CN113170785A - Copper antibacterial composite material and preparation method thereof - Google Patents
Copper antibacterial composite material and preparation method thereof Download PDFInfo
- Publication number
- CN113170785A CN113170785A CN202110370204.4A CN202110370204A CN113170785A CN 113170785 A CN113170785 A CN 113170785A CN 202110370204 A CN202110370204 A CN 202110370204A CN 113170785 A CN113170785 A CN 113170785A
- Authority
- CN
- China
- Prior art keywords
- copper
- amino
- resin
- composite material
- propanol
- 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.)
- Pending
Links
Images
Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
- A01N25/10—Macromolecular compounds
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
- A01N59/20—Copper
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Zoology (AREA)
- Nanotechnology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Environmental Sciences (AREA)
- Agronomy & Crop Science (AREA)
- Physics & Mathematics (AREA)
- Toxicology (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a copper antibacterial composite material and a preparation method thereof. The invention has the advantages of low preparation cost, simple and feasible process, no expensive and toxic reducing agent adopted in the preparation process and the like, is suitable for large-scale preparation, and the prepared material has excellent antibacterial activity.
Description
Technical Field
The invention relates to the field of biological antibiosis, in particular to a copper antibacterial composite material and a preparation method thereof.
Background
Copper nanoparticles have excellent physical and chemical properties, have attracted great interest in many fields such as chemistry, physics, material science, and bioscience, and have been widely used as precursors of conductive structures incorporated in printed circuit boards, Radio Frequency Identification (RFID) tags, flexible displays, and other electronic devices, and they have also been added as additives to lubricating oils, and exhibit excellent anti-wear and anti-friction properties in base oils due to their enhanced thermal and electrical conductivity, and in addition, they have high antibacterial activity and can replace expensive silver nanoparticles as potential antibacterial materials for many applications in biological antibacterial applications.
The copper nanoparticles can be prepared by chemical reduction method using reducing agent such as sodium borohydride, H2CO, glucose, ascorbic acid, etc., in the presence of a surfactant to reduce CuCl or CuCl2、CuSO4Or Cu (NO)3)2The preparation method of the copper nanoparticles is complex, the preparation cost is high, and the copper has low optimized reduction potential and is easy to oxidize in the air to lose antibacterial activity.
Disclosure of Invention
The invention aims to provide a preparation method of a copper antibacterial composite material, which comprises the steps of dispersing copper oxide or cuprous oxide in hydroxylamine, carrying out heat treatment, reducing part or all of the copper oxide or cuprous oxide into elemental copper by the hydroxylamine to obtain a nano material containing the elemental copper, and further compounding the nano material with resin to obtain the copper antibacterial composite material.
The specific technical scheme for realizing the purpose of the invention is as follows:
a preparation method of a copper antibacterial composite material is characterized by comprising the following specific steps:
1) stirring and mixing copper oxide and hydroxylamine uniformly at room temperature to obtain copper oxide dispersion liquid, heating the dispersion liquid at 80-180 ℃ for 20-180 minutes, cooling to room temperature, and adding a solvent for washing to obtain a nano material containing elemental copper;
2) adding the elemental copper-containing nano material prepared in the step 1) into an alcohol solution containing resin, uniformly dispersing for 1-12 hours, and then carrying out vacuum drying to obtain the copper antibacterial composite material;
wherein:
the copper oxide is copper oxide or cuprous oxide;
the molar mass ratio of the copper oxide to the hydroxylamine is 10-1: 1-4;
the mass ratio of the elemental copper-containing nano material to the resin is 10-1: 1-10;
the hydroxylamine is at least one of 1-ethanolamine, 2-amino-propanol, 3-amino-propanol, 2-amino-1-butanol, 3-amino-butanol, 4-amino-butanol, 2-amino-pentanol, 3-amino-pentanol, 5-amino-pentanol and 2-amino-2-methyl-1-propanol;
the solvent is water or ethanol;
the resin is at least one of epoxy resin, acrylic resin, alkyd resin, polyester resin, amino resin and organic silicon resin;
the alcohol is: at least one of ethanol, methanol, dimethanol and propanol, all of which are analytically pure.
