CN112301726B - Antibacterial fabric obtained by plasma technology and preparation method thereof - Google Patents

Antibacterial fabric obtained by plasma technology and preparation method thereof Download PDF

Info

Publication number
CN112301726B
CN112301726B CN201910713099.2A CN201910713099A CN112301726B CN 112301726 B CN112301726 B CN 112301726B CN 201910713099 A CN201910713099 A CN 201910713099A CN 112301726 B CN112301726 B CN 112301726B
Authority
CN
China
Prior art keywords
plasma
fabric
treated
treatment
antimicrobial
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Active
Application number
CN201910713099.2A
Other languages
Chinese (zh)
Other versions
CN112301726A (en
Inventor
林子聪
陈永敏
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hong Kong Research Institute of Textiles and Apparel Ltd
Original Assignee
Hong Kong Research Institute of Textiles and Apparel Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hong Kong Research Institute of Textiles and Apparel Ltd filed Critical Hong Kong Research Institute of Textiles and Apparel Ltd
Priority to CN201910713099.2A priority Critical patent/CN112301726B/en
Priority to PCT/CN2020/106334 priority patent/WO2021023121A1/en
Publication of CN112301726A publication Critical patent/CN112301726A/en
Application granted granted Critical
Publication of CN112301726B publication Critical patent/CN112301726B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/02Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/06Inorganic compounds or elements
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M10/00Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/04Physical treatment combined with treatment with chemical compounds or elements
    • D06M10/08Organic compounds
    • D06M10/10Macromolecular compounds
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating 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
    • D06M11/68Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof
    • D06M11/70Treating 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 phosphorus or compounds thereof, e.g. with chlorophosphonic acid or salts thereof with oxides of phosphorus; with hypophosphorous, phosphorous or phosphoric acids or their salts
    • D06M11/71Salts of phosphoric acids
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/01Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
    • D06M15/03Polysaccharides or derivatives thereof
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/10Animal fibres
    • D06M2101/12Keratin fibres or silk

Abstract

The invention relates to an antibacterial fabric obtained by a plasma technology and a preparation method thereof. The plasma technology treatment of the present invention is applied only to the surface, and the overall properties of the material can be maintained, and thus the obtained antibacterial fabric still has antibacterial activity after being washed.

