CN104477967A - Method for preparing cuprous oxide microcrystals by taking carbon quantum dots as reducing agent - Google Patents
Method for preparing cuprous oxide microcrystals by taking carbon quantum dots as reducing agent Download PDFInfo
- Publication number
- CN104477967A CN104477967A CN201410656234.1A CN201410656234A CN104477967A CN 104477967 A CN104477967 A CN 104477967A CN 201410656234 A CN201410656234 A CN 201410656234A CN 104477967 A CN104477967 A CN 104477967A
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- China
- Prior art keywords
- carbon quantum
- quantum dot
- copper oxide
- red copper
- reductive agent
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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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
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention relates to cuprous oxide and provides a method for synthesizing cuprous oxide microcrystals with special appearance by taking carbon quantum dots as a reducing agent. The carbon quantum dots are prepared from grass as a raw material through a hydrothermal method. According to the synthesis of cuprous oxide, the carbon quantum dots are taken as the reducing agent, a copper salt is taken as a copper source, and in the presence of a surfactant and a NaOH solution, the cuprous oxide microcrystals with local special appearance are obtained by reaction through a hydrothermal method, then water washing, alcohol washing and centrifugal drying. Cuprous oxide prepared by the method is in micrometer size, the size and appearance distribution is uniform, and the purity is high.
Description
Technical field
The present invention relates to a kind of take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent; Preparation technology is simple, and raw material environmental protection, cheap and easy to get, product purity is high.
Technical background
As a kind of important P-type mos material, Red copper oxide in opto-electronic conversion, gas sensing, there is potential value and be subject to the extensive concern of Chinese scholars in the fields such as photochemical catalysis; Find, between the character of Red copper oxide and its pattern and size, there is important contacting in research in the past; Such as, find in the process taking Red copper oxide as catalyzer photo-catalytic degradation of methyl-orange, the cubic cuprous oxide catalysis activity exposing (100) crystal face is starkly lower than the regular octahedron type Red copper oxide of exposure (111) crystal face, the people such as Cao find that the photocatalytic activity of cubic Red copper oxide increases along with the reduction of its particle diameter (Materials Letters, 2014,114,88); Because Red copper oxide pattern has important impact to its character, thus control the focus that synthesis has specific dimensions, the Red copper oxide of pattern is research both at home and abroad always; In the past few years, many micro Nano materials with specific morphology are successively synthesized, such as: cubic, regular octahedron shape, spherical, nanometer wire, nanotube-shaped etc.
Carbon quantum dot is a kind of novel carbon nanomaterial, it has nontoxic, environmental sound, synthesize low cost and other advantages and be widely used in bio-imaging, photochemical catalysis, the fields such as detection of heavy metal ion, prepare in the experiment of Red copper oxide in the past, the reductive agent of usual employing is micromolecular compound, as: xitix, hydrazine hydrate, polyvalent alcohol etc.Relative to above-mentioned adopted reductive agent, carbon quantum dot reductive agent used in this experiment has cheap and easy to get, environmental protection, the advantage such as stable.
Up to now, not yet finding that there is that people adopts take green grass as the carbon quantum dot prepared of raw material for reductive agent hydrothermal reduction prepares Red copper oxide, and Red copper oxide prepared by the method is micron-scale and scale topography is evenly distributed, and purity is high.
Summary of the invention
The object of the invention be to provide a kind of with the carbon quantum dot prepared by hydro-thermal green grass for reductive agent, the method for Hydrothermal Synthesis Red copper oxide crystallite.
The present invention is realized by following steps:
(1) carbon quantum dot reductive agent is prepared: take a certain amount of green grass and be placed in the reactor that liner is tetrafluoroethylene, add distilled water, hydro-thermal reaction; Filtration obtains carbon quantum dot solution.
(2) take certain mass mantoquita, add distilled water, NaOH solution, carbon quantum dot solution, tensio-active agent, after magnetic agitation, transfer in water heating kettle, after hydro-thermal reaction; The products in water obtained and alcohol are cleaned, centrifugal, dry, obtain Red copper oxide.
In step 1, green grass is jielu grass, bent grass or Herba Stenotaphri helferi; The distilled water of every 10 ~ 30 mL adds the green grass of 2 ~ 6 g.
In step 1, hydrothermal temperature is 160 ~ 200
oc, the reaction times is 2 ~ 6 h.
In step 2, mantoquita, NaOH solution, tensio-active agent, the mass volume ratio of carbon quantum dot solution and distilled water is: 255 mL:200 ~ 800, mg:10 ~ 20 mg:8 mL:10 mL; Wherein the concentration of NaOH solution is 1 mol/L.
