CN116752344A - Preparation method of super-hydrophobic antibacterial cotton fabric - Google Patents
Preparation method of super-hydrophobic antibacterial cotton fabric Download PDFInfo
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- CN116752344A CN116752344A CN202310839892.3A CN202310839892A CN116752344A CN 116752344 A CN116752344 A CN 116752344A CN 202310839892 A CN202310839892 A CN 202310839892A CN 116752344 A CN116752344 A CN 116752344A
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- cotton fabric
- geranium oil
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- 239000004744 fabric Substances 0.000 title claims abstract description 134
- 229920000742 Cotton Polymers 0.000 title claims abstract description 131
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 36
- 230000003075 superhydrophobic effect Effects 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 235000019717 geranium oil Nutrition 0.000 claims abstract description 51
- 239000010648 geranium oil Substances 0.000 claims abstract description 51
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- -1 alkyl mercaptan Chemical compound 0.000 claims abstract description 17
- 230000010355 oscillation Effects 0.000 claims abstract description 14
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 27
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 16
- 239000012266 salt solution Substances 0.000 claims description 10
- 229910002651 NO3 Inorganic materials 0.000 claims description 7
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 7
- 229960002089 ferrous chloride Drugs 0.000 claims description 7
- 239000011790 ferrous sulphate Substances 0.000 claims description 7
- 235000003891 ferrous sulphate Nutrition 0.000 claims description 7
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 claims description 7
- 229910000359 iron(II) sulfate Inorganic materials 0.000 claims description 7
- QJAOYSPHSNGHNC-UHFFFAOYSA-N octadecane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCS QJAOYSPHSNGHNC-UHFFFAOYSA-N 0.000 claims description 6
- WNAHIZMDSQCWRP-UHFFFAOYSA-N dodecane-1-thiol Chemical compound CCCCCCCCCCCCS WNAHIZMDSQCWRP-UHFFFAOYSA-N 0.000 claims description 5
- NNZMLOHQRXHPOZ-UHFFFAOYSA-N docosane-1-thiol Chemical compound CCCCCCCCCCCCCCCCCCCCCCS NNZMLOHQRXHPOZ-UHFFFAOYSA-N 0.000 claims description 4
- YAJYJWXEWKRTPO-UHFFFAOYSA-N 2,3,3,4,4,5-hexamethylhexane-2-thiol Chemical compound CC(C)C(C)(C)C(C)(C)C(C)(C)S YAJYJWXEWKRTPO-UHFFFAOYSA-N 0.000 claims description 3
- MZRQZJOUYWKDNH-UHFFFAOYSA-N diphenylphosphoryl-(2,3,4-trimethylphenyl)methanone Chemical compound CC1=C(C)C(C)=CC=C1C(=O)P(=O)(C=1C=CC=CC=1)C1=CC=CC=C1 MZRQZJOUYWKDNH-UHFFFAOYSA-N 0.000 claims description 3
- 230000001678 irradiating effect Effects 0.000 claims description 3
- 229910000859 α-Fe Inorganic materials 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 12
- 239000004753 textile Substances 0.000 abstract description 7
- 230000002209 hydrophobic effect Effects 0.000 abstract description 6
- 230000002045 lasting effect Effects 0.000 abstract description 3
- 238000011068 loading method Methods 0.000 abstract description 3
- 238000012545 processing Methods 0.000 abstract description 3
- 230000009471 action Effects 0.000 abstract description 2
- 230000009920 chelation Effects 0.000 abstract description 2
- 229910001448 ferrous ion Inorganic materials 0.000 abstract description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 24
- 239000000835 fiber Substances 0.000 description 13
- 239000007864 aqueous solution Substances 0.000 description 8
- 241000208152 Geranium Species 0.000 description 4
- 239000003242 anti bacterial agent Substances 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 4
- 238000001035 drying Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 229920000728 polyester Polymers 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- FRQQKWGDKVGLFI-UHFFFAOYSA-N 2-methylundecane-2-thiol Chemical compound CCCCCCCCCC(C)(C)S FRQQKWGDKVGLFI-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000004043 dyeing Methods 0.000 description 2
- 239000004005 microsphere Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- CMLFRMDBDNHMRA-UHFFFAOYSA-N 2h-1,2-benzoxazine Chemical compound C1=CC=C2C=CNOC2=C1 CMLFRMDBDNHMRA-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 230000003373 anti-fouling effect Effects 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000005661 hydrophobic surface Effects 0.000 description 1
- 238000005470 impregnation Methods 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 238000001020 plasma etching Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
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- 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
- 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
