CN112276107A - Nano-copper particles and application thereof in preparation of nano-copper fabric after-finishing agent - Google Patents
Nano-copper particles and application thereof in preparation of nano-copper fabric after-finishing agent Download PDFInfo
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- CN112276107A CN112276107A CN201910674790.4A CN201910674790A CN112276107A CN 112276107 A CN112276107 A CN 112276107A CN 201910674790 A CN201910674790 A CN 201910674790A CN 112276107 A CN112276107 A CN 112276107A
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- deionized water
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 61
- 239000010949 copper Substances 0.000 title claims abstract description 61
- 239000002245 particle Substances 0.000 title claims abstract description 55
- 239000004744 fabric Substances 0.000 title claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 15
- 238000010438 heat treatment Methods 0.000 claims abstract description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 5
- 150000001879 copper Chemical class 0.000 claims abstract description 5
- 239000003513 alkali Substances 0.000 claims abstract description 4
- 238000004321 preservation Methods 0.000 claims abstract description 3
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- 229920005989 resin Polymers 0.000 claims description 4
- 239000011347 resin Substances 0.000 claims description 4
- 239000004925 Acrylic resin Substances 0.000 claims description 3
- 229920000178 Acrylic resin Polymers 0.000 claims description 3
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical group [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 3
- 229920005749 polyurethane resin Polymers 0.000 claims description 3
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- 239000004814 polyurethane Substances 0.000 claims description 2
- 239000002105 nanoparticle Substances 0.000 claims 3
- 230000007613 environmental effect Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 7
- 241000894006 Bacteria Species 0.000 description 6
- 239000003242 anti bacterial agent Substances 0.000 description 5
- 239000004753 textile Substances 0.000 description 5
- 241000222122 Candida albicans Species 0.000 description 4
- 241000588724 Escherichia coli Species 0.000 description 4
- 241000191967 Staphylococcus aureus Species 0.000 description 4
- 230000001580 bacterial effect Effects 0.000 description 4
- 229940095731 candida albicans Drugs 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 230000001954 sterilising effect Effects 0.000 description 3
- 238000004659 sterilization and disinfection Methods 0.000 description 3
- 239000000725 suspension Substances 0.000 description 3
- 206010059866 Drug resistance Diseases 0.000 description 2
- 210000000170 cell membrane Anatomy 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- SXTLQDJHRPXDSB-UHFFFAOYSA-N copper;dinitrate;trihydrate Chemical compound O.O.O.[Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O SXTLQDJHRPXDSB-UHFFFAOYSA-N 0.000 description 2
- 239000000675 fabric finishing Substances 0.000 description 2
- 238000009962 finishing (textile) Methods 0.000 description 2
- 239000001963 growth medium Substances 0.000 description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 description 1
- 239000006159 Sabouraud's agar Substances 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000003899 bactericide agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 238000012258 culturing Methods 0.000 description 1
- 210000000805 cytoplasm Anatomy 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000000787 lecithin Substances 0.000 description 1
- 235000010445 lecithin Nutrition 0.000 description 1
- 229940067606 lecithin Drugs 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000006916 nutrient agar Substances 0.000 description 1
- 230000036542 oxidative stress Effects 0.000 description 1
- -1 oxygen ions Chemical class 0.000 description 1
- 238000004917 polyol method Methods 0.000 description 1
- 239000000244 polyoxyethylene sorbitan monooleate Substances 0.000 description 1
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 description 1
- 229920000053 polysorbate 80 Polymers 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001850 reproductive effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
Images
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/263—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/564—Polyureas, polyurethanes or other polymers having ureide or urethane links; Precondensation products forming them
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M16/00—Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention discloses a nano-copper particle, which is in a porous particle structure shape, has the particle size of 50-200nm, and comprises the following steps: dissolving copper salt and alkali in deionized water, and uniformly stirring in a supercritical reaction kettle; step two, heating the reaction kettle to 150 ℃ below zero, adding polyhydric alcohol as a reducing agent, heating to 220 ℃ below zero under the stirring state, increasing the pressure to 10-20MPA, and carrying out heat preservation reaction for 10-22 hours; and step three, after the reaction is finished, filtering out a reaction product after the reaction device is cooled to room temperature, washing with absolute ethyl alcohol, then washing with deionized water, and then drying in vacuum at 80-120 ℃ for 10-22 hours to obtain the nano copper particles. The invention also discloses the application of the nano-copper particles in preparing the nano-copper fabric after-finishing agent, and the nano-copper fabric after-finishing agent has good antibacterial effect when being used on fabrics such as fabrics and the like, and has huge environmental protection advantages and wide market prospect.