In step 2, mantoquita is CuCl
22H
2o, Cu (NO
3) 3H
2o or CuSO
45H
2o.
In step 2, tensio-active agent is polyoxyethylene glycol, and its molecular weight is 2000.
In step 2, churning time is 10 ~ 150 min, and stir speed (S.S.) is 100 ~ 1500 r/min.
In step 2, the temperature of hydro-thermal reaction is 160 ~ 200 DEG C, and the time of hydro-thermal reaction is 6 ~ 10 h.
During washing, water used is distilled water, and alcohol used during alcohol wash is dehydrated alcohol.
The pattern of Red copper oxide is the cuprous or flower-shaped Red copper oxide of the spherical Red copper oxide of classification, spherical alumina; X x ray diffractometer x (XRD), scanning electronic microscope (SEM), transmission electron microscope (TEM) is utilized to carry out micromorphology analysis to product.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope picture of prepared carbon quantum dot, the carbon quantum dot particle diameter as can be seen from the figure prepared by hydro-thermal green grass at 3-5 nm, good dispersity.
Fig. 2 is the XRD diffraction spectrogram of prepared three kinds of different-shape Red copper oxide crystallite samples, in figure diffraction peak all with Emission in Cubic Red copper oxide standard card one_to_one corresponding; A: the spherical Cu of classification
2o; B: spherical Cu
2o; C: flower-shaped Cu
2o.
Fig. 3 is the stereoscan photograph of prepared different-shape Red copper oxide crystallite: a, b: the spherical Cu of classification
2o; C, d: spherical Cu
2o; E, f: flower-shaped Cu
2o.
Embodiment
the preparation of embodiment 1 carbon quantum dot
What the preparation of carbon quantum dot adopted is hydrothermal synthesis method: the green grass taking 4 g, in the reactor of the tetrafluoroethylene of 50 mL, then adds 20 mL distilled water, and is placed on 180
obe incubated 4 h in the loft drier of C, take out reactor after naturally cooling to room temperature, filters solid impurity obtains carbon quantum dot solution.
the preparation of the spherical Red copper oxide of embodiment 2 classification
By the Cu (NO of 255 mg
3) 3H
2o is dissolved in 10 mL distilled water, then add 10 mL NaOH solution (1 mol/L), the Macrogol 2000 of 600 mg and the carbon quantum solution prepared by 8 mL is added after dripping, mixing solutions 1500 r/min stirs 10 min, then transfer in the reactor of 50 mL tetrafluoroethylene, put into baking oven, 180
oreact 8 h under C, take out reactor and naturally cool to room temperature; Gained sample deionized water and dehydrated alcohol are cleaned 3 times respectively, to be centrifugally placed in vacuum drying oven 60
odry 8 h of C.
the preparation that embodiment 3 spherical alumina is cuprous
By the CuCl of 255 mg
22H
2o is dissolved in 10 mL distilled water, then add 20 mL NaOH solution (1 mol/L), the Macrogol 2000 of 800 mg and the carbon quantum solution prepared by 8 mL is added after dripping, mixing solutions 100 r/min stirs 150 min, then transfer in the reactor of 50 mL tetrafluoroethylene, put into baking oven, 200
oreact 6 h under C, take out reactor and naturally cool to room temperature; Gained sample deionized water and dehydrated alcohol are cleaned 3 times respectively, to be centrifugally placed in vacuum drying oven 60
odry 8 h of C.
the preparation of the flower-shaped Red copper oxide of embodiment 4
By the CuCl of 255 mg
22H
2o is dissolved in 10 mL distilled water, then add 20 mL NaOH solution (1 mol/L), the Macrogol 2000 of 200 mg and the carbon quantum solution prepared by 8 mL is added after dripping, mixing solutions 900 r/min stirs 80 min, then transfer in the reactor of 50 mL tetrafluoroethylene, put into 160
oreact 10 h in the baking oven of C, take out reactor and naturally cool to room temperature; Gained sample distilled water and dehydrated alcohol are cleaned 3 times respectively, to be centrifugally placed in vacuum drying oven 60
odry 8 h of C.
Claims (10)
1. one kind is the method that Red copper oxide crystallite prepared by reductive agent with carbon quantum dot, it is characterized in that: take certain mass mantoquita, add distilled water, NaOH solution, carbon quantum dot solution and tensio-active agent, after magnetic agitation, transfer in water heating kettle, after hydro-thermal reaction; The products in water obtained and alcohol are cleaned, centrifugal, dry, obtain Red copper oxide.
2. a kind of as claimed in claim 1 take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent, it is characterized in that the preparation method of described carbon quantum dot solution is as follows: take a certain amount of green grass and be placed in the reactor that liner is tetrafluoroethylene, add distilled water, hydro-thermal reaction; Filtration obtains carbon quantum dot solution.