- D06M11/07—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—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 halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/28—Halides of elements of Groups 8, 9, 10 or 18 of the Periodic Table
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- 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
- D06M11/51—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 sulfur, selenium, tellurium, polonium or compounds thereof
- D06M11/55—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 sulfur, selenium, tellurium, polonium or compounds thereof with sulfur trioxide; with sulfuric acid or thiosulfuric acid or their salts
- D06M11/56—Sulfates or thiosulfates other than of elements of Groups 3 or 13 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
- 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
- D06M11/58—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 nitrogen or compounds thereof, e.g. with nitrides
- D06M11/64—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 nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
- D06M11/65—Salts of oxyacids of nitrogen
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- 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
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- 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
- D06M13/244—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 sulfur or phosphorus
- D06M13/248—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 sulfur or phosphorus with compounds containing sulfur
- D06M13/252—Mercaptans, thiophenols, sulfides or polysulfides, e.g. mercapto acetic acid; Sulfonium compounds
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- 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
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- 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
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- 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
- D06M2200/00—Functionality of the treatment composition and/or properties imparted to the textile material
- D06M2200/10—Repellency against liquids
- D06M2200/12—Hydrophobic properties
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a preparation method of a super-hydrophobic antibacterial cotton fabric, and relates to the technical field of textile processing. Comprising the following steps: pretreating cotton fabric by using sodium hydroxide solution to obtain pretreated cotton fabric; immersing the pretreated cotton fabric in the geranium oil solution for oscillation treatment to obtain the geranium oil modified cotton fabric and the like. According to the invention, the cotton fabric is endowed with excellent antibacterial performance by loading the geranium oil on the cotton fabric, and a network structure is formed by the chelation of ferrous ions and the geranium oil on the cotton fabric, so that the geranium oil can be stably attached to the cotton fabric for a long time, and a lasting antibacterial effect is achieved. Then, the geranium oil on the cotton fabric is subjected to click chemical reaction with alkyl mercaptan under the action of a photoinitiator, a super-hydrophobic layer is efficiently introduced into the surface of the cotton fabric, and the hydrophobic capacity of the cotton fabric can be effectively adjusted by adjusting the types and the quantity of the alkyl mercaptan.
Description
Technical Field
The invention relates to the technical field of textile processing, in particular to a preparation method of a super-hydrophobic antibacterial cotton fabric.
Background
Cotton fiber is the most abundant natural polymer substance in nature, and the fiber and the product thereof have the advantages of soft hand feeling, good moisture absorption and air permeability, comfortable warm keeping and taking, good biocompatibility and the like, and are widely applied to the fields of clothing, home textile, military medical treatment and the like. With the development of science and technology, the meaning of the traditional textile industry is continuously changed and richer, and the requirements of people on textiles in new period are gradually increased, so that the textiles are hoped to have more functionalities so as to meet specific requirements. The natural cotton fabric is a hydrophilic and porous material, is easy to be stained with stains and is easy to be affected by bacteria and microorganisms in the taking process, so that the multifunctional hydrophobic antibacterial fabric is prepared, the waterproof, antifouling and self-cleaning performances and the bacterial growth and reproduction inhibiting performances of the fabric are endowed, and the requirements of people on the aspects of health, beauty and the like of clothing are met.
