CN104477968A - Method for preparing cuprous oxide nanometer wire by utilizing plant phenolic acid - Google Patents
Method for preparing cuprous oxide nanometer wire by utilizing plant phenolic acid Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/02—Oxides; Hydroxides
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
Aiming at the shortcomings of an existing technology for preparing a cuprous oxide nanometer wire, the invention discloses a method for preparing the cuprous oxide nanometer wire by utilizing plant phenolic acid and belongs to the field of a nanometer material and a novel material. The method comprises the following steps: heating a plant phenolic acid solution to the temperature of 50 to 95 DEG C under an alkaline condition by taking natural plant phenolic acids including protocatechuic acid, gallic acid and ellagic acid as a reducing agent; dropwise adding inorganic salt solutions of copper sulfate, copper chloride, cupric nitrate and copper acetate into the plant phenolic acid solution, reacting for 0.5-5 hours and directly precipitating to obtain a cuprous oxide nanometer wire material. The method is environmental friendly, simple in technological process, capable of directly finishing the technological process by one step in an alkaline solution, free of toxin or low in toxicity in raw materials, low in cost, pure in product and suitable for large-scale production.
Description
Technical field
The invention belongs to nano material and field of new, particularly a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire.
Background technology
One-dimensional nano structure material, owing to having special optical, electrical, magnetic and mechanical property, more and more causes the concern of every field.At semiconductor materials and devices manufacture view, the applicating and exploitation of one-dimensional nano line and micro/nano level device becomes a kind of development trend gradually.Therefore, the preparation of industrialization of low dimension semiconductor compound nano line becomes more and more important.
Red copper oxide (Cu
2o) be a kind of p-type semiconductor material of intrinsic, energy gap is 2.1eV, and this band gap determines all kinds of device such as photoelectricity, photochemical energy conversion that Red copper oxide is extremely suitable for sun power, such as solar cell material, water-splitting, photochemical catalysis etc.1-dimention nano wire Red copper oxide has the feature such as high surface energy, large length-to-diameter ratio, and high surface area can high-density absorb photons, has higher assimilated efficiency than the bulk material of identical component, so be conducive to the efficiency improving photovoltaic cell.In addition, nano cuprous oxide wire shows more and more crucial effect in sensor, catalysis, water photodissociation hydrogen manufacturing, lithium ion battery, the fields such as malicious sterilizing of going out.
At present, the method adopting a step, directly synthesis to prepare nano cuprous oxide wire concentrates on wet-chemical technique.Having of having reported uses porous cathode aluminum oxide as template, grows the method (Shin H S, 2009Mater.Lett.63,397) of nano cuprous oxide wire in the solution.In addition, there is use Surfactant CTAB (hexadecyl trimethyl ammonium bromide) as growth shape diverting agent, then be that reductive agent directly synthesizes nano cuprous oxide wire (Cao M H, Chemical Comm with hydrazine hydrate, 2003,1884-1885; YU Y, Du F P, Journal ofsolid state chemistry, 2004,177,4640); Or use polymer molecule PEG (wang W Z, et al.2002, adv.mater, 14,67) to produce nano cuprous oxide wire.The nano cuprous oxide wire that a step directly manufactures above all belongs to polycrystalline structure.Chinese invention patent (application number: 201410018809.7 and 201410831465.3) disclose one and utilize cuprous thiocyanate for presoma, use or do not use ultrasonic wave in the liquid phase chemical reaction prepare the method for nano cuprous oxide wire.This method equally directly obtains nano cuprous oxide wire, but the composition of chemical reaction product mutually in also have a small amount of unreacted mantoquita.
Commercial applications require nano cuprous oxide wire manufacture can quick, controlled, can repeatedly scale operation.At present, still there is lot of challenges in the high-quality nano cuprous oxide wire of manufacture in enormous quantities, the existing technology ubiquity raw materials cost preparing nano cuprous oxide wire is high, toxicity large, and the synthesis and preparation process time is long, temperature is high, and the limitation such as nano cuprous oxide wire composition is mutually impure.
