CN110205797B - Preparation method of cuprous oxide antibacterial textile - Google Patents
Preparation method of cuprous oxide antibacterial textile Download PDFInfo
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- CN110205797B CN110205797B CN201910520683.6A CN201910520683A CN110205797B CN 110205797 B CN110205797 B CN 110205797B CN 201910520683 A CN201910520683 A CN 201910520683A CN 110205797 B CN110205797 B CN 110205797B
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- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 48
- 239000004753 textile Substances 0.000 title claims abstract description 34
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 title claims abstract description 29
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229940112669 cuprous oxide Drugs 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000004744 fabric Substances 0.000 claims abstract description 86
- 108090000765 processed proteins & peptides Proteins 0.000 claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229920003043 Cellulose fiber Polymers 0.000 claims abstract description 32
- 238000011065 in-situ storage Methods 0.000 claims abstract description 6
- 239000011248 coating agent Substances 0.000 claims abstract description 3
- 238000000576 coating method Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims description 39
- 238000006243 chemical reaction Methods 0.000 claims description 30
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- 238000005406 washing Methods 0.000 claims description 27
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 14
- 238000009832 plasma treatment Methods 0.000 claims description 12
- 238000002791 soaking Methods 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 11
- 239000007789 gas Substances 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 230000000087 stabilizing effect Effects 0.000 claims description 6
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 5
- YPFDHNVEDLHUCE-UHFFFAOYSA-N propane-1,3-diol Chemical compound OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 229960004063 propylene glycol Drugs 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 abstract description 12
- 229910001431 copper ion Inorganic materials 0.000 abstract description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract 1
- 238000005530 etching Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000003795 chemical substances by application Substances 0.000 description 5
- 229920001795 coordination polymer Polymers 0.000 description 4
- 239000013256 coordination polymer Substances 0.000 description 4
- 230000006641 stabilisation Effects 0.000 description 3
- 238000011105 stabilization Methods 0.000 description 3
- VZSRBBMJRBPUNF-UHFFFAOYSA-N 2-(2,3-dihydro-1H-inden-2-ylamino)-N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]pyrimidine-5-carboxamide Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)C(=O)NCCC(N1CC2=C(CC1)NN=N2)=O VZSRBBMJRBPUNF-UHFFFAOYSA-N 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 description 1
- 229940035437 1,3-propanediol Drugs 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 210000000170 cell membrane Anatomy 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- WCVRQHFDJLLWFE-UHFFFAOYSA-N pentane-1,2-diol Chemical compound CCCC(O)CO WCVRQHFDJLLWFE-UHFFFAOYSA-N 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 235000013772 propylene glycol Nutrition 0.000 description 1
- 230000017854 proteolysis Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 210000000106 sweat gland Anatomy 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 230000035899 viability Effects 0.000 description 1
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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
- D06M10/00—Physical 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
- D06M10/02—Physical 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
- D06M10/025—Corona discharge or low temperature plasma
-
- 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
- D06M11/42—Oxides or hydroxides of copper, silver or gold
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/01—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with natural macromolecular compounds or derivatives thereof
- D06M15/15—Proteins or derivatives thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- 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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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Physics & Mathematics (AREA)
- Plasma & Fusion (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Microbiology (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention provides a preparation method of cuprous oxide antibacterial textile, which comprises the steps of firstly adopting low-temperature plasma to pretreat a cellulose fiber fabric, introducing amino on the surface of the fabric, and simultaneously etching the surface of the cellulose fiber fabric; then coating silk peptide solution; padding copper acetate solution again, utilizing copper ions and-COOH and-NH on silk peptide molecules2The coordination effect reduces the water solubility of silk peptide and improves the combination fastness of the silk peptide, copper ions and textiles; and then cuprous oxide is formed in situ on the textile to obtain the antibacterial textile. The obtained fabric has good antibacterial property and is washable.
Description
Technical Field
The invention belongs to the technical field of spinning, and particularly relates to a preparation method of a cuprous oxide antibacterial textile.
Background
With the improvement of living standard, the health consciousness of people is increased day by day. The porous textile fiber is easy to absorb sweat glands of a human body, and microorganisms are easy to grow and breed under proper temperature and humidity. The presence of microorganisms on textiles not only causes the textiles to mildew, but also can be harmful to the health of the user. Therefore, it is necessary to perform an antibacterial finishing of the fabric.