In recent years, various methods have been developed for functionally modifying fibers, for example, simulating hydrophobic surfaces by surface impregnation, chemical vapor deposition, plasma etching, and the like, realizing superhydrophobic and self-cleaning functions of fibers, integrating inorganic, organic, natural antibacterial agents, and the like into fiber finishing agents, attaching the agents to fiber surfaces, and imparting antibacterial functions to the fibers. Chinese patent (CN 2013105064908) discloses a super-hydrophobic natural fiber fabric, wherein the surface of the natural fiber fabric is coated with carbon nano tubes and benzoxazine resin coating for multiple times to realize the super-hydrophobic characteristic of the fiber fabric. A knitted fabric antibacterial treatment method (CN 202000010805709) is disclosed in Chinese patent, cotton yarn is sequentially put into silicate antibacterial agent and fiber antibacterial agent for heating treatment, and antibacterial function is realized through loading of antibacterial agent in cotton fiber. Chinese patent (CN 2021113513424) discloses a super-hydrophobic antibacterial fabric and a preparation method thereof, wherein hydrophobic antibacterial nano-porous hollow microspheres are mixed into polyester chips, and the microspheres are fixed on polyester fiber molecular chains by utilizing the melt blending processing and forming process of polyester fibers, so that the polyester fibers are endowed with super-hydrophobic and antibacterial functions.
However, the existing method has the problems of long reaction steps, complex reaction system, large chemical consumption or high price, high wastewater yield, environmental threat, poor hydrophobic antibacterial durability and the like. How to realize ecological dyeing and finishing or low-carbon dyeing and finishing of textiles and develop a simple, efficient, environment-friendly and low-cost method for preparing hydrophobic antibacterial cotton fabric are still a problem to be solved.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of the super-hydrophobic antibacterial cotton fabric, which is simple and convenient to operate and low in cost, and the obtained cotton fabric has lasting antibacterial and self-cleaning functions.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a super-hydrophobic antibacterial cotton fabric, which comprises the following steps:
1) Pretreating cotton fabric by using sodium hydroxide solution to obtain pretreated cotton fabric;
2) Immersing the pretreated cotton fabric obtained in the step 1) in a geranium oil solution for oscillation treatment to obtain a geranium oil modified cotton fabric;
3) Immersing the geranium oil modified cotton fabric obtained in the step 2) in a ferrite solution for treatment to obtain a geranium oil/Fe cotton fabric;
4) Immersing the geranium oil/Fe cotton fabric obtained in the step 3) in a solution containing alkyl mercaptan and a photoinitiator, and carrying out water bath oscillation treatment for 5-10 minutes to obtain an oscillation cotton fabric;
5) And (3) respectively irradiating the front and the back of the oscillating cotton fabric obtained in the step (4) with ultraviolet lamps for 30 minutes to obtain the super-hydrophobic antibacterial cotton fabric.
Preferably, the concentration of the sodium hydroxide solution in the step 1) is 15-25 g/L.
Preferably, the pretreatment conditions in the step 1) include: the mass ratio of the cotton fabric to the sodium hydroxide solution is 1 g/30 ml, the temperature is 80-90 ℃, and the time is 60-90 min.
Preferably, the concentration of the geranium oil solution in the step 2) is 1-3 g/L.
Preferably, the conditions of the oscillating treatment in the step 2) include: the mass ratio of the pretreated cotton fabric to the geranium oil is 1 g:50-100 ml, the temperature is 80-90 ℃ and the time is 20-30 min.
Preferably, the concentration of the ferrous salt solution in the step 3) is 20-50 mM; the ferrous salt in the ferrous salt solution comprises one or more of ferrous chloride, ferrous sulfate and ferrous nitrate.
Preferably, the conditions of the treatment in the step 3) include: the mass ratio of the geranium oil modified cotton fabric to the ferrous salt solution is 1 g:20-30 ml, the temperature is 40-60 ℃, and the time is 30-60 min.