Description

Antibacterial fabric obtained by plasma technology and preparation method thereof
Technical Field
The invention relates to an antibacterial fabric obtained by a plasma technology and a preparation method thereof.
Background
Natural fibers, such as cotton and wool, provide an environment with heat, moisture and oxygen that promotes the growth of microorganisms and ultimately causes malodor and deterioration of laundry. In addition, these materials are likely to absorb moisture, thereby promoting the growth of microorganisms. To address these problems, chemical finishing processes are used to apply functional coatings to textile materials.
Conventionally, antimicrobial treatment has been achieved by the application of antibacterial agents such as triclosan, chitosan, quaternary ammonium salts, and metal salts such as cu (ii), ni (ii), and Ag (i), as well as nanosized metals and metal oxides such as Ag, Ti oxygen, and ZnO, which control, destroy, and inhibit the growth of microorganisms.
These chemical treatments are applied from solution to the outside of the laundry mainly by two different methods, i.e. the dip method and the tumbler method. The dipping method requires sufficient water where the material to liquid ratio (MLR) is 1:5, while the drum method requires less water where MLR is less than 1: 1. Both methods require long processing times (-1 h) and two thirds of the processing time require heating (drying and curing) (i.e. with large energy consumption).
Plasma technology is a pollution-free, safe, economical and water-free process, and is a new method that can be used for antimicrobial treatment. It is a well-developed process and can be applied to a variety of materials.
Disclosure of Invention
The invention provides an antibacterial fabric obtained by a plasma technology and a preparation method thereof. Plasma technology treatments are only applied to the surface and therefore the bulk properties of the material can be maintained.
According to one aspect, the present invention provides a fabric having a coating comprising a coating material selected from the group consisting of: sodium zirconium silver hydrogen phosphate or chitosan; and the coating is plasma treated before or after coating.
According to some embodiments, the fabric of the invention is selected from cotton fabric or wool fabric.
According to another aspect, the present invention provides a method of preparing the above coated fabric, comprising the step of applying a coating after treating the fabric with plasma.
According to some embodiments, the plasma used for the plasma treatment according to the invention is selected from nitrogen, argon, oxygen, n-heptane and/or air.
According to some embodiments, the plasma treatment is performed under low pressure conditions. The preferred pressure is 5x100Pa to 8x102Pa. The plasma treatment time may be 1-10 min. For example, 1-2 min.
According to some embodiments, the plasma treatment is performed one or more times.
According to some embodiments, when the coating material is silver zirconium hydrogen phosphate sodium salt, the fabric is a cotton fabric, the fabric is pretreated with a citric acid, aconitic acid, citraconic acid and/or itaconic acid solution prior to the plasma treatment.
According to some embodiments, the sodium zirconium hydrogen phosphate is used in a concentration of not less than 0.5% w/v, for example 0.5% to 2% w/v.
According to some embodiments, the plasma treatment of the method is a treatment with nitrogen at 400W for 1 minute.
According to some embodiments, when the fabric is a cotton fabric, the method may be preceded by a pretreatment with 10% citric acid and followed by a treatment with 2% W/v sodium zirconium silver hydrogen phosphate at 400W with nitrogen for 1 min.
According to some embodiments, when the coating material is chitosan, the concentration of the chitosan solution is not less than 0.05% w/v, for example 0.05-2% w/v.
According to some embodiments, when the fabric is a wool fabric, the fabric may be pre-treated with oxygen plasma prior to coating, then treated with a chitosan solution, dried, and then treated with nitrogen plasma. For example, pretreatment with oxygen plasma at 200W for 5min, followed by treatment twice with a 2% aqueous chitosan solution containing 5% acetic acid, drying at 80 deg.C, and then treatment with nitrogen plasma at 400W for 1 min. Optionally, the pre-treatment step further comprises treatment with peroxide oxidation and/or digestion with a protease.
Drawings
FIG. 1 aerobic bacteria testing of chitin treated cotton fabrics
FIG. 2 Yeast and mold test for chitin treated Cotton Fabric