3. a kind of is as claimed in claim 2 the method that Red copper oxide crystallite prepared by reductive agent with carbon quantum dot, it is characterized in that: described green grass is jielu grass, bent grass or Herba Stenotaphri helferi; The distilled water of every 10 ~ 30 mL adds the green grass of 2 ~ 6 g.
4. a kind of is as claimed in claim 2 the method that Red copper oxide crystallite prepared by reductive agent with carbon quantum dot, it is characterized in that: hydrothermal temperature is 160 ~ 200
oc, the reaction times is 2 ~ 6 h.
5. a kind of as claimed in claim 1 take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent, it is characterized in that: mantoquita, NaOH solution, tensio-active agent, the mass volume ratio of carbon quantum dot solution and distilled water is: 255 mL:200 ~ 800, mg:10 ~ 20 mg:8 mL:10 mL; Wherein the concentration of NaOH solution is 1 mol/L.
6. a kind of as described in claim 1 or 5 take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent, it is characterized in that: mantoquita is CuCl
22H
2o, Cu (NO
3) 3H
2o or CuSO
45H
2o.
7. a kind of as described in claim 1 or 5 take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent, and it is characterized in that: tensio-active agent is polyoxyethylene glycol, its molecular weight is 2000.
8. a kind of is as claimed in claim 1 the method that Red copper oxide crystallite prepared by reductive agent with carbon quantum dot, and it is characterized in that: churning time is 10 ~ 150 min, stir speed (S.S.) is 100 ~ 1500 r/min.
9. a kind of is as claimed in claim 1 the method that Red copper oxide crystallite prepared by reductive agent with carbon quantum dot, it is characterized in that: the temperature of hydro-thermal reaction is 160 ~ 200 DEG C, and the time of hydro-thermal reaction is 6 ~ 10 h.
10. a kind of as claimed in claim 1 take carbon quantum dot as the method that Red copper oxide crystallite prepared by reductive agent,
It is characterized in that: during washing, water used is distilled water, alcohol used during alcohol wash is dehydrated alcohol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410656234.1A CN104477967B (en) | 2014-11-18 | 2014-11-18 | A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot |
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| CN201410656234.1A CN104477967B (en) | 2014-11-18 | 2014-11-18 | A kind of method preparing Red copper oxide crystallite for reducing agent with carbon quantum dot |
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| CN104477967B CN104477967B (en) | 2016-08-17 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110269093A (en) * | 2019-07-19 | 2019-09-24 | 云南省农业科学院农产品加工研究所 | A kind of fresh-cut fruit and vegetable fresh-keeping liquid |
| CN111524716A (en) * | 2020-01-10 | 2020-08-11 | 厦门理工学院 | Preparation and application of composite electrode material with manila herb as carbon source |
| CN116396749A (en) * | 2023-02-15 | 2023-07-07 | 桂林电子科技大学 | Synthesis of metal selenide quantum dot and carbon dot and preparation method of light-emitting device |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462720A (en) * | 2003-06-10 | 2003-12-24 | 东北师范大学 | Method for preparing nano tube of some metalloid oxides and metals with size and shape being controllable |
| CN103100725A (en) * | 2013-02-28 | 2013-05-15 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
-
2014
- 2014-11-18 CN CN201410656234.1A patent/CN104477967B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1462720A (en) * | 2003-06-10 | 2003-12-24 | 东北师范大学 | Method for preparing nano tube of some metalloid oxides and metals with size and shape being controllable |
| CN103100725A (en) * | 2013-02-28 | 2013-05-15 | 江苏大学 | Preparation method of silver/carbon quantum dot composite nanometer materials |
Non-Patent Citations (1)
| Title |
|---|
| SEN LIU ET AL.: "Hydrothermal Treatment of Grass: A Low-Cost, Green Route to Nitrogen-Doped, Carbon-Rich, Photoluminescent Polymer Nanodots as an Effective Fluorescent Sensing Platform for Label-Free Detection of Cu(II) Ions", 《ADV.MATER.》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110269093A (en) * | 2019-07-19 | 2019-09-24 | 云南省农业科学院农产品加工研究所 | A kind of fresh-cut fruit and vegetable fresh-keeping liquid |
| CN111524716A (en) * | 2020-01-10 | 2020-08-11 | 厦门理工学院 | Preparation and application of composite electrode material with manila herb as carbon source |
| CN116396749A (en) * | 2023-02-15 | 2023-07-07 | 桂林电子科技大学 | Synthesis of metal selenide quantum dot and carbon dot and preparation method of light-emitting device |
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