Preferably, the alkyl mercaptan in the step 4) comprises one or more of n-dodecyl mercaptan, tert-dodecyl mercaptan, n-octadecyl mercaptan and n-docosyl mercaptan;
the photoinitiator is 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide.
Preferably, the concentration of the alkyl mercaptan in the solution containing the alkyl mercaptan and the photoinitiator in the step 4) is 1.5-2.5 g/L, and the concentration of the photoinitiator is 0.01-0.05 g/L.
Preferably, the ultraviolet lamp treatment conditions in the step 5) are as follows: 150-220W,50Hz.
The beneficial effects of the invention are as follows:
according to the invention, the cotton fabric is endowed with excellent antibacterial performance by loading the geranium oil on the cotton fabric, and a network structure is formed by the chelation of ferrous ions and the geranium oil on the cotton fabric, so that the geranium oil can be stably attached to the cotton fabric for a long time, and a lasting antibacterial effect is achieved. Then, the geranium oil on the cotton fabric is subjected to click chemical reaction with alkyl mercaptan under the action of a photoinitiator, a super-hydrophobic layer is efficiently introduced into the surface of the cotton fabric, and the hydrophobic capacity of the cotton fabric can be effectively adjusted by adjusting the types and the quantity of the alkyl mercaptan.
Detailed Description
The invention provides a preparation method of a super-hydrophobic antibacterial cotton fabric, which comprises the following steps:
1) Pretreating cotton fabric by using sodium hydroxide solution to obtain pretreated cotton fabric;
2) Immersing the pretreated cotton fabric obtained in the step 1) in a geranium oil solution for oscillation treatment to obtain a geranium oil modified cotton fabric;
3) Immersing the geranium oil modified cotton fabric obtained in the step 2) in a ferrite solution for treatment to obtain a geranium oil/Fe cotton fabric;
4) Immersing the geranium oil/Fe cotton fabric obtained in the step 3) in a solution containing alkyl mercaptan and a photoinitiator, and carrying out water bath oscillation treatment for 5-10 minutes to obtain an oscillation cotton fabric;
5) And (3) respectively irradiating the front and the back of the oscillating cotton fabric obtained in the step (4) with ultraviolet lamps for 30 minutes to obtain the super-hydrophobic antibacterial cotton fabric.
The invention pretreats cotton fabric by sodium hydroxide solution to obtain pretreated cotton fabric. In the present invention, the concentration of the sodium hydroxide solution is preferably 15 to 25g/L. In the present invention, the pretreatment conditions preferably include: the mass ratio of the cotton fabric to the sodium hydroxide solution is 1 g/30 ml, the temperature is 80-90 ℃, and the time is 60-90 min. The method is preferably to wash the cotton fabric treated by sodium hydroxide for a plurality of times and then air-dry the cotton fabric to obtain the pretreated cotton fabric.
The obtained pretreated cotton fabric is immersed in the geranium oil solution for oscillation treatment, so that the geranium oil modified cotton fabric is obtained. In the present invention, the concentration of the geranium oil solution is preferably 1 to 3g/L. In the present invention, the conditions of the oscillation treatment preferably include: the mass ratio of the pretreated cotton fabric to the geranium oil is 1 g:50-100 ml, the temperature is 80-90 ℃ and the time is 20-30 min. In the present invention, the shaking treatment is preferably performed under a water bath.
According to the invention, the obtained geranium oil modified cotton fabric is immersed in a ferrous salt solution for treatment, so that the geranium oil/Fe cotton fabric is obtained. In the present invention, the concentration of the ferrous salt solution is preferably 20 to 50mM. In the present invention, the ferrous salt in the ferrous salt solution preferably includes one or more of ferrous chloride, ferrous sulfate and ferrous nitrate. In the present invention, the conditions of the treatment preferably include: the mass ratio of the geranium oil modified cotton fabric to the ferrous salt solution is 1 g:20-30 ml, the temperature is 40-60 ℃, and the time is 30-60 min. In the present invention, the treatment is preferably performed under a water bath.