A copper antibacterial composite material prepared by the method.
The invention has the advantages of
The preparation method of the elemental copper-containing nano material is simple, hydroxylamine is used as a solvent and a reducing agent, the cost is low, the amplification preparation is easy, the elemental copper nano material is easy to be compounded with resin, and the copper antibacterial nano composite material is easy to prepare.
Drawings
FIG. 1 is a SEM image of elemental copper-containing nanomaterial obtained in example 1 of the present invention;
FIG. 2 is a SEM image of elemental copper-containing nanomaterial obtained in example 1 of the present invention;
FIG. 3 is a schematic diagram of a copper antibacterial composite material prepared in example 7 of the present invention;
FIG. 4 is a comparison graph of the antibacterial effect of the copper antibacterial composite material prepared in example 7 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following specific examples and drawings, and the present invention is not limited to the following examples. Variations that may occur to those skilled in the art are included herein without departing from the spirit and scope of the inventive concept, and the scope of the appended claims is to be accorded the full scope of the claims.
Example 1
1.45 g of Cu2O is slowly added into a round bottom flask containing 4.8 g of ethanolamine, and the mixture is magnetically stirred at room temperature, is heated by oil bath after being stirred for 10 minutes, is heated to 140 ℃, is cooled at room temperature after being reacted for 60 minutes, and is washed with ethanol for three times to obtain 1.24 g of nano material containing the elemental copper, and the SEM pictures of the nano material are shown in figure 1 and figure 2.
Example 2
1.45 g of Cu2And slowly adding O into a round bottom flask filled with 2.8 g of 2-amino-propanol, magnetically stirring at room temperature, stirring for 10 minutes, heating by adopting an oil bath, heating the solution to 120 ℃, reacting for 120 minutes, cooling at room temperature, and washing with ethanol for three times to obtain 1.34 g of the nano material containing the elemental copper.
Example 3
1.25 g of Cu2Slowly adding O into a round bottom flask filled with 2.0 g of 3-amino-pentanol, magnetically stirring at room temperature, stirring for 10 minutes, heating by adopting an oil bath, heating the solution to 160 ℃, reacting for 40 minutes, cooling at room temperature, and washing with ethanol for three times to obtain 1.14 g of the nano material containing the elemental copper.
Example 4
Slowly adding 0.9 g of CuO into a round bottom flask filled with 1.0 g of 2-amino-2-methyl-1-propanol, magnetically stirring at room temperature, heating by adopting an oil bath after stirring for 10 minutes, heating the solution to 140 ℃, reacting for 50 minutes, cooling at room temperature, and washing with water for three times to obtain 0.82 g of the nano material containing the elemental copper.
Example 5
Slowly adding 3.1 g of CuO into a round bottom flask filled with 6.0 g of 2-amino-1-butanol, magnetically stirring at room temperature, heating by adopting an oil bath after stirring for 10 minutes, heating the solution to 140 ℃, reacting for 60 minutes, cooling at room temperature, and washing with water for three times to obtain 2.8 g of the nano material containing the elemental copper.
Example 6
Slowly adding 2.4 g of CuO into a round bottom flask filled with 2.0 g of 2-amino-1-butanol and 1.0 g of ethylene glycol, magnetically stirring at room temperature, heating by adopting an oil bath after stirring for 10 minutes, heating the solution to 130 ℃, reacting for 100 minutes, cooling at room temperature, and washing with water for three times to obtain 2.2 g of the nano material containing the elemental copper.