The antibacterial finishing agent can be divided into an inorganic antibacterial finishing agent, an organic antibacterial finishing agent and a natural antibacterial finishing agent. The inorganic antibacterial finishing agent has broad-spectrum antibacterial property and strong bactericidal capability. Research shows that the nano cuprous oxide can be adsorbed to the cell surface, and the permeability of cell membranes is increased and the viability of bacteria is reduced by destroying cell walls. However, cuprous oxide has poor binding fastness to the textile and the resulting antimicrobial textile is not resistant to washing.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of a cuprous oxide antibacterial textile, which comprises the steps of firstly adopting low-temperature plasma to pretreat a cellulose fiber fabric, and then coating a silk peptide solution; and then cuprous oxide is formed in situ on the textile to obtain the antibacterial textile. The obtained fabric has good antibacterial property and is washable.
The invention provides a preparation method of an antibacterial textile, which comprises the following steps:
(1) placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20-50 Pa; stabilizing glow discharge after 3-5min, and immediately taking out the fabric after the discharge is finished and entering the next operation;
(2) immersing the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating for a certain time at a certain temperature, drying at 80-85 ℃ after the treatment is finished, then drying at 130-145 ℃ for 3-5min, finally washing for 3-5 times by deionized water, and drying at 60-80 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70-100%; drying at 80-90 deg.C, soaking in dihydric alcohol, reacting at a certain temperature for a certain time, taking out the fabric after the reaction is finished, washing with deionized water for 3-5 times, and drying at 60-80 deg.C.
Wherein, the glow discharge power in the step (1) is 50-150W, and the discharge time is 5-15 min.
Wherein, the silk peptide in the step (2) is commercially available silk peptide powder with the molecular weight of 500-5000, and the silk peptide solution takes deionized water as a solvent, wherein the mass fraction of the silk peptide powder is 1-10%; the silk peptide solution treatment temperature is 30-50 deg.C, and the treatment time is 30-60 min.
Wherein the mass concentration of the copper acetate solution in the step (3) is 10-20 g/L.
Wherein the dihydric alcohol in the step (3) is one of 1, 4-butanediol, 1, 2-propanediol and 1, 3-propanediol, the reaction temperature is 160-180 ℃, and the reaction time is 2-4 h.
The method firstly utilizes low-temperature plasma treatment to introduce amino on the surface of the fabric and simultaneously etches the surface of the cellulose fiber fabric. The silk peptide is silkThe protein degradation product is obtained by hydrolyzing natural silk under proper conditions. The silk peptide has many hydrophilic groups (such as-OH, -COOH, -NH) on its molecular structure2NH-, etc.), and the silk peptide itself has a certain antibacterial property, but the binding fastness with the textile is poor due to its excellent water solubility. There are studies showing that: the copper ions can coordinate with carboxyl and amino on the amino acid to form a coordination polymer. The fabric is treated by silk peptide and then dipped into copper acetate solution, copper ions pass through-COOH and-NH on silk peptide molecules2The coordination forms a coordination polymer, which reduces the water solubility of the silk peptide. And finally, under the reduction action of the dihydric alcohol, copper ions adsorbed on the textile form cuprous oxide in situ, so that the textile is endowed with excellent antibacterial performance.
The invention has the beneficial effects that:
(1) the fabric is pretreated by low-temperature plasma, so that amino groups are introduced to the surface of the fabric while the roughness of the fabric is improved.
(2) The silk peptide with certain antibacterial activity is adopted to pretreat the textile, and the copper ions and the silk peptide molecules form coordination polymers, so that the loading capacity of the copper ions on the textile can be improved, and the binding fastness of the copper ions and the textile can be improved.
(3) And the in-situ generation of cuprous oxide is realized by using dihydric alcohol as a solvent and a reducing agent.
Drawings
FIG. 1 XRD patterns of the samples obtained in comparative examples 1 to 5.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It will be understood that these examples are intended to illustrate the invention and are not intended to limit the scope of the invention in any way.
Example 1
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20 Pa; stabilizing for 3min, then performing glow discharge with the discharge power of 50W for 15min, and after the discharge is finished, taking out the fabric and immediately entering the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-; then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating at 30 ℃ for 60min, after the treatment is finished, drying at 80 ℃, then baking at 130 ℃ for 5min, finally washing with deionized water for 3 times, and drying at 60 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 10g/L, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70%; drying at 80 ℃, soaking in 1, 4-butanediol, reacting at 160 ℃ for 4h, taking out the fabric after the reaction is finished, washing for 3 times by using deionized water, and drying at 60 ℃.
Comparative example 1-1 (without Low temperature plasma treatment)
(1) Dissolving commercially available silk peptide powder with the molecular weight of 500-; then soaking the cellulose fiber fabric into silk peptide solution, treating at 30 ℃ for 60min, after the treatment, drying at 80 ℃, then baking at 130 ℃ for 5min, finally washing with deionized water for 3 times, and then drying at 60 ℃ for later use;
(2) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 10g/L, padding the cellulose fiber fabric treated in the step (1) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70%; drying at 80 ℃, soaking in 1, 4-butanediol, reacting at 160 ℃ for 4h, taking out the fabric after the reaction is finished, washing for 3 times by using deionized water, and drying at 60 ℃.
