CN108872204A - A kind of preparation and application of two dimension porous graphene/cuprous oxide composite material - Google Patents
A kind of preparation and application of two dimension porous graphene/cuprous oxide composite material Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of two-dimentional porous graphene/cuprous oxide composite material, are that Copper dichloride dihydrate is added to 5 ~ 30 min of ultrasound in the aqueous dispersions of graphene oxide, filter, obtain the mixture of copper chloride and graphene oxide；After mixture to be placed in 40 ~ 60 DEG C of oven drying again, it is placed in Muffle furnace and calcines to obtain crude product；Crude product is washed with water and dehydrated alcohol repeatedly, dry to get two-dimentional porous graphene/cuprous oxide composite material.The composite material generates in chemical luminous system in catalysis hydrogen peroxide oxidation luminol, and good linear relationship is presented between the logarithm of the chemiluminescence intensity concentration at 425 nm, and the range of linearity is 1.0 × 10‑8 M~8.0×10‑4 Therefore M is widely used prospect in fields such as catalysis, biochemical analysis and detections.
Description
Technical field
The present invention relates to a kind of preparation methods of two-dimentional porous graphene/cuprous oxide composite material, mainly as catalysis
Agent generates chemiluminescence reaction for being catalyzed hydrogen peroxide oxidation luminol, belongs to field of compound material and Measurement for Biotechnique neck
Domain.
Background technique
Luminol（luminol）Also known as luminol, English name 5-Amino-2,3-dihydro-1,4-
phthalazinedione.It is a kind of yellow crystals or Beige powder under its room temperature, is a kind of more stable chemistry examination
Agent.Meanwhile luminol is a kind of strong acid again, has certain stimulation to eyes, skin, respiratory tract.On medical jurisprudence, luminol
Reaction is called the reaction of two acyl of aminobenzene, one callosity, it is possible to authenticate by cleaning, the blood stain of time long ago.Biologically then use
Luminol detects the copper in cell, iron and the presence of cyanide.Luminol was just synthesized early in 1853.1928
Year, chemist has found that this compound has a marvellous characteristic for the first time, blue light can be issued when it is oxidized.After several years, just
Someone expects removing detection bloodstain using this characteristic.Contain hemoglobin in blood, the oxygen that we suck from air is exactly
By this protein delivery to whole body each section.Hemoglobin contains iron, and the decomposition of iron energy catalyzing hydrogen peroxide, allows peroxide
Change hydrogen and become water and single oxygen, single oxygen reoxidizes luminol and shines by it.When examining blood stain, luminol and ferroheme
（Hemoglobin is responsible for a kind of protein of transport oxygen in hemoglobin）It reacts, shows glaucous fluorescence.This inspection
Survey method is extremely sensitive, can detect the blood of only hundred a ten thousandth contents, can quilt dripping a droplet of blood into a large cylinder water
It detected.
Luminol is only crossed with oxidizer treatment and can just be shone.Usually using hydrogen peroxide and a kind of mixing of hydroxide bases
Aqueous solution is as exciting agent.Under iron compound catalysis, decomposing hydrogen dioxide solution is oxygen and water：2 H2O2→ O2 + 2 H2O.It is real
It tests often using the potassium ferricyanide as the source of catalyst iron in room, and the catalyst on medical jurisprudence is then precisely in hemoglobin
Iron.Enzyme in many biosystems can also catalyzing hydrogen peroxide decomposition reaction.Since nano material has the property of class catalyzing enzyme
Can, it can be used to be catalyzed hydrogen peroxide（H2O2）Aoxidize luminol（Luminol）Generate chemiluminescence.Document 1（Nano Lett.
2017,17,2043 ~ 2048）It is middle to use Cu2+- GO nanoparticle generates chemiluminescence to be catalyzed hydrogen peroxide oxidation luminol, but
It is using the Cu arrived2+The concentration of-GO nanoparticle is 10 μ g mL−1, the range of linearity of hydrogen peroxide is 0 ~ 1.5 × 10-3 M；
Document 2（ACS Nano 2017,11,3247 ~ 3253）It is middle to use Cu2+-g-C3N4Nanoparticle is as the catalyst to catalysis dioxygen
Water oxygen esterification luminol generates chemiluminescence, and the material concentration used is 5.0 μ g mL−1, hydrogen peroxide 0 ~ 2 × 10 as the result is shown-3 M
There is good linear relationship in range.However, the nanoparticle Cu that document 1,2 is reported2+-GO、Cu2+-g-C3N4It is catalyzed dioxygen
Water oxygen esterification luminol generates chemiluminescence, can only be in hydrogen peroxide 0 ~ 2 × 10-3In the range of M effectively.
Summary of the invention
The object of the present invention is to provide a kind of preparation methods of two-dimentional porous graphene/cuprous oxide composite material；
It is a further object of the present invention to provide two-dimentional porous graphene/cuprous oxide composite materials of above-mentioned preparation as catalyst
For being catalyzed hydrogen peroxide（H2O2）Aoxidize luminol（Luminol）Generate chemiluminescence reaction.
