CN110026550A - A kind of nano zero-valence copper and preparation method and application - Google Patents
A kind of nano zero-valence copper and preparation method and application Download PDFInfo
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- CN110026550A CN110026550A CN201811318777.7A CN201811318777A CN110026550A CN 110026550 A CN110026550 A CN 110026550A CN 201811318777 A CN201811318777 A CN 201811318777A CN 110026550 A CN110026550 A CN 110026550A
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- nano zero
- valence copper
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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
- 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
- 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
- B22F1/0553—Complex form nanoparticles, e.g. prism, pyramid, octahedron
-
- 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
- B22F1/07—Metallic powder characterised by particles having a nanoscale microstructure
-
- 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
- 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
-
- 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 belongs to metal nanoparticle technical field, a kind of nano zero-valence copper and preparation method and application is provided.Preparation method includes: that dispersing agent is added into copper salt solution and quickly stirs, while reducing agent and tea extract is added；To be restored dose be added dropwise after continue stirring until not generating bubble until to get arrive nano zero-valence copper suspension；Black solid is obtained from the nano zero-valence copper suspension, is sufficiently washed through distilled water, ethyl alcohol, supernatant is toppled over after centrifugation, under vacuum-pumping conditions by the solid obtained after centrifugation, freeze-drying obtains nano zero-valence copper particle.The preparation method of nano zero-valence copper provided by the invention, select tea extract as antioxidant, the antioxygenic property for also substantially increasing nano zero-valence copper while nanoparticle high activity is kept, the recycling of discarded tealeaves is realized, increases the added value of tealeaves industry.
Description
Technical field
The present invention relates to metal nanoparticle technical fields, and in particular to a kind of nano zero-valence copper and preparation method thereof and answers
With.
Background technique
In recent years, with the raising of living standards of the people and rhythm of life, comfort of the people to textile, health
Property, safety and feature of environmental protection etc. require higher and higher.After-finishing of textile products, which has become, improves functions of textile fabrics and raising product is attached
One of the important channel of price markup value.Using capsule of nano technology make textile have functionality be future development hot spot it
One.Mainly in terms of final finishing, micro- glue can be made in various fabric post-finishing agents for application of the microcapsules technology in weaving
After capsule be used for fabric final finishing, such as depilation, gas defence, antifog, anti-pollution, wrinkle resistant, shrinkproof, deodorization, heat storing and heat preserving, softness, fragrance,
Fire-retardant, antibacterial, antiultraviolet etc..The overwhelming majority is applied on fiber or fabric in a manner of co-blended spinning or coating, but is blended
Spinning is more demanding to equipment and technology content, and there are no obtain large-scale production application.
Summary of the invention
For the defects in the prior art, the present invention provides a kind of preparation methods of nano zero-valence copper, effectively to prevent
The reunion of nano zero-valence copper improves the reactivity and inoxidizability of nano zero-valence copper.
The present invention also provides a kind of applications of nano zero-valence copper, can effectively remove peculiar smell and antibacterial.
In a first aspect, the present invention provides a kind of preparation methods of nano zero-valence copper, comprising: be added and divide into copper salt solution
Powder simultaneously quickly stirs, while reducing agent and tea extract is added；To be restored dose be added dropwise after continue stirring until do not produce
Anger bubble until to get arrive nano zero-valence copper suspension；Black solid is obtained from the nano zero-valence copper suspension, through distilling
Water, ethyl alcohol sufficiently wash, and supernatant is toppled over after centrifugation, and under vacuum-pumping conditions by the solid obtained after centrifugation, freeze-drying obtains
Obtain nano zero-valence copper particle.
Optionally, the tea extract is prepared using following steps: tealeaves being dried, by being added in every 100ml water
Tea leaf solution is made in 0.05-2.5g tealeaves, in 60-100 DEG C of heating 0.5-3h, filters off tea waste residue and obtains the tealeaves extraction
Liquid.
Optionally, the dispersing agent is the mixture that polyvinylpyrrolidone and beta-cyclodextrin are formed, wherein the poly- second
Mass fraction shared by alkene pyrrolidone is 10-90%.
Optionally, the mass ratio of the dispersing agent and the mantoquita is 0.1-1:1.