FIG. 3 aerobic test of cotton fabric treated with sodium zirconium silver hydrogen phosphate (oxygen or nitrogen plasma treatment at 400W power and 2min time)
FIG. 4 Yeast and mold test of cotton fabric treated with sodium zirconium hydrogen phosphate sodium salt [ oxygen or nitrogen plasma treatment at 400W power for 2min ]
FIG. 5 SEM image of the coating obtained by treating the fabric with sodium zirconium hydrogen phosphate silver salt (left panel: untreated right panel: plasma treated cotton fibers)
FIG. 6 aerobic test of cotton fabric treated with sodium zirconium silver hydrogen phosphate salt [ nitrogen plasma treatment at 400W power for 1min ]
FIG. 7 aerobic test of cotton fabric treated with sodium zirconium silver hydrogen phosphate salt [ nitrogen plasma treatment at 400W power for 1min ]
FIG. 8 aerobic test of cotton fabric treated with sodium zirconium silver hydrogen phosphate salt [ nitrogen plasma treatment at 400W power for 1min ]
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Examples
I. Plasma treatment
The plasma treatment of the present invention is carried out in a laboratory scale low pressure plasma treatment system. A Radio Frequency (RF) generator provides a variety of powers to establish a plasma field at reduced pressure between two parallel electrodes. In this system, three gas inlets allow for the simultaneous application of multiple gases. Some of the liquid monomer is transferred to the reaction chamber through an evaporator. The specifications of the press are as follows:
gas used Nitrogen, argon, oxygen, n-heptane/air
Flow rate of flow Maximum 10l/min
Pressure of 5x 100Pa to 8x102Pa
Time of treatment 0.5min to 10min
Power of Maximum 400W
Temperature of At room temperature
II. Material
The wool fabric is 100% merino wool, the single-sided knitted fabric has the weight of 265g/m2The structure is 22 needles per inch in the longitudinal direction and 16 needles per inch in the transverse direction.
The cotton fabric is 100% cotton and is divided into two types: i) single-knit fabric having a weight of 230g/m2The structure is 48 needles per inch in the longitudinal direction and 30 needles per inch in the transverse direction; and ii) a scoured and bleached plain weave fabric having a weight of 265g/m2. Antimicrobial treatment of both types of cotton fabrics was investigated.
Characterization of
i) Durability of laundry
Laundry durability evaluation was performed according to the following: i) AATCC test method 61-2010, condition 2A; or ii) ISO 6330: 2012. In AATCC test method 61, the fabric is cut into 50mm by 150mm pieces and washed in a rotating closed tank containing 150ml of an aqueous solution of AATCC standard WOB detergent (0.15%, w/v) and 50 stainless steel balls, in which a thermostatic water bath is controlled at 49 ℃ and at a speed of 40 + -2 rpm for 45 min. A single 45min wash cycle corresponds to 5 domestic wash cycles. In ISO 6330, test procedure 4N, the fabrics are washed in a drum washing machine at 40 ℃ for 15min and rinsed 4 times, then drum dried at a temperature <60 ℃ and repeated 20 times. For test procedure 4H, the fabric was washed in a 40 ℃ drum washer for 1min and rinsed 2 times, then dried flat and repeated 20 times.
ii) antibacterial Activity
Antimicrobial activity was characterized based on AATCC test method 100-. Gram-positive Staphylococcus aureus (ATCC 6538) and gram-negative Klebsiella pneumoniae (ATCC 4352) were used in the test. In addition, Petrifilm was performedTMAerobic Count (AC) test to initially assess antimicrobial activity. A1 cm by 2cm size fabric sample was immersed for 24 hours in an autoclave tube with 10ml sterile solvent (distilled water). Thereafter, 1ml of the sample solution was placed in PetrifilmTMThe center of the plate was counted aerobically, covered with a top film and the inoculum was distributed over a circular area with an applicator, waiting at least 1min to allow the gel to set. The plate was incubated in a humidified incubator at 35 ℃ for 48 hours. Plates can then be counted on a standard colony counter.
iii) surface analysis
The surface morphology of the coating was examined by Scanning Electron Microscopy (SEM).
Antimicrobial treatment
Chitin I
Chitin is a long-chain polymer of N-acetyl glucosamine, and it is found to have bacteriostatic effects on gram-negative bacteria, escherichia coli (e. coli), vibrio cholerae (v. cholerae), shigella dysenteriae (s. dysenteriae), and bacteroides fragilis (b. fragilis). In this study chitin was grafted onto cotton fabric by plasma technique (introducing oxygen or nitrogen) (table 14) and antimicrobial activity was studied (fig. 1 and 2).
Figure BDA0002154445780000051
Chemical structure of chitin
TABLE 14 antimicrobial treatment conditions for cotton fabrics with chitin