According to the invention, the obtained geranium oil/Fe cotton fabric is immersed in a solution containing alkyl mercaptan and a photoinitiator, and is subjected to water bath oscillation treatment for 5-10 minutes, so that the oscillation cotton fabric is obtained. In the present invention, the alkyl mercaptan preferably includes one or more of n-dodecyl mercaptan, t-dodecyl mercaptan, n-octadecyl mercaptan and n-docosyl mercaptan. In the present invention, the photoinitiator is preferably 2,4,6 (trimethylbenzoyl) diphenyl phosphine oxide. In the present invention, the concentration of the alkyl mercaptan in the solution containing the alkyl mercaptan and the photoinitiator is preferably 1.5 to 2.5g/L, and the concentration of the photoinitiator is preferably 0.01 to 0.05g/L.
The front and the back of the obtained oscillating cotton fabric are respectively irradiated by ultraviolet lamps for 30 minutes to obtain the super-hydrophobic antibacterial cotton fabric. In the present invention, the ultraviolet lamp treatment conditions are preferably: 150-220W,50Hz. The invention preferably dries the cotton fabric irradiated by the ultraviolet lamp for 24 hours at 60 ℃ to obtain the super-hydrophobic antibacterial cotton fabric.
The present invention will be described in detail with reference to examples for further illustration of the invention, but they should not be construed as limiting the scope of the invention.
Example 1
(1) Cotton fabric (10 x 10 cm) 2 ) The mixture was pretreated in 25g/L sodium hydroxide solution at a bath ratio of 1:30 (w/v) (i.e., 1g:30 ml) at 90℃for 60 minutes. Washing the pretreated cotton fabric with water for several times, and air drying to obtain pretreated cotton fabricA cotton fabric;
(2) Putting the pretreated cotton fabric into a geranium oil-water solution with the concentration of 3g/L, wherein the bath ratio is 1:100 (w/v), and oscillating for 30 minutes in a constant-temperature water bath at 90 ℃ to obtain a geranium oil modified cotton fabric;
(3) Putting the obtained geranium oil modified cotton fabric into a ferrous nitrate aqueous solution with the concentration of 50mM at 60 ℃, and carrying out oscillating treatment for 60 minutes in a constant-temperature water bath, wherein the bath ratio is 1:30 (w/v), so as to obtain the geranium oil/Fe cotton fabric;
(4) And adding an ethanol solution containing n-docosyl mercaptan and TPO into the ferrous nitrate reaction system, wherein the concentration of n-octadecyl mercaptan in the ethanol solution is 1.75g/L, the concentration of TPO is 0.03g/L, and the volume ratio of the ethanol solution to the ferrous nitrate aqueous solution is 1:5.
(5) After the reaction system is continuously treated in a 60 ℃ constant-temperature water bath oscillator for 10 minutes, the front and the back of the cotton fabric are respectively treated by ultraviolet lamps. The treatment conditions are as follows: 220W,50Hz,30 minutes. And then drying the cotton fabric at 60 ℃ to obtain the super-hydrophobic antibacterial cotton fabric.
Example 2
(1) Cotton fabric (10 x 10 cm) 2 ) The mixture was pretreated in a 20g/L aqueous sodium hydroxide solution at a bath ratio of 1:30 (w/v) (i.e., 1g:30 ml) at 90℃for 70 minutes. Washing the pretreated cotton fabric with water for a plurality of times, and airing to obtain the pretreated cotton fabric;
(2) Putting the pretreated cotton fabric into a geranium oil-water solution with the concentration of 2g/L, wherein the bath ratio is 1:70 (w/v), and oscillating for 20 minutes in a constant-temperature water bath at 80 ℃ to obtain a geranium oil modified cotton fabric;
(3) Putting the obtained geranium oil modified cotton fabric into a ferrous chloride aqueous solution with the concentration of 45mM at 50 ℃, wherein the bath ratio is 1:20 (w/v), and carrying out oscillating treatment in a constant-temperature water bath for 50 minutes to obtain the geranium oil/Fe cotton fabric;
(4) And adding an ethanol solution containing n-octadecyl mercaptan and TPO into the ferrous nitrate reaction system, wherein the concentration of the n-octadecyl mercaptan in the ethanol solution is 1.65g/L, the concentration of the TPO is 0.02g/L, and the volume ratio of the ethanol solution to the ferrous chloride aqueous solution is 1:4.
