 wt% of the mass of the plant essential oil.
3. The method for preparing an antibacterial textile according to claim 2, wherein the nonionic emulsifier comprises Tween 80, the anionic emulsifier comprises sodium dodecyl sulfate, and the mass ratio of Tween 80 to sodium dodecyl sulfate is 1:1-3:1.
4. The method for preparing the antibacterial textile according to claim 2, wherein the plant essential oil is a compound plant essential oil containing thyme essential oil and mugwort essential oil, and the mass ratio of the thyme essential oil to the mugwort essential oil is 1:1-1:3.
5. The method of manufacturing an antimicrobial textile according to claim 1, wherein the castor oil modified diol has a hydroxyl number of 180mg KOH/g; the molar ratio of the functional group NCO in the hexamethylene diisocyanate and the isophorone diisocyanate to the functional group OH in the castor oil modified dihydric alcohol and the 1, 4-butanediol is 1.2-1.4.
6. The method for preparing the antibacterial textile according to claim 1, wherein the catalyst is dibutyl tin dilaurate, the cationic chain extender is N-methyldiethanolamine, and the addition amount of the dibutyl tin dilaurate is 0.5-1.0 wt% of the total mass of dihydric alcohol and isocyanate in the system; the addition amount of the N-methyldiethanolamine is 3-6 wt% of the total mass of the dihydric alcohol and the isocyanate in the system; the adding amount of the hydroxyethyl acrylate is 1.0-1.5 wt% of the total mass of the dihydric alcohol and the isocyanate in the system.
7. The method for preparing an antibacterial textile according to claim 1, wherein when preparing the plant essential oil microcapsule, the mass ratio of the blocked cationic aqueous polyurethane emulsion to the plant essential oil emulsion is 1:1-2:1, the inlet temperature during spray drying is 160-180 ℃, the peristaltic pump sample injection amount is set to 5-10 mL/min during spray drying, the spray air pressure is 0.1MPa, and the drying air flow rate is 100m 3 /h。
8. The method for preparing the antibacterial textile according to claim 1, wherein the coating finishing liquid is prepared by dispersing the plant essential oil microcapsules in deionized water, adding a thickening agent and uniformly stirring, wherein the adding amount of the thickening agent is 3-wt% of the total mass of the system, and the mass of the plant essential oil microcapsules is 10-30% of the total mass of the system.
9. A method of preparing an antimicrobial textile according to claim 1, wherein the step of carboxymethylation treatment comprises: padding the fabric in caustic soda solution with the mass fraction of 25-30%, wherein the padding is performed twice, and the padding residual rate is 80-90%; taking out the fabric, and drying the fabric in a 60 ℃ oven for 5-10 min; immersing the fabric subjected to alkali treatment into chloroacetic acid solution with the mass fraction of 15-25%, and reacting at 60-70 ℃ for 30-50 min; and (5) taking out the fabric, washing the fabric with deionized water for 3-5 times, and drying at 60-80 ℃.
10. An antibacterial textile product characterized by being prepared by the preparation method of the antibacterial textile product according to any one of claims 1-9.
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