Optionally, the copper salt solution includes CuCl2Or CuSO4；Cu in the copper salt solution2+Concentration be 0.005-
0.050mol/L。
Optionally, the reducing agent be hydrazine hydrate, sodium borohydride, potassium borohydride or sodium hypophosphite, the mantoquita with also
The molar ratio of former agent is 1:2-4.
Optionally, the mass ratio of the tea extract and mantoquita is 0.05-1:100.
Optionally, tealeaves includes any one of green tea, white tea, black tea.
Second aspect, the present invention also provides a kind of nano zero-valence copper, are prepared using the preparation method.
The third aspect, the present invention also provides a kind of applications of nano zero-valence copper, and the nano zero-valence copper is applied to
Textile fabric remove odors and antibacterial.
As shown from the above technical solution, the preparation method of nano zero-valence copper provided by the invention selects tea extract to make
For antioxidant, the antioxygenic property for also substantially increasing nano zero-valence copper while nanoparticle high activity is kept, is realized
The recycling of discarded tealeaves, increases the added value of tealeaves industry.
Nano zero-valence copper prepared by the present invention is can absorb various due to its distinctive pore fungus cloud structure strong adsorption
Peculiar smell, while there is very strong antibacterial effect, it is inorganic it is organic it is netted meet connection chemical bond, therefore, can accomplish to adsorb various
Peculiar smell, spectrum sterilization, quick sterilization, long-acting lasting sterilization.
Specific embodiment
The embodiment of technical solution of the present invention will be described in detail below.Following embodiment is only used for clearer
Ground illustrates technical solution of the present invention, therefore is only used as example, and not intended to limit the protection scope of the present invention.
It should be noted that unless otherwise indicated, technical term or scientific term used in this application should be this hair
The ordinary meaning that bright one of ordinary skill in the art are understood.
First embodiment of the invention provides a kind of preparation method of nano zero-valence copper.
Firstly, carrying out the preparation of tea extract, common tealeaves can be selected, last progress tealeaves can also be selected
The tealeaf residue of extracting solution preparation, that is to say, that tealeaves not using once, can be used for multiple times, avoid wasting.Tealeaves mentions
It takes liquid to prepare using following steps: tealeaves is dried, tea leaf solution is made by 0.05-2.5g tealeaves is added in every 100ml water, in
60-100 DEG C of heating 0.5-3h filters off tea waste residue and obtains the tea extract.
Then, nano zero-valence copper is prepared.The original material of selection can be CuCl2Or CuSO4。
Specific steps are as follows: dispersing agent is added into copper salt solution and quickly stirs, while reducing agent and tea is added
Leaf extract, to be restored dose be added dropwise after continue stirring until not generating bubble until to get arrive nano zero-valence copper suspension；
Black solid is obtained from the nano zero-valence copper suspension, is sufficiently washed through distilled water, ethyl alcohol, supernatant is toppled over after centrifugation,
Under vacuum-pumping conditions by the solid obtained after centrifugation, it is freeze-dried, obtains nano zero-valence copper particle, be sealed molten with ethyl alcohol
In liquid.
Specifically a bit, Cu in copper salt solution2+Concentration be 0.005-0.050mol/L.
Specifically a bit, the dispersing agent is the mixture that polyvinylpyrrolidone and beta-cyclodextrin are formed, wherein described poly-
Mass fraction shared by vinylpyrrolidone is 10-90%.The mass ratio of the dispersing agent and the mantoquita is 0.1-1:1.
Polyvinylpyrrolidone (polyvinyl pyrrolidone) abbreviation PVP is a kind of non-ionic macromolecule chemical combination
Object is most characteristic in N vinylamide polymer, and is studied most deep, extensive fine chemicals kind.Poly- second
Alkene pyrrolidone is the powder that there is hydrophily easily to flow white or substantial white, is had micro- smelly.PVP is as a kind of synthesizing water-solubility
High-molecular compound, the general aspects with water-soluble high-molecular compound, colloid protective effect, film forming, caking property, moisture absorption
Property, solubilising or cohesion, but its is most characteristic, thus is its excellent solubility property and PHYSIOLOGICALLY COMPATIBLE by people's attention
Property.