Comparative examples 1-2 (No Silk peptide treatment)
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20 Pa; stabilizing for 3min, then performing glow discharge with the discharge power of 50W for 15min, and after the discharge is finished, taking out the fabric and immediately entering the next operation;
(2) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 10g/L, padding the cellulose fiber fabric treated in the step (1) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70%; drying at 80 ℃, soaking in 1, 4-butanediol, reacting at 160 ℃ for 4h, taking out the fabric after the reaction is finished, washing for 3 times by using deionized water, and drying at 60 ℃.
Comparative examples 1-3 (no cuprous oxide treatment)
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20 Pa; stabilizing for 3min, then performing glow discharge with the discharge power of 50W for 15min, and after the discharge is finished, taking out the fabric and immediately entering the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-; and (2) then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating at 30 ℃ for 60min, after the treatment is finished, drying at 80 ℃, then baking at 130 ℃ for 5min, finally washing with deionized water for 3 times, and then drying at 60 ℃.
Comparative examples 1 to 4 (pentanediol as solvent)
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20 Pa; stabilizing for 3min, then performing glow discharge with the discharge power of 50W for 15min, and after the discharge is finished, taking out the fabric and immediately entering the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-; then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating at 30 ℃ for 60min, after the treatment is finished, drying at 80 ℃, then baking at 130 ℃ for 5min, finally washing with deionized water for 3 times, and drying at 60 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 10g/L, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70%; drying at 80 ℃, immersing into 1, 2-pentanediol, reacting for 4h at 160 ℃, taking out the fabric after the reaction is finished, washing for 3 times by using deionized water, and drying at 60 ℃ to obtain the fabric.
Comparative examples 1 to 5
Dissolving copper acetate in 1, 4-butanediol, preparing a copper acetate solution with the mass concentration of 10g/L, reacting for 4h at 160 ℃, after the reaction is finished, carrying out centrifugal separation, washing solid precipitate for 3 times by using deionized water, and drying at 60 ℃.
Example 2
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Opphs plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 50 Pa; after 3min of stabilization, glow discharge is carried out, the discharge power is 150W, the discharge time is 5min, and after the discharge is finished, the fabric is taken out and immediately enters the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-5000-; then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating at 50 ℃ for 30min, after the treatment is finished, drying at 85 ℃, then baking at 145 ℃ for 3min, finally washing with deionized water for 5 times, and drying at 80 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 20g/L, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times with the padding allowance of 100%; drying at 90 ℃, immersing into 1, 2-propylene glycol, reacting at 180 ℃ for 2h, taking out the fabric after the reaction is finished, washing with deionized water for 5 times, and drying at 80 ℃.
Example 3
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Opphs plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 40 Pa; after 4min of stabilization, glow discharge is carried out, the discharge power is 100W, the discharge time is 10min, and after the discharge is finished, the fabric is taken out and immediately enters the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-5000-; then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating at 40 ℃ for 40min, after the treatment is finished, drying at 82 ℃, then baking at 135 ℃ for 4min, finally washing with deionized water for 4 times, and drying at 70 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 15g/L, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 80%; drying at 85 ℃, immersing into 1, 3-propylene glycol, reacting at 170 ℃ for 3h, taking out the fabric after the reaction is finished, washing for 4 times by deionized water, and drying at 70 ℃ to obtain the fabric.
Example 4
(1) Placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 30 Pa; after 3.5min of stabilization, glow discharge is carried out, the discharge power is 120W, the discharge time is 8min, and after the discharge is finished, the fabric is taken out and immediately enters the next operation;
(2) dissolving commercially available silk peptide powder with the molecular weight of 500-5000-; then, soaking the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating for 45min at 45 ℃, drying at 83 ℃ after the treatment is finished, then baking for 3.5min at 140 ℃, finally washing for 4 times by deionized water, and drying at 75 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution with the mass concentration of 12g/L, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 90%; drying at 83 ℃, immersing into 1, 4-butanediol, reacting at 175 ℃ for 3.5h, taking out the fabric after the reaction is finished, washing for 4 times by using deionized water, and drying at 75 ℃ to obtain the fabric.
Example 5
20944.2-2007 evaluation of antibacterial Properties of textiles part 2: absorption method determines the antibacterial properties of finished fabrics. antibacterial property test: according to GB/T
Antibacterial effect wash resistance test: the fabric antibacterial effect water washing resistance test is carried out according to the test condition A1M in GB/T12490-. And after the specified washing times are reached, fully washing the sample by using water, and airing.