Plant phenolic acid is the aromatics that a class has carboxyl and hydroxyl, at present the phenolic acid compound of extracting and developing, qualification existing thousands of kinds from plant.Protocatechuic Acid or title PCA, structural formula is as follows:
Gallic acid or title Gallic Acid, structural formula is as follows:
Ellagic acid or title two contracting two (trihydroxybenzoic acid), structural formula is as follows:
They are the three kinds of Polyphenols organic acids extensively existing in plant, be easy to get.
Summary of the invention
The object of the invention is the deficiency for preparing nano cuprous oxide wire technology at present, proposing a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire.Its method is, utilizes the natural phant phenolic acid not polluting physical environment as reductive agent, in the basic conditions from containing Cu
2+in the inorganic salt solution of ion, a step, Direct precipitation prepare nano cuprous oxide wire.The method environmental protection, technological process is simple, and in basic solution, a step directly completes, and raw material does not have toxicity or hypotoxicity, and cost is low, products pure, and applicable scale operation.
Utilize plant phenolic acid to prepare a method for nano cuprous oxide wire, comprise the following steps:
1, dissolve appropriate plant phenolic acid in deionized water, with highly basic, the pH value of solution is adjusted to 7≤pH≤12, good pH value is 9≤pH≤11; Then solution being heated to 50 ~ 95 DEG C, is 60 ~ 90 DEG C preferably, and stirs 0.5 ~ 3 hour with the speed of 100 ~ 200rpm, is 1-2 hour preferably, obtains plant phenols acid solution;
Wherein, described plant phenolic acid is one or several the mixture in Protocatechuic Acid, gallic acid, ellagic acid;
Described highly basic is NaOH or the KOH aqueous solution or other similar strong base solutions of concentration 2 ~ 3mol/L;
2, will containing 0.05 ~ 0.5mol/LCu
2+the Inorganic Copper salts solution of ion joins in plant phenols acid solution according to the speed of 5-10mL/min, controlling plant phenols acid solution pH value in dropping process is 7≤pH≤12, be 9≤pH≤11 preferably, continue with 50 ~ 95 DEG C after mixing, be 60 ~ 90 DEG C preferably, the stirring velocity reaction 0.5-5 hour of 100 ~ 200rpm; After reaction terminates, by reaction soln cool to room temperature, isolate precipitation, good separate mode is the centrifugation with 4000 ~ 8000rpm, after precipitate with deionized water and washing with alcohol, then through 60-80 DEG C of vacuum-drying, obtain Red copper oxide nanometer monocrystalline wire material; The reaction times of this reaction and temperature can affect the size of nano cuprous oxide wire, by improving temperature of reaction or extending diameter and the length that the reaction times can improve nano cuprous oxide wire;
Wherein, described Cu
2+ion/plant phenolic acid mol ratio is (1:2) ~ (20:1), preferably (1:1) ~ (10:1);
Described inorganic mantoquita is the mixture of one or more in copper sulfate, cupric chloride, cupric nitrate, neutralized verdigris.
The present invention compared with prior art, it is advantageous that:
1, raw material of the present invention is easy to get.Protocatechuic Acid, gallic acid, ellagic acid are the three kinds of Polyphenols organic acids extensively existing in plant, be easy to get.
2, the present invention uses plant phenolic acid as reactant, directly can generate Red copper oxide.Feature due to plant phenols acid compounds molecular structure there is carboxyl and multiple phenolic hydroxyl group.In basic solution environment and when other preparation conditions are identical, if cupric oxide compound can only be produced when not using plant phenolic acid, i.e. cupric oxide (CuO); Bivalent cupric ion can be reduced to univalent copper ion and produce Red copper oxide (Cu after adding plant phenolic acid
2o).
3, present method directly can obtain nano cuprous oxide wire, without the need to additional step.