Description
Technical Field
The invention relates to a nano-copper particle, and in addition, the invention also relates to application of the nano-copper particle in preparing a nano-copper fabric after-finishing agent.
Background
Heavy metals such as silver and copper have the advantages of broad-spectrum antibacterial property, good dispersibility, small drug resistance and the like, and are applied to various biological materials and medical instruments. Silver and copper have two bactericidal mechanisms, 1) metal ions are positively charged, cell membranes are negatively charged, and the metal ions can firmly adsorb the cell membranes by means of coulomb attraction, penetrate the cell walls, cause the rupture of the cell walls, cause the outflow of cytoplasm and cause the death of bacteria. 2) The metal can be used as a catalytic active center to stimulate water or oxygen in the air to generate hydroxyl radicals (-OH) and active oxygen ions (O)2-) Thereby generating oxidative stress to destroy the reproductive capacity of the bacteria and leading to the death of the bacteria. Since silver is expensive and its antibacterial effect is affected by light and heat, it is easily reduced to lower the antibacterial effect after long-term use. Therefore, it is very meaningful to research a novel antibacterial material of copper.
Chinese patent CN109944065A discloses a preparation method of an antibacterial fabric finishing agent, the bactericide prepared by the method is an organic matter, the preparation cost is high, the process is complex, and the antibacterial effect is general; chinese patent CN10103668954A discloses a preparation method of an antibacterial fabric finishing agent containing compound organic matters, the antibacterial agent prepared by the method is a compound organic matter, the process is complex, and the bacterial drug resistance is easy to cause; chinese patent CN107287905A discloses a preparation method of an antibacterial finishing agent for silk fabrics, and the antibacterial agent prepared by the method is an antibacterial composition, has a common antibacterial effect and has a certain influence on the environment.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, according to embodiments of the present invention, it is desirable to provide a nano-copper particle having a porous particle structure, a large surface area, a strong adsorption effect, and thus a strong sterilization effect. Furthermore, the method is simple. The invention also aims to provide the nano-copper particles for the antibacterial agent of the fabric after-finishing agent.
According to the embodiment, the nano copper particle provided by the invention is in a porous particle structure shape, the particle size is 50-200nm, and the preparation method comprises the following steps:
dissolving copper salt and alkali in deionized water, and uniformly stirring in a supercritical reaction kettle;
step two, heating the reaction kettle to 150 ℃ below zero, adding polyhydric alcohol as a reducing agent, heating to 220 ℃ below zero under the stirring state, increasing the pressure to 10-20MPA, and carrying out heat preservation reaction for 10-22 hours;
and step three, after the reaction is finished, filtering out a reaction product after the reaction device is cooled to room temperature, washing with absolute ethyl alcohol, then washing with deionized water, and then drying in vacuum at 80-120 ℃ for 10-22 hours to obtain the nano copper particles.
Preferably, in step one, the copper salt is copper acetate, copper sulfate or copper nitrate.
Preferably, in step one, the base is sodium hydroxide or potassium hydroxide.
Preferably, in step two, the reducing agent is ethylene glycol or propylene glycol.
According to an embodiment, the application of the nano-copper particles in preparing the nano-copper fabric after-finishing agent comprises the following steps:
step four, preparing the antibacterial liquid from the nano-copper particles and deionized water in a weight ratio of 1:4, and preparing the antibacterial liquid and resin in a weight ratio of 1:1 into the nano-copper fabric after-finishing agent.
Preferably, in step four, the resin is polyurethane or acrylic.
Compared with the prior art, the following examples and experimental examples prove that the nano copper particles are prepared by a supercritical polyol method, have a porous particle structure, large specific surface area and good antibacterial effect, can be widely applied to the fields of textile products, internal and external wall coatings and the like, and have huge environmental protection advantages and wide market prospects. The nano-copper fabric after-finishing agent prepared by the invention also has the advantages of simple preparation method, low cost, easy industrialization and the like.
Drawings
FIG. 1A picture of a porous particle of nano-copper particles is obtained in example 1.