The antibacterial property test results of the fabric are as follows:
TABLE 1 antibacterial Properties of the fabrics
As can be seen from Table 1, the fabrics obtained in examples 1-4 have excellent antibacterial properties against Escherichia coli, Staphylococcus aureus, Bacillus subtilis, and the finished fabric has excellent wash fastness. In comparative example 1-1, the amount of silk peptide coated on the fabric without low temperature plasma treatment was small and the amount of cuprous oxide finally attached to the fabric was small, and thus the antibacterial activity of the resulting fabric was inferior, and the fabric also had good washing fastness because the silk peptide and cuprous oxide formed a coordination polymer on the fabric, and the cuprous oxide and silk peptide eluted from the fabric during washing were mechanically hindered more. In comparative examples 1-2, the fabric was not treated with silk peptide, which resulted in a decrease in the amount of copper ions adsorbed on the fabric, a decrease in the amount of cuprous oxide generated in situ, and no synergistic antibacterial effect of silk peptide, and thus, the antibacterial activity of the finished fabric was poor. Because no coordination between copper ions and silk peptide exists, the generated cuprous oxide is only attached by machinery, and therefore, the obtained fabric has poor antibacterial effect and poor water washing resistance. In comparative examples 1 to 3, since the fabric was not treated with cuprous oxide, the antibacterial property of the fabric was provided only by the silk peptide, and since the silk peptide had excellent water solubility, the obtained fabric was inferior in both antibacterial property and antibacterial effect and water-washing resistance. In comparative examples 1 to 4, since pentanediol is poor in reducibility and copper ions cannot be reduced to cuprous oxide, the antibacterial performance of the obtained fabric is mainly provided by silk peptide, and since a small amount of copper ions are adsorbed on the fabric, the antibacterial performance of the obtained fabric is superior to that of comparative examples 1 to 3.
Claims (5)
1. A preparation method of cuprous oxide antibacterial textile is characterized by comprising the following steps: the preparation method comprises the following steps of,
firstly, pretreating a cellulose fiber fabric by adopting low-temperature plasma, and then coating a silk peptide solution; then, nano cuprous oxide is formed in situ on the textile to obtain the antibacterial textile; the method comprises the specific steps of carrying out the following steps,
(1) placing the cellulose fiber fabric on a frame in a cavity of a DT-01 low-temperature plasma treatment instrument produced by Oppu plasma science and technology Limited, Suzhou, starting a vacuum pump, introducing nitrogen into the plasma cavity when the vacuum degree in the reaction cavity is 5Pa, and adjusting the gas flow until the vacuum degree in the reaction cavity is 20-50 Pa; stabilizing glow discharge after 3-5min, and immediately taking out the fabric after the discharge is finished and entering the next operation;
(2) immersing the cellulose fiber fabric treated in the step (1) into a silk peptide solution, treating for a certain time at a certain temperature, drying at 80-85 ℃ after the treatment is finished, then drying at 130-145 ℃ for 3-5min, finally washing for 3-5 times by deionized water, and drying at 60-80 ℃ for later use;
(3) dissolving copper acetate in deionized water to prepare a copper acetate solution, padding the cellulose fiber fabric treated in the step (2) with the copper acetate solution, and padding for two times, wherein the padding allowance is 70-100%; drying at 80-90 deg.C, and soaking in dihydric alcohol, wherein the dihydric alcohol is one of 1, 4-butanediol, 1, 2-propylene glycol, and 1, 3-propylene glycol; reacting for a certain time at a certain temperature, taking out the fabric after the reaction is finished, washing the fabric for 3 to 5 times by using deionized water, and drying the fabric at the temperature of between 60 and 80 ℃.
2. The preparation method of the cuprous oxide antibacterial textile as claimed in claim 1, wherein the cuprous oxide antibacterial textile comprises the following steps: the glow discharge power in the step (1) is 50-150W, and the discharge time is 5-15 min.
3. The preparation method of the cuprous oxide antibacterial textile as claimed in claim 1, wherein the cuprous oxide antibacterial textile comprises the following steps: the silk peptide in the step (2) is commercially available silk peptide powder with the molecular weight of 500-5000, and the silk peptide solution takes deionized water as a solvent, wherein the mass fraction of the silk peptide powder is 1-10%; the silk peptide solution treatment temperature is 30-50 deg.C, and the treatment time is 30-60 min.
4. The preparation method of the cuprous oxide antibacterial textile as claimed in claim 1, wherein the cuprous oxide antibacterial textile comprises the following steps: the mass concentration of the copper acetate solution in the step (3) is 10-20 g/L.
5. The preparation method of the cuprous oxide antibacterial textile as claimed in claim 1, wherein the cuprous oxide antibacterial textile comprises the following steps: the reaction temperature in the step (3) is 160-180 ℃, and the reaction time is 2-4 h.
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