4, present method environmental protection, technological process is simple, and in basic solution, a step directly completes, and raw material does not have toxicity or hypotoxicity, and cost is low, products pure, and applicable scale operation.
Accompanying drawing explanation
The XRD figure of the nano cuprous oxide wire that Fig. 1, embodiment 1 are obtained.
The SEM figure of the nano cuprous oxide wire that Fig. 2, embodiment 1 are obtained.
The TEM figure of the nano cuprous oxide wire that Fig. 3, embodiment 2 are obtained.
The electron-diffraction diagram of the nano cuprous oxide wire that Fig. 4, embodiment 2 are obtained.
Embodiment
Raw material in following examples and reagent are commercial.
Embodiment 1
Take 4.62g Protocatechuic Acid (molecular weight=154.12), add 1000mL deionized water, after dissolving, utilize the pH=11 of the NaOH aqueous solution regulator solution of concentration 2mol/L, solution be heated to 75 DEG C and keep this temperature to stir 60 minutes with the speed of 100 ~ 200rpm; Again the copper sulfate solution 600mL of 0.05mol/L is joined in the Protocatechuic Acid aqueous solution with the speed of 10mL/min, and keep pH=11 constant; After mixing, solution continues to keep reacting 60 minutes with the stirring velocity of the temperature of 75 DEG C, 100 ~ 200rpm, then isolates solid deposits with the centrifugation of 4000 ~ 5000rpm; After settling deionized water and washing with alcohol, 60 DEG C of vacuum-drying 24 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 55 ~ 67 nanometers, and length is about 5.5 ~ 6.2 microns.
Fig. 1 and Fig. 2 is XRD figure and the SEM figure of nano cuprous oxide wire prepared by present method.
Embodiment 2
Take 2.55g gallic acid (molecular weight=170.12), add 800mL deionized water, after dissolving, utilize the pH=10 of the KOH aqueous solution regulator solution of 2mol/L, heated solution is to 85 DEG C and keep this temperature to stir 2 hours with the speed of 100 ~ 200rpm; Then the Cupric Chloride Solution 400mL of concentration 0.5mol/L is joined in the gallic acid aqueous solution with the speed of 5mL/min, and keep pH=10 constant; After mixing, solution continues to keep reacting 2 hours with the stirring velocity of the temperature of 85 DEG C, 100 ~ 200rpm, then isolates solid deposits with the centrifugation of 7000 ~ 8000rpm; After settling deionized water and washing with alcohol, 80 DEG C of vacuum-drying 36 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 93 ~ 97 nanometers, and length is about 12.9 ~ 14.6 microns.
Fig. 3 and Fig. 4 is TEM image and the image K-M of nano cuprous oxide wire prepared by present method.
Embodiment 3
Take 8.51g gallic acid, add 1000mL deionized water, after dissolving, utilize the KOH aqueous solution regulator solution pH=7 of 3mol/L, heated solution is to 60 DEG C and keep temperature to stir 30 minutes with the speed of 100 ~ 200rpm; Then the copper nitrate solution 1000mL of 0.2mol/L is joined in the gallic acid aqueous solution with the speed of 8mL/min, and keep pH=7 constant; After mixing, solution continues to keep reacting 30 minutes with the stirring velocity of the temperature of 60 DEG C, 100 ~ 200rpm, filters, and after precipitate with deionized water and washing with alcohol, 70 DEG C of vacuum-drying 24 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 72 ~ 77 nanometers, and length is about 11.7 ~ 13 microns.
Embodiment 4
Take 9.98g ellagic acid (molecular weight=302.28), add 800mL deionized water, after dissolving, utilize the NaOH aqueous solution of 3mol/L to regulate pH=11, heated solution is to 90 DEG C and keep temperature to stir 2 hours with the speed of 100 ~ 200rpm; Then the neutralized verdigris solution 600mL of 0.5mol/L is joined in the ellagic acid aqueous solution with the speed of 6mL/min, and keep pH=11 constant; After mixing, solution continues to keep reacting 5 hours with the stirring velocity of the temperature of 90 DEG C, 100 ~ 200rpm, then with the centrifugation of 6000 ~ 7000rpm, settling deionized water and washing with alcohol, 80 DEG C of vacuum-drying 24 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 96 ~ 103 nanometers, and length is about 9.7 ~ 10.4 microns.