Beta-cyclodextrin also known as beta cyclodextrin, cyclohexose, Ring Maltose, white crystals, are easier to tie in water
It is brilliant.The solubility of beta-cyclodextrin in water is relatively low, is at room temperature 1.85%, increases as temperature increases solubility.Do not have
There is a hygroscopicity, but stable hydrate easy to form.Hydration levels between relative humidity 50-70%, are equivalent to every point
Sub- β-CD absorbs 10-11 hydrone (water content is in 13.7-14.8%), and moisture absorption isothermal curve is two phases.Insoluble in general
Organic solvent, but being capable of slightly soluble in pyridine, dimethylformamide, dimethyl sulfoxide and ethylene glycol.
The nano zero-valence copper activity that the present invention is prepared using polyvinylpyrrolidone and beta-cyclodextrin as mixed dispersant
Height, treatment effeciency is high, and it is good to reuse effect.
Specifically a bit, the reducing agent is hydrazine hydrate (N2H4·H2O), sodium borohydride, potassium borohydride or sodium hypophosphite,
The molar ratio of the mantoquita and reducing agent is 1:2-4.
Hydrazine hydrate is also known as hydrazine hydrate.Sterling is colorless and transparent oily liquids, has light ammonia taste, smolders in humid air,
With strong basicity and hygroscopicity.Under normal pressure, hydrazine can form azeotropic with water (hydrazine content is about 69% in azeotropic mixture).Industrial one
As using content be 40%--80% hydrazine hydrate aqueous solution or hydrazine salt.Hydrazine hydrate liquid exists with dimer form, with water
It is miscible with ethyl alcohol, do not dissolve in ether and chloroform；Its energy attack glass, rubber, leather, cork etc., resolve into N at high temperature2、NH3
And H2；Hydrazine hydrate reduction is extremely strong, with halogen, HNO3、KMnO4Equal intense reactions, can absorb CO in air2, generate smog.
Stablize under sodium borohydride normal temperature and pressure.Sodium borohydride alkaline solution is in brown color.One of most common reducing agent.It is right
Aqueous vapor and oxygen in air is more stable, and operation processing is easy.Suitable for commercial scale, because deliquescent problem, usually used
Methanol, ethyl alcohol are as solvent.Under normal conditions, sodium borohydride can not ester reduction, amide, carboxylic acid and nitrile compounds, but work as ester
Carbonyl α have and make an exception in the presence of hetero atom, ester can be restored.
Potassium borohydride is fluffy white powder or crystal.It is stable in the air, non-hygroscopic.Potassium borohydride is soluble easily in water,
It is dissolved in liquefied ammonia, is slightly soluble in methanol and ethyl alcohol, is practically insoluble in ether, benzene, tetrahydrofuran, methyl ether and other hydrocarbons.?
Stablize in alkaline environment, meets inorganic acid and decompose and release hydrogen.With strong reducing property.
Sodium hypophosphite is strong reductant, the salt of gold, silver, mercury, copper, chromium, cobalt etc. can be reduced into metallic state.In normal pressure
Under, heating evaporation sodium hypophosphite solution can explode, therefore evaporation should carry out under reduced pressure.
Specifically a bit, the mass ratio of the tealeaves and mantoquita is 0.05-1:100.Tealeaves described herein is to produce tealeaves to mention
The tealeaves used when taking object, and whole tea extracts are all added in copper salt solution.
Specifically a bit, tealeaves includes any one of green tea, white tea, black tea.
Tea polyphenols (Tea Polyphenols) are the general name of Polyphenols of Tea, including flavanol compound, anthocyanin
Class, flavonoids, flavonols and phenolic acid class etc..Predominantly flavanols (catechin) class, catechin account for 60~80%.Tea polyphenols tool
There are stronger antioxidation, especially ester catechin EGCG, reproducibility is even up to 100 times of the different bad hematic acid of L-.4 kinds of masters
Want in catechin compounds, oxidation resistance EGCG > EGC > ECG > EC > BHA, and antioxygenic property with the raising of temperature and
Enhancing.Polyphenol content in all kinds of tealeaves is substantially presented below as rule: green tea > white tea > black tea.
The preparation method of nano zero-valence copper provided by the invention selects tea extract as antioxidant, keeps nanometer
The antioxygenic property that nano zero-valence copper is also substantially increased while particle high activity realizes the recycling of discarded tealeaves, increases
The added value of tealeaves industry is added.