Testing Power of Carrier gas Time
1 400W Oxygen gas 2min
2 400W Nitrogen gas 2min
The antimicrobial activity of cotton fabric treated with chitin via plasma was investigated. Aerobic bacteria count, contrast, 10 under oxygen and nitrogen respectively3,103And 3. Antimicrobial activity was found to be unsatisfactory in both tests, in particular the yeast and mould tests. Therefore, chitin is clearly not suitable as an antimicrobial agent in this study. It should be noted, however, that plasma treatment with nitrogen gas showed good bacteriostatic effects, especially in aerobic experiments. One possible explanation is that the plasma with nitrogen gas produces quaternary amines with antimicrobial properties.
Ii sodium zirconium hydrogen phosphate
It is known to use various metal-based chemicals to improve antimicrobial activity because they kill microorganisms by binding to intracellular proteins and inactivating them at very low concentrations. In this study, silver zirconium hydrogen phosphate sodium salt was applied by plasma technique to improve the antimicrobial activity of cotton fabric (table 15).
Figure BDA0002154445780000061
Chemical structure of silver zirconium hydrogen phosphate sodium salt
TABLE 15 antimicrobial treatment conditions for cotton fabrics with silver zirconium hydrogen phosphate sodium salt (0.5%)
Testing Power of Carrier gas Time
1 400W Oxygen gas 2min
2 400W Nitrogen gas 2min
3 400W Nitrogen gas 1min
The cotton fabric was impregnated with an aqueous solution of silver zirconium hydrogen phosphate sodium salt (0.5% w/v) and air dried overnight before plasma treatment. The plasma treated cotton fabric was subjected to an aerobic test (figure 3), a yeast test and a mold test (figure 4) to investigate antimicrobial activity. The positive bacteriostasis effect is shown in the aerobic test of the plasma treatment of oxygen and nitrogen, and the count of aerobic bacteria is 0. Nitrogen plasma treated cotton fabric showed better activity in yeast and mould tests, where there was little or no growth of yeast and mould. Based on the current research, nitrogen plasma is found to produce better bacteriostatic effect than oxygen plasma, so it is used for further research.
The formation of the coating was confirmed by SEM imaging, and the result is shown in fig. 5. The results clearly show that a smooth and uniform deposit was formed on the plasma treated cotton fibers, whereas no such deposit was observed on the untreated sample.
The antimicrobial properties were confirmed by standard evaluation (AATCC 100) and the results are shown in table 16. The results demonstrate that treatment of cotton with silver zirconium hydrogen phosphate sodium salt reduced bacteria by more than 99%. The wash durability of the treated cotton fabric was investigated with treatment times of 1min and 2min, respectively, and the results are shown in fig. 6 and 7. The results show that antimicrobial performance (greater than 99% bacteria reduction) can only be maintained for 10 wash cycles at 1min treatment time. Similar results were observed for the 2min treated samples. To improve the wash durability, the cotton fabric was pre-treated with citric acid, wherein the cotton fabric was impregnated with aqueous citric acid solution (10% w/v) and dried at 100 ℃ for 3 min. The use of citric acid results in the formation of unsaturated carboxylic acids, which are ligands for metal ions, under plasma conditions. The wash durability of the treated cotton fabric was investigated and the results are shown in figure 8. The results show that the pretreatment successfully improved wash durability with greater than 99% reduction of bacteria after 20 washes. AATCC 100 evaluation after 20 washes based on the BS EN ISO 6330:2012 program showed antimicrobial activity against Staphylococcus aureus (89% bacterial reduction) only, but not Klebsiella pneumoniae (table 17). To ensure sufficient antimicrobial active, the dose of antimicrobial agent was increased from 0.5% w/v to 2% w/v. The fabric was first impregnated with aqueous citric acid (10% w/v) and dried at 100 ℃ for 3min, then impregnated with aqueous zirconium silver hydrogen phosphate sodium salt (2% w/v) and air dried. The nitrogen plasma treatment was performed at 400W for 1 min. Dipping with aqueous solution of sodium zirconium silver hydrogen phosphate (2% w/v), and then air-drying; the plasma treatment was repeated once. After 20 washes, AATCC 100 evaluation showed greater than 99% reduction of bacteria against both staphylococcus aureus and klebsiella pneumoniae (table 17).
TABLE 16 test results of antibacterial finish evaluation (AATCC 100) of fabrics treated with zirconium silver hydrogen phosphate sodium salt solution via plasma