Example 7
1.24 g of the nanoparticles containing elemental copper prepared in example 1 was added to 100 g of an ethanol solution of silicone resin, dispersed in the ethanol solution of resin for 2 hours, and vacuum-dried to obtain a copper antibacterial composite material, as shown in fig. 3, which is a real image of the obtained copper silicone resin composite material.
The obtained copper organic silicon resin composite material is subjected to an antibacterial activity test, wherein fig. 4 (a) is a schematic diagram of a colony without any material, and fig. 4 (B) is an antibacterial activity diagram of the copper organic silicon resin composite material with 20 mg, and the antibacterial effect is illustrated; FIG. 4 (C) is a test chart of the inhibition zone of the composite material added with 0.1 mg of copper-silicone resin; fig. 4 (B) and 4 (C) are two biological test methods for testing antibacterial activity.
Example 8
1.34 g of the nanoparticles containing elemental copper prepared in example 2 was added to 100 g of a methanol solution of acrylic resin, and the copper-containing antibacterial composite material was prepared after 4 hours of compounding and vacuum drying.
Example 9
1.14 g of the nanoparticles containing elemental copper prepared in example 3 were added to 50 g of dimethanol solution of alkyd resin, compounded for 1 hour and vacuum dried to prepare the copper-containing antibacterial composite.
Example 10
0.8 g of the nanoparticles containing elemental copper prepared in example 4 was added to 120 g of an ethanol solution of alkyd resin, compounded for 12 hours and vacuum-dried to prepare the copper-containing antibacterial composite material.
Example 11
2.8 g of the nanoparticles containing elemental copper prepared in example 5 were added to 100 g of a methanol solution of polyester resin and 20 g of silicone resin, and the copper-containing antibacterial composite material was prepared by compositing for 8 hours and vacuum drying.
Example 12
2.2 g of the nanoparticles containing elemental copper prepared in example 6 were added to a dimethyl alcohol solution of 60 g of polyester resin and 10 g of amine-based resin, and the copper-containing antibacterial composite material was prepared by compounding for 10 hours and vacuum drying.
Claims (2)
1. The preparation method of the copper antibacterial composite material is characterized by comprising the following specific steps of:
1) stirring and mixing copper oxide and hydroxylamine uniformly at room temperature to obtain copper oxide dispersion liquid, heating the dispersion liquid at 80-180 ℃ for 20-180 minutes, cooling to room temperature, and adding a solvent for washing to obtain a nano material containing elemental copper;
2) adding the elemental copper-containing nano material prepared in the step 1) into an alcohol solution containing resin, uniformly dispersing for 1-12 hours, and then carrying out vacuum drying to obtain the copper antibacterial composite material;
wherein:
the copper oxide is copper oxide or cuprous oxide;
the molar mass ratio of the copper oxide to the hydroxylamine is 10-1: 1-4;
the mass ratio of the elemental copper-containing nano material to the resin is 10-1: 1-10;
the hydroxylamine is at least one of 1-ethanolamine, 2-amino-propanol, 3-amino-propanol, 2-amino-1-butanol, 3-amino-butanol, 4-amino-butanol, 2-amino-pentanol, 3-amino-pentanol, 5-amino-pentanol and 2-amino-2-methyl-1-propanol;
the solvent is water or ethanol;
the resin is at least one of epoxy resin, acrylic resin, alkyd resin, polyester resin, amino resin and organic silicon resin;
the alcohol is: at least one of ethanol, methanol, dimethanol and propanol, all of which are analytically pure.