The above-mentioned preparation method for preparing nano zero-valence copper is applied in following multiple embodiments, see Table 1 for details for design parameter.
Table 1
Second embodiment of the invention provides a kind of nano zero-valence copper, is prepared using the preparation method.
Prepared nano zero-valence copper favorable dispersibility of the invention, crystal form are perfect.
Third embodiment of the invention additionally provides a kind of application of nano zero-valence copper, and the nano zero-valence copper is applied to
Textile fabric remove odors and antibacterial.
Nano zero-valence copper prepared by the present invention is can absorb various due to its distinctive pore fungus cloud structure strong adsorption
Peculiar smell, while there is very strong antibacterial effect, it is inorganic it is organic it is netted meet connection chemical bond, therefore, can accomplish to adsorb various
Peculiar smell, spectrum sterilization, quick sterilization, long-acting lasting sterilization.
Preparation method provided by the invention can effectively prevent the reunion of nano zero-valence copper, improve the reaction of nano zero-valence copper
Activity and inoxidizability, and can effectively remove textile remove odors and antibacterial.
In specification of the invention, numerous specific details are set forth.It is to be appreciated, however, that the embodiment of the present invention can be with
It practices without these specific details.In some instances, well known method, structure and skill is not been shown in detail
Art, so as not to obscure the understanding of this specification.
In the description of this specification, reference term " one embodiment ", " some embodiments ", " example ", " specifically show
The description of example " or " some examples " etc. means specific features, structure, material or spy described in conjunction with this embodiment or example
Point is included at least one embodiment or example of the invention.In the present specification, schematic expression of the above terms are not
It must be directed to identical embodiment or example.Moreover, particular features, structures, materials, or characteristics described can be in office
It can be combined in any suitable manner in one or more embodiment or examples.In addition, without conflicting with each other, the skill of this field
Art personnel can tie the feature of different embodiments or examples described in this specification and different embodiments or examples
It closes and combines.
Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention., rather than its limitations；To the greatest extent
Pipe present invention has been described in detail with reference to the aforementioned embodiments, those skilled in the art should understand that: its according to
So be possible to modify the technical solutions described in the foregoing embodiments, or to some or all of the technical features into
Row equivalent replacement；And these are modified or replaceed, various embodiments of the present invention technology that it does not separate the essence of the corresponding technical solution
The range of scheme should all cover within the scope of the claims and the description of the invention.
Claims (10)
1. a kind of preparation method of nano zero-valence copper, comprising: dispersing agent is added into copper salt solution and quickly stirs, is added simultaneously
Reducing agent and tea extract；To be restored dose be added dropwise after continue stirring until not generating bubble until to get arrive nanometer zero
Valence copper suspension；Black solid is obtained from the nano zero-valence copper suspension, is sufficiently washed through distilled water, ethyl alcohol, after centrifugation
Topple over supernatant, under vacuum-pumping conditions by the solid obtained after centrifugation, freeze-drying obtains nano zero-valence copper particle.
2. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the tea extract is using such as
Lower step preparation: tealeaves is dried, and tea leaf solution is made by 0.05-2.5g tealeaves is added in every 100ml water, adds in 60-100 DEG C
Hot 0.5-3h filters off tea waste residue and obtains the tea extract.
3. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the dispersing agent is polyethylene pyrrole
The mixture that pyrrolidone and beta-cyclodextrin are formed, wherein mass fraction shared by the polyvinylpyrrolidone is 10-90%.
4. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the dispersing agent and the mantoquita
Mass ratio be 0.1-1:1.
5. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the copper salt solution includes CuCl2
Or CuSO4；Cu in the copper salt solution2+Concentration be 0.005-0.050mol/L.
6. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the reducing agent be hydrazine hydrate,
The molar ratio of sodium borohydride, potassium borohydride or sodium hypophosphite, the mantoquita and reducing agent is 1:2-4.
7. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that the tealeaves and the mantoquita
Mass ratio is 0.05-1:100.
8. the preparation method of nano zero-valence copper according to claim 1, which is characterized in that tealeaves includes green tea, white tea, red
Any one of tea.
9. a kind of nano zero-valence copper, is prepared using preparation method of any of claims 1-8.
10. nano zero-valence copper as claimed in claim 9 is applied to removing odors for textile by a kind of application of nano zero-valence copper
And antibacterial.
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