Figure BDA0002154445780000071
TABLE 17 test results of the evaluation of the antibacterial finishing (AATCC 100) of cotton fabrics treated with a solution of silver zirconium hydrogen phosphate sodium salt via plasma after 20 laundries
Figure BDA0002154445780000072
The effect of plasma treatment on physical properties was investigated. No significant change in color was observed for both cotton samples (table 18). The air permeability of the cotton sample was found to increase slightly. On the other hand, the fabric touch test was performed, and the results are shown in table 19. The treated samples were found to be free of harmful chemicals including formaldehyde, chlorinated phenols, short chain chlorinated paraffins, etc., and the results are shown in table 20.
TABLE 18 color change (AATCC evaluation procedures 1-2007) and air permeability (ASTM D737) test results for plasma treated cotton fabrics
Colour(s)Variations in Air permeability
Initial test (control) - 84.28cm3/cm2/s
Initial test 4–5 93.0cm3/cm2/s
Optimized (control) - 1.2cm3/cm2/s
Optimized 4–5 1.2cm3/cm2/s
Note:
color change/coloration
Grade 5 negligible or no color change/coloration
Grade 4 slight color change/coloration
TABLE 19 Fabric touch test results for plasma treated Cotton fabrics
Figure BDA0002154445780000081
Note:
due to the size limitations of plasma machines, the samples used for fabric touch testing are smaller than required and the results may not be reliable.
TABLE 20 hazardous chemical test results for plasma treated fabrics
Figure BDA0002154445780000082
Figure BDA0002154445780000091
iii Chitosan
Since sodium zirconium silver hydrogen phosphate has no antibacterial activity against wool, another antimicrobial agent is used to achieve the antibacterial activity against wool. Chitosan is a natural linear biological polyamino sugar obtained by alkaline deacetylation of chitin. Chitin is a major component of the protective cuticle of crustaceans (such as crabs, shrimps, lobsters) and the cell walls and mucosa of some fungi such as aspergillus. It has been found that for many common bacterial species, the minimum inhibitory concentration for inhibiting microbial growth is 0.05-0.1% (w/v).
Chitosan exhibits antibacterial activity only in acidic media. The antimicrobial activity of chitosan is reported to depend on its molecular weight and degree of deacetylation. It is generally believed that the antimicrobial mechanism stems from the protonated form of the primary amine (NH)3 +) Interaction with negatively charged residues on the surface of the microorganism. This interaction causes significant changes in cell surface and cell permeability, resulting in leakage of intracellular material.
Chitosan is used in the present invention to achieve the antimicrobial properties of wool. To apply the chitosan, the wool fabric was impregnated with a 0.5% W/v aqueous chitosan solution containing 5% acetic acid and dried at 80 ℃ and then treated with a nitrogen plasma at 400W for 1 min. Antibacterial performance was confirmed by standard evaluation (AATCC 100) and results indicated that greater than 99% reduction in bacteria was achieved. The wash durability of the treated fabrics was studied and the evaluation from the third party laboratory showed that negative results were shown in AATCC 100 evaluation where the fabrics were washed 20 times based on the BS EN ISO 6330:2012 procedure (table 22). The PetrifilmTM AC test gave a positive result, indicating that no microorganisms were present on the test sample, which microorganisms could be removed due to the antimicrobial properties obtained after treatment and/or during washing.
Due to the hydrophobic and non-reactive nature of the wool fiber surface, pre-treatment involves oxidation with peroxide and digestion with proteases; and plasma treatment is required to enable the polymer of chitosan to adhere to the surface [1 ].
In order to enhance the adsorption of chitosan in wool fibers and to improve the uniformity of its distribution, an oxidative plasma treatment, i.e. oxygen plasma, was performed [3,4 ]. The wool fabric was first treated with 200W oxygen plasma for 5min and then impregnated with a 0.5% aqueous chitosan solution containing 5% acetic acid and 4% citric acid and a 30% aqueous ethanol solution containing 4.0% sodium hypophosphite. The sample was then dried at 80 ℃ and then plasma treated with nitrogen at 400W for 1 min. However, AATCC 100 evaluation showed that after 20 washes using the BS EN ISO 6330:2012 program, no longer had antibacterial properties, i.e. was not sterilizable.