2. A copper antimicrobial composite made by the method of claim 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110370204.4A CN113170785A (en) | 2021-04-07 | 2021-04-07 | Copper antibacterial composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110370204.4A CN113170785A (en) | 2021-04-07 | 2021-04-07 | Copper antibacterial composite material and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113170785A true CN113170785A (en) | 2021-07-27 |
Family
ID=76923138
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110370204.4A Pending CN113170785A (en) | 2021-04-07 | 2021-04-07 | Copper antibacterial composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113170785A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103724938A (en) * | 2013-12-06 | 2014-04-16 | 黑龙江大学 | Method for preparing nano-copper/epoxy resin composite material |
| CN103740210A (en) * | 2014-01-26 | 2014-04-23 | 南通广泰生化制品有限公司 | Microporous type nano coating |
| CN103752843A (en) * | 2014-01-07 | 2014-04-30 | 华东师范大学 | Synthesis method of superfine copper powder |
-
2021
- 2021-04-07 CN CN202110370204.4A patent/CN113170785A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103724938A (en) * | 2013-12-06 | 2014-04-16 | 黑龙江大学 | Method for preparing nano-copper/epoxy resin composite material |
| CN103752843A (en) * | 2014-01-07 | 2014-04-30 | 华东师范大学 | Synthesis method of superfine copper powder |
| CN103740210A (en) * | 2014-01-26 | 2014-04-23 | 南通广泰生化制品有限公司 | Microporous type nano coating |
Non-Patent Citations (1)
| Title |
|---|
| 刘欣: "纳米铜抗菌性能研究", 《中国优秀博硕士学位论文全文数据库（硕士） 工程科技Ⅰ辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101653828B (en) | Silver nanoparticles and process for producing same | |
| CN101798462B (en) | Graphene/conductive polymer composite film and preparation method thereof | |
| KR100702595B1 (en) | Metal nanoparticles and method for producing the same | |
| CN110724493B (en) | Multi-walled carbon nanotube/ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof | |
| KR101303324B1 (en) | Expanded graphite having high conductivity and manufacturing method of them | |
| CN105633266A (en) | Preparation method for composite thermoelectric film with flexible reduced graphene oxide and tellurium nano wires | |
| CN104471652B (en) | Silver composition and silver composition form base material | |
| CN110681872B (en) | Preparation method of copper/silver corn-shaped structure nanoparticles | |
| CN111117265A (en) | Core-shell structure composite microwave absorbing material | |
| CN105153614A (en) | Method for manufacturing modified graphene oxide/PMMA (polymethyl methacrylate) composite materials | |
| CN113170785A (en) | Copper antibacterial composite material and preparation method thereof | |
| CN107840324A (en) | A kind of lightweight, Flexible graphene Quito member composite wave-absorbing film and preparation method thereof | |
| CN103506619B (en) | A kind of Fe 3o 4the silver-colored line that magnetic nanoparticle is coated and preparation and purposes | |
| WO2014069698A1 (en) | Oxidation resistant copper nanoparticles and method for producing same | |
| CN103224831A (en) | Electrorheological fluid and its preparation method | |
| CN105315964A (en) | Method for synthesizing ferriferrous oxide conductive polymer graphene ternary composite wave absorbing agent | |
| Liu et al. | Green synthesis of air-stable tellurium nanowires via biomolecule-assisted hydrothermal for thermoelectrics | |
| CN110724492B (en) | Ferroferric oxide/nano oxide hybrid wave-absorbing material and preparation method thereof | |
| CN105609305B (en) | A kind of Fe3O4The preparation method of/graphene composite film | |
| CN111040571A (en) | Heat dissipation coating and preparation method and application thereof | |
| KR20170124660A (en) | Electroconductive ink composite including metal-organic precursor and polyhydric alcohol capable of heating in the air and method for forming the metal line using the same | |
| CN115092914A (en) | Method for preparing graphene by reducing graphene oxide | |
| KR20120087454A (en) | Silver nanowire ink using liquid-crystalline polymer and preparation method thereof | |
| Bhattacharjee et al. | Surfactant-assisted low-temperature thermal decomposition route to spherical NiO nanoparticles | |
| Togashi et al. | N, N-Diethyl-diaminopropane-copper (ii) Oxalate Self-reducible Complex for the Solution-based Synthesis of Copper Nanocrystals |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210727 |
|
| RJ01 | Rejection of invention patent application after publication |