Embodiment 5
Take 3.08g Protocatechuic Acid and 5.1g gallic acid, add 400mL deionized water, after dissolving, utilize the NaOH aqueous solution of 2.5moL/L to regulate pH=12, heated solution is to 50 DEG C and keep temperature to stir 2 hours with the speed of 100 ~ 200rpm; Then the copper nitrate aqueous solution 150mL of copper sulfate solution 100mL and 0.1mol/L of 0.1mol/L is joined in plant phenols aqueous acid respectively with the speed of 5mL/min, and keep pH=12 constant; After mixing, solution continues to keep reacting 1.5 hours with the stirring velocity of the temperature of 50 DEG C, 100 ~ 200rpm, and then filter, precipitate with deionized water and washing with alcohol, 60 DEG C of vacuum-drying 24 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 47 ~ 55 nanometers, and length is about 4.8 ~ 5.6 microns.
Embodiment 6
Take 1.54g Protocatechuic Acid and 3.02g ellagic acid, add 300mL deionized water, after dissolving, utilize the NaOH aqueous solution of 2.5mol/L to regulate pH=10, heated solution is to 95 DEG C and keep temperature to stir 3 hours with the speed of 100 ~ 200rpm; Then the Cupric Chloride Solution 400mL of neutralized verdigris solution 400mL and 0.5mol/L of 0.5mol/L is joined in plant phenols aqueous acid respectively with the speed of 8mL/min, and keep pH=10 constant; After mixing, solution continues to keep reacting 4 hours with the stirring velocity of the temperature of 95 DEG C, 100 ~ 200rpm, then with the centrifugation of 6000 ~ 7000rpm, settling deionized water and washing with alcohol, 80 DEG C of vacuum-drying 40 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 94 ~ 106 nanometers, and length is about 4.8 ~ 5.0 microns.
Embodiment 7
Take 3.4g gallic acid and 3.02g ellagic acid, add 1000mL deionized water, after dissolving, utilize the NaOH aqueous solution of 2mol/L to regulate pH=9, heated solution is to 90 DEG C and keep temperature to stir 1 hour with the speed of 100 ~ 200rpm; Then the Cupric Chloride Solution 250mL of copper-bath 250mL and 0.3mol/L of 0.3mol/L is joined in plant phenols aqueous acid respectively with the speed of 10mL/min, and keep pH=9 constant; After mixing, solution continues to keep reacting 5 hours with the stirring velocity of the temperature of 90 DEG C, 100 ~ 200rpm, then with the centrifugation of 6000 ~ 7000rpm, settling deionized water and washing with alcohol, 60 DEG C of vacuum-drying 24 hours, obtains Red copper oxide monocrystal nanowire.
The diameter of Red copper oxide monocrystal nanowire is about 73 ~ 86 nanometers, and length is about 7.8 ~ 8.7 microns.
Claims (6)
1. utilize plant phenolic acid to prepare a method for nano cuprous oxide wire, it is characterized in that, comprise the following steps:
(1) dissolve appropriate plant phenolic acid in deionized water, after the pH value of solution being adjusted to 7≤pH≤12 with highly basic, solution being heated to 50 ~ 95 DEG C, obtaining plant phenols acid solution;
(2) Inorganic Copper salts solution is joined in plant phenols acid solution with the speed of 5-10mL/min, controlling solution ph in dropping process is 7≤pH≤12, continues to keep solution temperature 50 ~ 95 DEG C, with the speed stirring reaction 0.5-5 hour of 100 ~ 200rpm after mixing; After reaction terminates, reaction soln is cooled to room temperature, isolates precipitation, precipitate after washing, then through vacuum-drying, obtain Red copper oxide nanometer monocrystalline wire material.