It should be noted that although no bactericidal activity was achieved for the samples treated as described above, the bacteriostatic activity measured to inhibit bacterial growth was 77-97% after 20 washes. These results indicate that the amount of active agent is insufficient for antibacterial activity.
In addition, 20 machine washes and drum dries were simulated using the wash and dry method. Laundry washing and drum drying have a detrimental effect on the quality of wool fabrics, making them unacceptable. Thus, samples for AATCC 100 evaluation were resubmitted, wherein again the samples were washed based on the BS EN ISO 6330:2012 program simulating hand washing and flat drying. Although a 50% reduction in staphylococcus aureus was still achieved after 20 washes, it had no antibacterial effect on klebsiella pneumoniae.
Similar to cotton fabric, to ensure sufficient antimicrobial active, the dose of antimicrobial agent was increased from 0.5% w/v to 2% w/v. The wool fabric was first pretreated with an oxygen plasma at 200W for 5min and then dipped into a 2% aqueous chitosan solution containing 5% acetic acid. The fabric was then treated by nitrogen plasma at 400W for 1 min. The impregnation and nitrogen plasma treatment were repeated once. In addition, the wool fabric is soaked and washed prior to the antibacterial treatment. This additional plasma pretreatment ensures that coating damage due to filling during laundering is minimized. After 20 washes, AATCC 100 evaluation showed greater than 99% reduction in both staphylococcus aureus and klebsiella pneumoniae bacteria (table 21).
TABLE 21 test results of the evaluation of the antibacterial finishing (AATCC 100) of the wool fabrics treated with plasma after 20 laundries
Figure BDA0002154445780000101
The effect of plasma treatment on physical properties was investigated. No significant change in color was observed for both cotton samples (table 22). The air permeability of the cotton sample was found to increase slightly. On the other hand, the fabric touch test was performed, and the results are shown in table 23.
TABLE 22 color change (AATCC evaluation procedure 1-2007) and air permeability (ASTM D737) test results for plasma treated wool fabrics
Color change Air permeability
Initial test (control) - 183.8cm3/cm2/s
Initial testing 4–5 171.0cm3/cm2/s
Optimized (control) - 113.2cm3/cm2/s
Optimized 4 110.4cm3/cm2/s
Note:
color change/coloration
Grade 5 negligible or no color change/coloration
Grade 4 slight color change/coloration
TABLE 23 Fabric touch test results for plasma treated wool fabrics
Figure BDA0002154445780000111
Note:
due to the size limitations of plasma machines, the samples used for fabric touch testing are smaller than required and the results may not be reliable.
Finally, table 24 summarizes the overall results of antimicrobial treatment of cotton and wool fabrics, including the treatment process, antimicrobial performance, and their physical properties.
TABLE 24 results of antimicrobial treatment of cotton and wool fabrics
Figure BDA0002154445780000121
Table 24 (continuation) summary of results of antimicrobial treatment of cotton and wool fabrics
Figure BDA0002154445780000131
Conclusion
Functional treatments using plasma technology under different conditions were investigated by varying the pressure, time and antimicrobial dose.
The antimicrobial properties of the treated fabrics were evaluated by evaluating the antimicrobial finish (AATCC 100) on the textile. Cotton and wool fabrics were found to have antimicrobial properties after laundering (even after 20 washes). The optimum treatment conditions for cotton fabric were found to be pre-treated with 10% citric acid followed by treatment with 2% W/v sodium zirconium silver hydrogen phosphate at 400W under nitrogen for 1 min. On the other hand, the optimized treatment conditions for wool fabrics are: first pre-treated with oxygen plasma at 200W for 5min, then treated twice with a 2% aqueous chitosan solution containing 5% acetic acid, dried at 80 c, and then treated with nitrogen plasma at 400W for 1 min.
Reference documents:
[1]Y.Gao and R.Cranston,“Recent Advances in Antimicrobial Treatments of Textiles”,Textile Research Journal,2008,78,60.
[2]S.-H.Hsieh,Z.K.Huang,Z.Z.Huang and Z.S.Tseng,“Antimicrobial and Physical Properties of Woolen Fabrics Cured with Citric Acid and Chitosan”,Journal of Applied Polymer Science,2004,94,1999.
[3]A.Cuesta and J.M.D.Tascon,“Shrinkage Properties of Wool Treated with Low Temperature Plasma andChitosan Biopolymer”,Textile Research Journal,1999,69,811.
[4]J.Yua,Z.Pang,J.Zhang,H.Zhou and Q.Wei,“Conductivity and Antibacterial Properties of Wool Fabrics Finished by Polyaniline/Chitosan”,Colloids and Surfaces A,2018,548,117.