（One）The preparation of two-dimentional porous graphene/cuprous oxide composite material
The method that the present invention prepares two-dimentional porous graphene/cuprous oxide composite material, is that Copper dichloride dihydrate is added to oxygen
5 ~ 30 min of ultrasound in the aqueous dispersions of graphite alkene filter, obtain the mixture of copper chloride and graphene oxide；It again will mixing
Object is placed in 40 ~ 60 DEG C of baking oven dry be placed on alcolhol burner and lights, and being burnt repeatedly to brick-red cuprous oxide, it is more to cover
There is obtaining crude product in hole graphene；Or mixture is placed in in 40 ~ 60 DEG C of baking oven drying and is placed in Muffle furnace, in 420 ~
The min of 1min ~ 5 is calcined at 450 DEG C, obtains crude product；Crude product water and dehydrated alcohol, which wash, removes impurity, dry to get two
Tie up porous graphene/cuprous oxide composite material.
The concentration of the graphene oxide dispersion is 1 ~ 10 g/L；The mass ratio of Copper dichloride dihydrate and graphene oxide
It is 100:1~800:1.
（Two）Porous graphene/cuprous oxide composite material structure
1, transmission electron microscope（TEM）And element mapping figure
For two-dimentional porous graphene/cuprous oxide composite material, need to utilize transmission electron microscope observing pattern.Figure 1A is that two dimension is more
Hole graphene/cuprous oxide composite material transmission electron microscope（TEM）.As can be seen that there is a large amount of oxidation in the surface of graphene
Cuprous particle, while graphene surface has a large amount of two-dimensional nano-pore（It is represented with small white spots）.Figure 1B is two-dimentional porous stone
Black alkene/cuprous oxide composite material dark field STEM figure, Fig. 1 C-F are the element mapping figure of respective element in composite material.
Wherein C：C-K；D：O-K；E：Cu-K；F：Cu-L.In conjunction with Figure 1B and Fig. 1 C-F it can be concluded that, the composite material mainly include C,
O, tri- kinds of elements of Cu.
2, power spectrum（EDX）Figure
Fig. 2 is the EDX figure of two-dimentional porous graphene/cuprous oxide composite material.From energy spectrum diagram as can be seen that the material by C,
O, tri- kinds of element compositions of Cu, this result are also to fit like a glove with the element mapping figure in Fig. 1 C-F.
3, x-ray photoelectron spectroscopy（XPS）Full spectrum and fine spectrum
Fig. 3 A is that the XPS of two-dimentional porous graphene/cuprous oxide composite material is composed entirely, equally illustrates two-dimentional porous graphene/oxygen
Change cuprous composite material to be mainly made of C, O and Cu.Fig. 3 B is C1SFine spectrum, deposited from can be confirmed in figure in the composite material
In C C (sp3, 284.6 eV), C O (sp2, 286.0 eV) and C=O (sp2, 287.8 eV) and key, Fig. 3 C is O1SEssence
Thin spectrum, two spectral peaks of the fine spectrum at 530.7 eV and 531.7 eV correspond respectively to Cu in composite material2O Lattice Oxygen and
The hydroxyl oxygen of composite material surface, the spectral peak at 532.8 eV correspond to C-OH/C-O-C key or copper oxide in composite material
Lattice Oxygen；Fig. 3 D is Cu2pFine spectrum, wherein spectral peak at 952.6 eV and 932.7 eV corresponds to oxygen in composite material
Change cuprous Cu 2p3/2With Cu 2p1/2Spectral peak, the spectral peak at 934.6 and 953.7 eV prove the presence for having small amounts copper.
4, XRD diagram
Fig. 4 is the XRD diagram of two-dimentional porous graphene/cuprous oxide composite material, as can be seen from the figure reproducibility graphite oxide
Alkene is 21.2o's（002）Crystal face is in two-dimentional porous graphene/cuprous oxide composite material（NPG/Cu2O）Middle presence.In addition, multiple
Condensation material, there is also a series of typical diffraction maximums, respectively corresponds at 29.4,36.4,42.2,61.3,73.6 and 77.3 °
The cube nano cuprous oxide in composite material（110）,（111）,（200）,（220）,（311）With（222）Crystal face, and
Peak type is sharp, and diffracted intensity is stronger, illustrates that its crystallinity is preferable.
5, Raman spectrogram
Fig. 5 is the Raman spectrogram of composite material.Graphite is equally existed from can be seen that in the composite material in Raman spectrogram
The D- band of alkene, G- band and 2D/G '-band, in addition in 124 cm−1, 147 cm−1, 218 cm−1With 628 cm−1The bands of a spectrum at place prove
Cu2The presence of O.