Detailed Description
The invention is further illustrated with reference to the following figures and specific examples. These examples are to be construed as merely illustrative and not limitative of the remainder of the disclosure in any way whatsoever. After reading the description of the invention, one skilled in the art can make various changes and modifications to the invention, and such equivalent changes and modifications also fall into the scope of the invention defined by the claims.
The starting materials used in the following examples of the present invention are all commercially available products unless otherwise specified.
Example 1
(1) Dissolving 8g of blue vitriod and 4.5g of sodium hydroxide in 80ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 100 ℃, adding 1.5g of glycol solution, and uniformly stirring;
(3) heating the reaction kettle to 200 ℃, increasing the pressure in the reaction kettle to 10MPa, and reacting for 14 hours under a stirring state;
(4) after the reaction is finished, after the reaction device is cooled to room temperature, filtering out a reaction product, washing the reaction product with absolute ethyl alcohol for three times, then washing the reaction product with deionized water for three times, and then drying the reaction product in vacuum at the temperature of 80 ℃ for 12 hours to obtain nano copper particles, wherein the nano copper particles are in porous particle structures, and the particle size of the nano copper particles is 50-200nm as shown in figure 1;
the prepared nano-copper particles are prepared into an antibacterial liquid by the weight ratio of 1:4 and water, and then are prepared into a nano-copper fabric after-finishing agent by the weight ratio of 1:1 and polyurethane resin.
Example 2
(1) Dissolving 8.2g of copper nitrate trihydrate and 6.2g of potassium hydroxide in 100ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 110 ℃, adding 2g of propylene glycol solution, and uniformly stirring;
(3) heating the reaction kettle to 190 ℃, increasing the pressure in the reaction kettle to 12MPa, and reacting for 16 hours under a stirring state;
(4) after the reaction is finished, after the reaction device is cooled to room temperature, filtering out a reaction product, washing the reaction product with absolute ethyl alcohol for three times, then washing the reaction product with deionized water for three times, and then carrying out vacuum drying at the temperature of 90 ℃ for 14 hours to obtain nano copper particles, wherein the nano copper particles are in porous particle structures, and the particle size of the nano copper particles is 50-200 nm;
the prepared nano-copper particles are prepared into an antibacterial liquid by the weight ratio of 1:4 and water, and then are prepared into a nano-copper fabric after-finishing agent by the weight ratio of 1:1 and acrylic resin.
Example 3
(1) Dissolving 10g of copper acetate and 5g of sodium hydroxide in 120ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 120 ℃, adding 1.5g of glycol solution, and uniformly stirring;
(3) heating the reaction kettle to 200 ℃, increasing the pressure in the reaction kettle to 15MPa, and reacting for 18 hours under a stirring state;
(4) after the reaction is finished, after the reaction device is cooled to room temperature, filtering out a reaction product, washing the reaction product with absolute ethyl alcohol for three times, then washing the reaction product with deionized water for three times, and then drying the reaction product in vacuum at the temperature of 100 ℃ for 16 hours to obtain nano copper particles, wherein the nano copper particles are in porous particle structures, and the particle size of the nano copper particles is 50-200 nm;
the prepared nano-copper particles are prepared into an antibacterial liquid by the weight ratio of 1:4 and water, and then are prepared into a nano-copper fabric after-finishing agent by the weight ratio of 1:1 and polyurethane resin.
Example 4
(1) Dissolving 9g of copper nitrate trihydrate and 6.5g of potassium hydroxide in 120ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 130 ℃, adding 2g of propylene glycol solution, and uniformly stirring;
(3) heating the reaction kettle to 190 ℃, increasing the pressure in the reaction kettle to 18MPa, and reacting for 20 hours under a stirring state;
(4) after the reaction is finished, after the reaction device is cooled to room temperature, filtering out a reaction product, washing the reaction product with absolute ethyl alcohol for three times, then washing the reaction product with deionized water for three times, and then drying the reaction product in vacuum at the temperature of 120 ℃ for 18 hours to obtain nano copper particles, wherein the nano copper particles are in porous particle structures, and the particle size of the nano copper particles is 50-200 nm;
the prepared nano-copper particles are prepared into an antibacterial liquid by the weight ratio of 1:4 and water, and then are prepared into a nano-copper fabric after-finishing agent by the weight ratio of 1:1 and acrylic resin.