Claims (2)

1. a method for preparing coated fabric, characterized in that when the fabric is wool fabric, oxygen plasma is usedPretreating fabric, treating fabric with chitosan solution, drying, and treating with nitrogen plasma at 5 × 100Pa to 8x102Pa, and the concentration of the applied chitosan solution is more than 0.05% w/v.
2. The method according to claim 1, characterized in that it comprises: the wool fabric was first pretreated with oxygen plasma at 200W for 5min, then twice with a 2% W/v aqueous chitosan solution containing 5% acetic acid, dried and then treated with nitrogen plasma at 400W for 1 min.
CN201910713099.2A 2019-08-02 2019-08-02 Antibacterial fabric obtained by plasma technology and preparation method thereof Active CN112301726B (en)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN201910713099.2A CN112301726B (en) 2019-08-02 2019-08-02 Antibacterial fabric obtained by plasma technology and preparation method thereof
PCT/CN2020/106334 WO2021023121A1 (en) 2019-08-02 2020-07-31 Anti-microbial fabric obtained by means of plasma technology and preparation method therefor

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910713099.2A CN112301726B (en) 2019-08-02 2019-08-02 Antibacterial fabric obtained by plasma technology and preparation method thereof

Publications (2)

Publication Number Publication Date
CN112301726A CN112301726A (en) 2021-02-02
CN112301726B true CN112301726B (en) 2022-06-17

Family

ID=74486589

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910713099.2A Active CN112301726B (en) 2019-08-02 2019-08-02 Antibacterial fabric obtained by plasma technology and preparation method thereof

Country Status (2)

Country Link
CN (1) CN112301726B (en)
WO (1) WO2021023121A1 (en)

Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113944056A (en) * 2021-05-31 2022-01-18 青岛大学 Method for improving inkjet printing performance of antibacterial silk fabric by adopting plasma-chitosan technology
CN115323568B (en) * 2022-08-25 2023-12-01 上海悠途实业有限公司 Soft, smooth, clean, moisture-absorbing and quick-drying fabric and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103882678A (en) * 2012-12-20 2014-06-25 青岛同冠王实业有限公司 Cotton cloth crease resistance and moisture permeation finishing method
CN105040402A (en) * 2015-03-05 2015-11-11 中霖中科环境科技(安徽)股份有限公司 Method of purifying bacteria in sewage with cotton fibers after chitosan stem grafting
CN106544863A (en) * 2015-09-18 2017-03-29 江苏阳光毛纺服装技术开发有限公司 A kind of anti-crease finishing technique of textile shirt
CN106930108A (en) * 2017-05-09 2017-07-07 深圳优普莱等离子体技术有限公司 A kind of method of textile chitosan antibacterial finishing

Family Cites Families (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US6641829B1 (en) * 2002-10-22 2003-11-04 Milliken & Company Topical application of solid antimicrobials to carpet pile fibers during carpet manufacture
US20050035327A1 (en) * 2003-08-14 2005-02-17 Canada T. Andrew Topical silver-based antimicrobial composition for wound care devices
US8110205B2 (en) * 2007-10-05 2012-02-07 Toagosei Co., Ltd. Silver-containing inorganic antibacterial
CN102978898A (en) * 2012-12-19 2013-03-20 上海汇泉实业有限公司 Preparation method of antibacterial non-woven fabric
CN106978721A (en) * 2017-03-22 2017-07-25 广西科技大学 A kind of preparation method of long-acting antibiotic textile