(5) After the reaction system is continuously treated in a 50 ℃ constant-temperature water bath oscillator for 8 minutes, the front and the back of the cotton fabric are respectively treated by ultraviolet lamps. The treatment conditions are as follows: 200W,50Hz,30 minutes. And then drying the cotton fabric at 60 ℃ to obtain the super-hydrophobic antibacterial cotton fabric.
Example 3
(1) Cotton fabric (10 x 10 cm) 2 ) The mixture was pretreated in a 20g/L aqueous sodium hydroxide solution at a bath ratio of 1:30 (w/v) (i.e., 1g:30 ml) at 80℃for 80 minutes. Washing the pretreated cotton fabric with water for a plurality of times, and airing to obtain the pretreated cotton fabric;
(2) Putting the pretreated cotton fabric into a geranium oil-water solution with the concentration of 1.5g/L, wherein the bath ratio is 1:80 (w/v), and carrying out oscillating treatment for 25 minutes in a constant-temperature water bath at the temperature of 85 ℃ to obtain a geranium oil modified cotton fabric;
(3) Putting the obtained geranium oil modified cotton fabric into a ferrous sulfate aqueous solution with the concentration of 30mM at 45 ℃, wherein the bath ratio is 1:25 (w/v), and carrying out oscillating treatment in a constant-temperature water bath for 40 minutes to obtain the geranium oil/Fe cotton fabric;
(4) And adding an ethanol solution containing tertiary dodecyl mercaptan and TPO into the ferrous sulfate reaction system, wherein the concentration of the tertiary dodecyl mercaptan in the ethanol solution is 2.5g/L, the concentration of the TPO is 0.05g/L, and the volume ratio of the ethanol solution to the ferrous chloride aqueous solution is 1:3.
(5) After the reaction system is continuously treated in a 45 ℃ constant-temperature water bath oscillator for 6 minutes, the front and the back of the cotton fabric are respectively treated by ultraviolet lamps. The treatment conditions are as follows: 180W,50Hz,30 minutes. And then drying the cotton fabric at 60 ℃ to obtain the super-hydrophobic antibacterial cotton fabric.
Example 4
(1) Cotton fabric (10 x 10 cm) 2 ) The mixture was pretreated in 15g/L aqueous sodium hydroxide solution at a bath ratio of 1:30 (w/v) (i.e., 1g:30 ml) at 80℃for 90 minutes. Washing the pretreated cotton fabric with water for a plurality of times, and airing to obtain the pretreated cotton fabric;
(2) Putting the pretreated cotton fabric into a geranium oil-water solution with the concentration of 1g/L, wherein the bath ratio is 1:50 (w/v), and oscillating for 30 minutes in a constant-temperature water bath at 90 ℃ to obtain a geranium oil modified cotton fabric;
(3) Putting the obtained geranium oil modified cotton fabric into a ferrous sulfate aqueous solution with the concentration of 20mM at 40 ℃, and carrying out oscillating treatment for 30 minutes in a constant-temperature water bath, wherein the bath ratio is 1:30 (w/v), so as to obtain the geranium oil/Fe cotton fabric;
(4) And adding an ethanol solution containing n-dodecyl mercaptan and TPO into the ferrous sulfate reaction system, wherein the concentration of the n-dodecyl mercaptan in the ethanol solution is 1.5g/L, the concentration of the TPO is 0.01g/L, and the volume ratio of the ethanol solution to the ferrous chloride aqueous solution is 1:4.