2. a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire according to claim 1, is characterized in that, in described step (1), stirs 0.5 ~ 3 hour while being heated by solution with the speed of 100 ~ 200rpm.
3. a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire according to claim 1, is characterized in that, described plant phenolic acid is one or several the mixture in Protocatechuic Acid, gallic acid, ellagic acid; Described highly basic is NaOH or the KOH aqueous solution of concentration 2 ~ 3mol/L; Described inorganic mantoquita is the mixture of one or more in copper sulfate, cupric chloride, cupric nitrate, neutralized verdigris.
4. a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire according to claim 1, is characterized in that, the Cu in the Inorganic Copper salts solution described in step (2)
2+the mol ratio of ion and plant phenolic acid is (1:2) ~ (20:1).
5. a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire according to claim 1, is characterized in that, Cu in the Inorganic Copper salts solution described in step (2)
2+the concentration of ion is 0.05 ~ 0.5mol/L.
6. a kind of method utilizing plant phenolic acid to prepare nano cuprous oxide wire according to claim 1, is characterized in that, comprise the following steps:
(1) dissolve appropriate plant phenolic acid in deionized water, after the pH value of solution being adjusted to 9≤pH≤11 with highly basic, solution is heated to 60 ~ 90 DEG C, and stir 1 ~ 2 hour with the speed of 100 ~ 200rpm, obtain plant phenols acid solution;
(2) join in plant phenols acid solution by Inorganic Copper salts solution with the speed of 5-10mL/min, controlling solution ph in dropping process is 9≤pH≤11, continues constant temperature stirring reaction 0.5-5 hour after mixing; After reaction terminates, solution is cooled to room temperature; Again solution is isolated precipitation with the centrifugation of 4000 ~ 8000rpm, after precipitate with deionized water and washing with alcohol, then through 60-80 DEG C of vacuum-drying, obtain Red copper oxide nanometer monocrystalline wire material;
Wherein, Cu in described Inorganic Copper salts solution
2+ion and plant phenolic acid mol ratio are (1:1) ~ (10:1).
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Cited By (6)
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| CN105776310A (en) * | 2016-02-03 | 2016-07-20 | 常州市好利莱光电科技有限公司 | Method for preparing cuprous oxide |
| CN107364882A (en) * | 2017-07-25 | 2017-11-21 | 东北大学 | The method of plant phenolic acid assisted hydrothermal synthesis CTS ternary compounds |
| CN109954887A (en) * | 2019-03-22 | 2019-07-02 | 扬州大学 | A kind of preparation method of silver nanowires |
| CN110327924A (en) * | 2019-06-28 | 2019-10-15 | 黄山学院 | A kind of preparation method and applications of cuprous oxide-metatitanic acid composite material |
| CN111939174A (en) * | 2020-06-05 | 2020-11-17 | 山东大学 | Metal polyphenol nano-composite as well as preparation method and application thereof |
| CN116285465A (en) * | 2023-03-08 | 2023-06-23 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | High-stability cuprous oxide composite antifouling agent material and preparation method thereof |
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| CN109954887A (en) * | 2019-03-22 | 2019-07-02 | 扬州大学 | A kind of preparation method of silver nanowires |
| CN110327924A (en) * | 2019-06-28 | 2019-10-15 | 黄山学院 | A kind of preparation method and applications of cuprous oxide-metatitanic acid composite material |
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| CN111939174A (en) * | 2020-06-05 | 2020-11-17 | 山东大学 | Metal polyphenol nano-composite as well as preparation method and application thereof |
| CN116285465A (en) * | 2023-03-08 | 2023-06-23 | 洛阳船舶材料研究所(中国船舶集团有限公司第七二五研究所) | High-stability cuprous oxide composite antifouling agent material and preparation method thereof |
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