Test examples
Test method
Adding the nano-copper fabric after-finishing agent prepared in the examples 1-4 into a water tank of a setting machine according to the proportion of 0.5%, 1%, 1.5% and 2% respectively; then the textile is dipped, baked at high temperature and dried by a setting machine, and the antibacterial agent is added into the textile. The prepared fabric containing the antibacterial agent is tested for the effects of resisting candida albicans (ATCC10231), staphylococcus aureus (ATCC 6538) and escherichia coli (ATCC 8099) according to the AATCC100-2012 textile antibacterial performance test standard. The standard of the antibacterial performance test is the American AATCC-100 test method. The method comprises the following steps:
(1) cutting each group of textile containing nano copper fiber into pieces, processing into 4.8cm round pieces, placing in a 120 ℃ oven for sterilization for 20min, and taking out;
(2) inoculating Candida albicans to Sabouraud's agar culture medium, inoculating Staphylococcus aureus and Escherichia coli to nutrient agar culture medium, culturing at 37 deg.C for 24 hr, selecting 6 th generation culture, washing with PBS and diluting to obtain bacterial suspension, recovering bacteria number (6-9) x104cfu/ml；
(3) At room temperature of 25 ℃, respectively adding 1ml of bacterial suspension into each group of yarns, transferring the bacterial suspension into a sterile test tube filled with a neutralizer, oscillating the neutralizer into PBS containing 20g/L polyoxyethylene sorbitan monooleate, 10g/L lecithin and 5g/L sodium thiosulfate on an oscillating table for 24h, extracting a sample solution, comparing with a blank control sample, and calculating the sterilization rate of each group. The experiment was performed in triplicate.
As can be seen from table 1, the nano-copper fabric after-finishing agents prepared in examples 1 to 4 have a particle structure and a large surface area, can adsorb more bacteria, and have a high antibacterial effect; after 2% of nano copper fabric after-finishing agent and 24 hours of water tank liquor are added, the average killing rate of the prepared fabric to candida albicans after 24 hours is over 97%, and the killing rate to staphylococcus aureus and escherichia coli is over 95%.
TABLE 1 average kill rate of bacteria after 24 hours for examples 1-4
| Candida albicans% | Staphylococcus aureus% | Escherichia coli% | |
| Example 1 | 85.7 | 86.9 | 87.8 |
| Example 2 | 90.2 | 91.2 | 90.5 |
| Example 3 | 94.5 | 93.4 | 92.4 |
| Example 4 | 97.8 | 96.6 | 95.9 |
Claims (7)
1. A nano-copper particle is characterized in that the shape of the nano-copper particle is a porous particle structure type, the particle size of the nano-copper particle is 50-200nm, and the preparation method comprises the following steps:
dissolving copper salt and alkali in deionized water, and uniformly stirring in a supercritical reaction kettle;
step two, heating the reaction kettle to 150 ℃ below zero, adding polyhydric alcohol as a reducing agent, heating to 220 ℃ below zero under the stirring state, increasing the pressure to 10-20MPA, and carrying out heat preservation reaction for 10-22 hours;
and step three, after the reaction is finished, filtering out a reaction product after the reaction device is cooled to room temperature, washing with absolute ethyl alcohol, then washing with deionized water, and then drying in vacuum at 80-120 ℃ for 10-22 hours to obtain the nano copper particles.
2. The copper nanoparticles as claimed in claim 1, wherein in the first step, the copper salt is copper acetate, copper sulfate or copper nitrate.
3. The copper nanoparticles as claimed in claim 1, wherein in the first step, the alkali is sodium hydroxide or potassium hydroxide.
4. The copper nanoparticles as claimed in claim 1, wherein in the second step, the reducing agent is ethylene glycol or propylene glycol.
5. Use of the nano-copper particles according to any one of claims 1 to 4 for the preparation of a nano-copper fabric after-finish.
6. Use according to claim 5, characterized in that it comprises the following steps:
step four, preparing the antibacterial liquid from the nano-copper particles and deionized water in a weight ratio of 1:4, and preparing the antibacterial liquid and resin in a weight ratio of 1:1 into the nano-copper fabric after-finishing agent.
7. The use according to claim 6, wherein in step four, the resin is a polyurethane or acrylic resin.
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Denomination of invention: Nano copper particles and their applications in the preparation of nano copper fabric finishing agents Effective date of registration: 20231030 Granted publication date: 20230106 Pledgee: Bank of China Limited by Share Ltd. Shanghai Development Zone Pudong branch Pledgor: SHANGHAI HUZHENG INDUSTRIAL CO.,LTD. Registration number: Y2023980063101 |