(5) After the reaction system is continuously treated in a 40 ℃ constant-temperature water bath oscillator for 5 minutes, the front and the back of the cotton fabric are respectively treated by ultraviolet lamps. The treatment conditions are as follows: 150W,50Hz,30 minutes. And then drying the cotton fabric at 60 ℃ to obtain the super-hydrophobic antibacterial cotton fabric.
The results of the performance test of the superhydrophobic antibacterial cotton fabrics produced in examples 1-4 are shown in table 1:
table 1 results of the performance tests of examples 1-4
As can be derived from table 1, the super-hydrophobic antibacterial cotton fabric obtained by the preparation method provided by the invention has a larger water contact angle and milk contact angle, namely, the super-hydrophobic antibacterial cotton fabric has a better self-cleaning performance; in addition, the cotton fabric also has higher escherichia coli antibacterial rate and staphylococcus aureus antibacterial rate.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.
Claims (10)
1. The preparation method of the super-hydrophobic antibacterial cotton fabric is characterized by comprising the following steps of:
1) Pretreating cotton fabric by using sodium hydroxide solution to obtain pretreated cotton fabric;
2) Immersing the pretreated cotton fabric obtained in the step 1) in a geranium oil solution for oscillation treatment to obtain a geranium oil modified cotton fabric;
3) Immersing the geranium oil modified cotton fabric obtained in the step 2) in a ferrite solution for treatment to obtain a geranium oil/Fe cotton fabric;
4) Immersing the geranium oil/Fe cotton fabric obtained in the step 3) in a solution containing alkyl mercaptan and a photoinitiator, and carrying out water bath oscillation treatment for 5-10 minutes to obtain an oscillation cotton fabric;
5) And (3) respectively irradiating the front and the back of the oscillating cotton fabric obtained in the step (4) with ultraviolet lamps for 30 minutes to obtain the super-hydrophobic antibacterial cotton fabric.
2. The method according to claim 1, wherein the concentration of the sodium hydroxide solution in step 1) is 15 to 25g/L.
3. The method according to claim 1, wherein the pretreatment conditions of step 1) include: the mass ratio of the cotton fabric to the sodium hydroxide solution is 1 g/30 ml, the temperature is 80-90 ℃, and the time is 60-90 min.
4. The method according to claim 1, wherein the concentration of the geranium oil solution in step 2) is 1 to 3g/L.
5. The method according to claim 1, wherein the conditions of the oscillating treatment of step 2) include: the mass ratio of the pretreated cotton fabric to the geranium oil is 1 g:50-100 ml, the temperature is 80-90 ℃ and the time is 20-30 min.
6. The method according to claim 1, wherein the concentration of the ferrous salt solution in the step 3) is 20 to 50mM; the ferrous salt in the ferrous salt solution comprises one or more of ferrous chloride, ferrous sulfate and ferrous nitrate.
7. The method according to claim 1, wherein the conditions of the treatment in step 3) include: the mass ratio of the geranium oil modified cotton fabric to the ferrous salt solution is 1 g:20-30 ml, the temperature is 40-60 ℃, and the time is 30-60 min.
8. The method of claim 1, wherein the alkyl mercaptans of step 4) include one or more of n-dodecyl mercaptan, t-dodecyl mercaptan, n-octadecyl mercaptan, and n-docosyl mercaptan;
the photoinitiator is 2,4,6 (trimethyl benzoyl) diphenyl phosphine oxide.
9. The method according to claim 1, wherein the concentration of the alkyl mercaptan in the solution containing the alkyl mercaptan and the photoinitiator in the step 4) is 1.5 to 2.5g/L, and the concentration of the photoinitiator is 0.01 to 0.05g/L.
10. The method of claim 1, wherein the ultraviolet lamp treatment conditions in step 5) are: 150-220W,50Hz.
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