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103882678A (en) * 2012-12-20 2014-06-25 青岛同冠王实业有限公司 Cotton cloth crease resistance and moisture permeation finishing method
CN105040402A (en) * 2015-03-05 2015-11-11 中霖中科环境科技(安徽)股份有限公司 Method of purifying bacteria in sewage with cotton fibers after chitosan stem grafting
CN106544863A (en) * 2015-09-18 2017-03-29 江苏阳光毛纺服装技术开发有限公司 A kind of anti-crease finishing technique of textile shirt
CN106930108A (en) * 2017-05-09 2017-07-07 深圳优普莱等离子体技术有限公司 A kind of method of textile chitosan antibacterial finishing

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
"Effect of plasma superficial treatments on antibacterial functionalization and coloration of cellulosic fabrics";Nabil A. Ibrahim 等;《Applied Surface Science》;20160928;第392卷;第1126-1133页 *
"生态法羊毛织物防毡缩整理";刘炳宏;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20090615(第6期);第B024-3页 *
"等离子体处理后的毛织物壳聚糖抗菌整理";王世花 等;《印染》;20061015(第20期);第6-8页 *
"银及氧化锌纳米颗粒对棉织物的制备整理及其抗菌抗紫外性能研究";巫云萍;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20190115(第1期);第B020-1210页 *

Also Published As

Publication number Publication date
CN112301726A (en) 2021-02-02
WO2021023121A1 (en) 2021-02-11

Similar Documents

Publication Publication Date Title
Haji et al. Natural dyeing and antibacterial activity of atmospheric‐plasma‐treated nylon 6 fabric
CN112301726B (en) Antibacterial fabric obtained by plasma technology and preparation method thereof
CN109944059B (en) Graphene conductive fabric and preparation method thereof
CN106978721A (en) A kind of preparation method of long-acting antibiotic textile
CN105862418A (en) Preparation method of bacteria-resistant polypropylene nonwoven fabric
Ibrahim et al. Smart options for functional finishing of linen-containing fabrics
Moazami et al. Antibacterial properties of raw and degummed silk with nanosilver in various conditions
Zhou et al. Excellent binding effect of l-methionine for immobilizing silver nanoparticles onto cotton fabrics to improve the antibacterial durability against washing
EP3543396B1 (en) Organic antimicrobial textile
Sophonvachiraporn et al. Surface characterization and antimicrobial activity of chitosan-deposited DBD plasma-modified woven PET surface
CN109487532B (en) Hydrophilic antibacterial non-woven fabric and preparation method thereof
CA2969821A1 (en) Method for producing antimicrobial yarns and fabrics by nanoparticle impregnation
Demir et al. The comparison of the effect of enzyme, peroxide, plasma and chitosan processes on wool fabrics and evaluation for antimicrobial activity
Demir et al. A new application method of chitosan for improved antimicrobial activity on wool fabrics pretreated by different ways
CN112647294A (en) Antibacterial cotton fabric with excellent washing fastness and preparation process thereof
Yorsaeng et al. Preparation and characterization of chitosan-coated DBD plasma-treated natural rubber latex medical surgical gloves with antibacterial activities
CN112878033A (en) Antibacterial and anti-mite ramie fiber and preparation method and application thereof
Li et al. Biocidal activity of n-halamine methylenebisacrylamide grafted cotton
CN111910432A (en) Antibacterial fabric and preparation method thereof
Mostafa et al. Innovative ecological method for producing easy care characteristics and antibacterial activity onto viscose fabric using glutaraldehyde and chitosan nanoparticles
CN108221371B (en) Method for preparing antibacterial polyester by using halamine compound and silver ions
CN113445314B (en) Catechol/aminated cationic polyelectrolyte modified antibacterial non-woven fabric and preparation method thereof
Mostafa et al. Alternative microwave curing approach for imparting ease and care characteristics and antimicrobial activity to viscose fabric
Chen et al. Silver nanoparticles deposited on a cotton fabric surface via an in situ method using reactive hyperbranched polymers and their antibacterial properties
CN112301725B (en) Waterproof fabric obtained by plasma technique

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant