CN112091230A - Nano copper particles and preparation method thereof - Google Patents
Nano copper particles and preparation method thereof Download PDFInfo
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- CN112091230A CN112091230A CN201910526327.5A CN201910526327A CN112091230A CN 112091230 A CN112091230 A CN 112091230A CN 201910526327 A CN201910526327 A CN 201910526327A CN 112091230 A CN112091230 A CN 112091230A
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- 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
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- 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
Abstract
The invention discloses a nano-copper particle, which is prepared by a supercritical hydrothermal method, is in a spherical nano-cluster shape, and has an average particle size of 100nm-200 nm. The nano copper particles are spherical nano cluster type, have good antibacterial effect, can be used for products such as yarns, fabrics, coatings, heat-insulating window films and the like, are widely applied to the fields of textile products, internal and external wall coatings, automotive interiors, antibacterial and deodorant materials and the like, and have huge environmental protection advantages and wide market prospects. In addition, the invention also discloses a preparation method of the nano-copper particles.
Description
Technical Field
The present invention relates to a nano-copper particle, and further, to a method for producing the nano-copper particle.
Background
Nanotechnology is a new technology for studying the law and characteristics of intramolecular movement. Atoms or molecules at the nanometer scale can exhibit many new properties, and a technology for manufacturing materials having specific functions using these properties is called nanotechnology. The nano material refers to a material with the size of a structural unit ranging from 1nm to 200 nm. The properties vary greatly as their size is already close to the coherence length of the electrons. And since its dimensions are close to the wavelength of light, plus surface effects, its properties, such as melting point, magnetic, optical, thermal, electrical conductivity, etc., tend to be different from the properties that the substance exhibits in its bulk state.
The metal silver and copper has broad-spectrum antibacterial property, good heat resistance, good dispersibility, small drug resistance and the likeExcellent performance and can be applied to various biological materials and medical appliances. The metal silver river copper has two sterilization mechanisms, namely 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 to penetrate through the cell walls, so that the cell walls are broken, cytoplasm flows outwards, and bacteria die. 2) The metal ions can be used as catalytic active centers 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 biomaterial of copper.
Chinese patent CN104186499A discloses a preparation method of a thiediazole copper bactericide, and the bactericide prepared by the method is a composition with high cost and general antibacterial effect; chinese patent CN105475375A discloses a method for preparing an antibacterial agent containing copper and calcium sulfate, the antibacterial agent prepared by the method is a composition, the process is complex, and the antibacterial effect is not ideal; chinese patent CN105815325A discloses a preparation method of an organic copper antibacterial agent, the antibacterial agent prepared by the method is an antibacterial composition, the antibacterial effect is general and has certain influence on the environment.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, it is desirable to provide a nano-copper particle having a spherical nanocluster type, a large surface area, a strong adsorption effect, and a strong sterilization effect according to an embodiment of the present invention. In addition, the invention also aims to provide a preparation method of the nano copper particles.
According to the embodiment, the nano copper particles are prepared by a supercritical hydrothermal method, are spherical nanocluster-shaped, and have the particle size of 100nm-200 nm.
According to an embodiment, the preparation method of the nano-copper particles provided by the invention comprises the following steps:
step one, dissolving copper salt and alkali in water, and uniformly stirring in a supercritical reaction kettle;
step two, heating the reaction kettle to 80-100 ℃, adding a solvent, and uniformly stirring;
step three, continuing to heat to 150-;
and step four, after the reaction is finished, filtering out a reaction product after the reaction device is cooled to room temperature, 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 80-100 ℃ for 12-20 hours to prepare the nano copper particles with the shapes of spherical nano clusters and the particle sizes of 100nm-200 nm.
Preferably, in the step one, the copper salt is copper nitrate, copper sulfate or copper chloride; the alkali is sodium hydroxide or potassium hydroxide.
Preferably, in the second step, the solvent is n-butane, n-pentane or n-hexane.
Preferably, in the third step, the reducing agent is pentaerythritol, neopentyl glycol or butanediol.
Compared with the prior art, the following embodiments and test examples prove that the nano copper particles have good antibacterial effect, can be widely applied to the fields of textile products, interior and exterior wall coatings, automotive interiors, antibacterial and deodorant materials and the like, and have huge environmental protection advantages and wide market prospects. The invention also has the advantages of simple preparation method, low cost, easy industrialization and the like.
Drawings
Fig. 1 is a diagram of spherical nanoclusters of the nano-copper particles of the present invention.
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 6.3g of blue vitriod and 4g of sodium hydroxide in 80ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 80 ℃, adding 80ml of n-butane solution, and uniformly mixing;
(3) heating the reaction kettle to 170 ℃, adding 1g of butanediol, increasing the pressure in the reaction kettle to 5MPa, and reacting for 10 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 the nano copper particles, wherein the nano copper particles are shown in figure 1 and are in spherical nano cluster shapes, and the average particle size of the nano copper particles is 100nm-200 nm.
Example 2
(1) Dissolving 6.1g of copper nitrate trihydrate and 5.6g of potassium hydroxide in 90ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 90 ℃, adding 90ml of n-pentane solution, and uniformly mixing;
(3) heating the reaction kettle to 200 ℃, adding 1.2g of neopentyl glycol, increasing the pressure in the reaction kettle to 8MPa, 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 for 14 hours at the temperature of 90 ℃ to obtain the nano copper particles, wherein the nano copper particles are spherical nano cluster type, and the average particle size of the nano copper particles is 100nm-200 nm.
Example 3
(1) Dissolving 4.2g of copper chloride dihydrate and 4g of sodium hydroxide in 80ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 100 ℃, adding 100ml of n-hexane solution, and uniformly mixing;
(3) heating the reaction kettle to 250 ℃, adding 1.4g of pentaerythritol, increasing the pressure in the reaction kettle to 9MPa, and reacting for 12 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 for 16 hours at the temperature of 100 ℃ to obtain the nano copper particles, wherein the nano copper particles are spherical nano cluster type, and the average particle size of the nano copper particles is 100nm-200 nm.
Example 4
(1) Dissolving 6.3g of blue vitriod and 5.6g of potassium hydroxide in 100ml of deionized water in a supercritical reaction kettle, and uniformly stirring;
(2) heating the reaction kettle to 80 ℃, adding 100ml of n-butane solution, and uniformly mixing;
(3) heating the reaction kettle to 185 ℃, adding 1.3g of neopentyl glycol, increasing the pressure in the reaction kettle to 10MPa, 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 drying the reaction product in vacuum for 16 hours at the temperature of 100 ℃ to obtain the nano copper particles, wherein the nano copper particles are spherical nano cluster type, and the average particle size of the nano copper particles is 100nm-200 nm.
Test examples
0.40g of the nano-copper particles prepared in examples 1 to 4 were weighed respectively, added to 100ml of water, and subjected to ultrasonic oscillation to be uniform, so as to prepare 4.0g/L of nano-copper colloid. The effect against candida albicans (ATCC10231) was tested according to AATCC 100-.
As can be seen from table 1, the nano-copper particles prepared in examples 1 to 4 have a spherical structure, a large surface area, and a high antibacterial effect, and can adsorb more bacteria; the average killing rate of the candida albicans after 15 minutes is more than 97 percent.
TABLE 1 average kill rate of Candida albicans after 15 minutes for examples 1-4
| Candida albicans% | |
| Example 1 | 97.9 |
| Example 2 | 98.2 |
| Example 3 | 98.4 |
| Example 4 | 97.6 |
Claims (5)
1. The nano copper particles are prepared by a supercritical hydrothermal method, and are characterized in that the nano copper particles are spherical nano cluster-shaped, and the particle size is 100nm-200 nm.
2. A preparation method of nano-copper particles is characterized by comprising the following steps:
step one, dissolving copper salt and alkali in water, and uniformly stirring in a supercritical reaction kettle;
step two, heating the reaction kettle to 80-100 ℃, adding a solvent, and uniformly stirring;
step three, continuing to heat to 150-;
and step four, after the reaction is finished, filtering out a reaction product after the reaction device is cooled to room temperature, 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 80-100 ℃ for 12-20 hours to prepare the nano copper particles with the shapes of spherical nano clusters and the particle sizes of 100nm-200 nm.
3. The method for preparing nano-copper particles as claimed in claim 1, wherein in the first step, the copper salt is copper nitrate, copper sulfate or copper chloride; the alkali is sodium hydroxide or potassium hydroxide.
4. The method for preparing nano-copper particles as recited in claim 1, wherein in the second step, the solvent is n-butane, n-pentane or n-hexane.
5. The method for preparing nano-copper particles as recited in claim 1, wherein in step three, the reducing agent is pentaerythritol, neopentyl glycol or butanediol.
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Citations (7)
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| CN102553594A (en) * | 2010-12-21 | 2012-07-11 | 冯刚 | Preparation method for metallic nano cluster catalyst |
| CN103143720A (en) * | 2013-03-12 | 2013-06-12 | 沈阳化工大学 | Preparation method of superfine copper powder |
| CN103496744A (en) * | 2013-10-19 | 2014-01-08 | 哈尔滨工业大学 | Preparation method of as-reduced ammonium tungsten bronze nanoparticles |
| CN103934468A (en) * | 2014-04-02 | 2014-07-23 | 西安交通大学 | Supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles |
| CN103949653A (en) * | 2014-04-02 | 2014-07-30 | 西安交通大学 | Product separation and organic ligand recovery system of supercritical hydro-thermal synthesis system |
| CN107127354A (en) * | 2017-06-29 | 2017-09-05 | 吉林大学 | A kind of synthesis of hydro-thermal method by light sensitivity electrum nano-cluster of the small molecule AMP for protection part |
| CN108907221A (en) * | 2018-06-10 | 2018-11-30 | 江苏经贸职业技术学院 | A kind of synthetic method of copper nano-cluster |
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2019
- 2019-06-18 CN CN201910526327.5A patent/CN112091230A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102553594A (en) * | 2010-12-21 | 2012-07-11 | 冯刚 | Preparation method for metallic nano cluster catalyst |
| CN103143720A (en) * | 2013-03-12 | 2013-06-12 | 沈阳化工大学 | Preparation method of superfine copper powder |
| CN103496744A (en) * | 2013-10-19 | 2014-01-08 | 哈尔滨工业大学 | Preparation method of as-reduced ammonium tungsten bronze nanoparticles |
| CN103934468A (en) * | 2014-04-02 | 2014-07-23 | 西安交通大学 | Supercritical hydrothermal synthesis method of nano metal or nano metal oxide particles |
| CN103949653A (en) * | 2014-04-02 | 2014-07-30 | 西安交通大学 | Product separation and organic ligand recovery system of supercritical hydro-thermal synthesis system |
| CN107127354A (en) * | 2017-06-29 | 2017-09-05 | 吉林大学 | A kind of synthesis of hydro-thermal method by light sensitivity electrum nano-cluster of the small molecule AMP for protection part |
| CN108907221A (en) * | 2018-06-10 | 2018-11-30 | 江苏经贸职业技术学院 | A kind of synthetic method of copper nano-cluster |
Non-Patent Citations (2)
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| 关清卿: "《亚/超临界水技术与原理》", 31 December 2014, 冶金工业出版社 * |
| 胡长伟: "《纳米材料的生态毒性效应与环境释放风险》", 28 February 2015, 山东人民出版社 * |
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Application publication date: 20201218 |