（Three）Two-dimentional porous graphene/cuprous oxide composite material performance
Fig. 6 is two-dimentional porous graphene/cuprous oxide composite material and simple cuprous oxide, two-dimentional porous graphene and goes back
Originality graphene oxide/cuprous oxide composite material catalytic performance compares.Wherein (i) luminol (0.5mM)+H2O2(7
mM)； (ii) luminol (0.5 mM)+ H2O2 (7mM)+ Cu2O (5.0 μg mL−1)； (iii) luminol (0.5
mM)+ H2O2 (7mM)+NPG(5.0μg mL−1)；(iv) luminol(0.5mM)+H2O2(7mM)+ rGO/Cu2O
nanocomposite (5.0μg mL−1)； (v) luminol (0.5mM)+H2O2 (7mM)+ NPG/Cu2O
nanocomposite (5.0μg mL−1).From fig. 6, it can be seen that two dimension porous graphene/cuprous oxide prepared by the present invention is multiple
Condensation material has optimal catalytic performance.
The Catalysis Principles figure of composite material prepared by the present invention is as shown in Figure 7.Its Catalysis Principles is：Two-dimentional porous graphite
Alkene/cuprous oxide composite material serves as Mimetic Peroxidase, has catalytic action.Under alkaline condition, two-dimentional porous graphite
Alkene/cuprous oxide composite material can be catalyzed hydrogen peroxide oxidation luminol reaction generate excitation state phthalate yin from
Son generates light radiation when to ground state transition at 425 nm.
Fig. 8 is the chemiluminescence light that two-dimentional porous graphene/cuprous oxide composite material is catalyzed hydrogen peroxide oxidation luminol
Spectrogram（A）And H2O2Canonical plotting（B）.Scheme in A, NPG/Cu2The concentration of O composite material is 5.0 μ g mL−1,
The concentration of luminol is 0.5 mM, the corresponding H of curve a to k2O2Concentration be respectively 0,0.05,0.1,0.2,0.5,0.8,1,
2,3,5 and 7 Mm.It can be seen that the increase with hydrogen peroxide concentration from Fig. 8 A, the catalytic performance of composite material gradually increases
By force.It can be seen from fig. 8b that being presented between the concentration of chemiluminescence intensity and hydrogen peroxide of the system at 425 nm good
Linear relationship, the range of linearity are 0 ~ 7 × 10-3 M。
In addition, we are in two-dimentional porous graphene/cuprous oxide composite material-luminol-hydrogen peroxide catalyst system, together
When introduce reduced nicotinamide adenine dinucleotide（NADH）, it is found that the chemiluminescence intensity of system can gradually weaken.Fig. 9 is
The detection principle diagram of NADH.Possible cause has two aspects：（1）The chemiluminescence spectra of luminol and the absorption spectrum of NADH are deposited
It is partly overlapping, is leading between luminol and NADH that there are Chemiluminescence Resonance energy transfers；（2）After NADH is added, due to multiple
Condensation material generates chemiluminescence in addition to catalysis hydrogen peroxide oxidation luminol, can also be catalyzed hydrogen peroxide oxidation NADH and generate NAD+,
Subsequent process can also consume a part of hydrogen peroxide, so the chemiluminescence intensity detected at 425 nm will be with NADH
The increase of concentration and weaken.
Figure 10 is two-dimentional porous graphene/cuprous oxide composite material-hydrogen peroxide-luminol after various concentration NADH is added
System chemistry luminescent spectrum figure（A）And the canonical plotting of NADH（B）.Scheme in A, NPG/Cu2The concentration of O composite material is 5.0
μg mL−1, the concentration of luminol is 0.5 mM, H2O2Concentration be 7 mM, the concentration of the corresponding NADH of curve a to l is respectively
0,0.01,0.02,0.05,0.2,2,5,20,50,80,200 and 800 μM.It is from Figure 10 A it can be seen that dense with NADH
Degree increases, and the chemiluminescence intensity of system gradually weakens.From in Figure 10 B as can be seen that chemiluminescence of the system at 425 nm
Good linear relationship is presented between intensity and the logarithm of NADH concentration, the range of linearity is 1.0 × 10-8 M~8.0×10-4 M,
The detection range has apparent advantage compared with result reported in the literature.
In conclusion two dimension porous graphene/cuprous oxide composite material prepared by the present invention, surface is dispersed with largely
Two-dimensional nanoscale hole and cuprous nano cube have bigger specific surface area and higher activity, in catalysis, biochemistry
The fields such as analysis detection are widely used prospect.
Detailed description of the invention
Fig. 1 is the Electronic Speculum phenogram of two-dimentional porous graphene/cuprous oxide composite material, and wherein A is two-dimentional porous graphite
Alkene/cuprous oxide composite material TEM figure；B is the dark field STEM figure of two-dimentional porous graphene/cuprous oxide composite material；C-F
For the element mapping figure of respective element in composite material.
Fig. 2 is the EDX figure of two-dimentional porous graphene/cuprous oxide composite material.
Fig. 3 is composed entirely for the XPS of two-dimentional porous graphene/cuprous oxide composite material and C1S、O1S、Cu2pFine spectrum.Fig. 4
For two-dimentional porous graphene/cuprous oxide composite material XRD diagram.
Fig. 5 is the Raman spectrogram of two-dimentional porous graphene/cuprous oxide composite material.
Fig. 6 be two-dimentional porous graphene/cuprous oxide composite material and simple cuprous oxide, two-dimentional porous graphene with
And reproducibility graphene oxide/cuprous oxide composite material catalytic performance compares.
Fig. 7 is that two-dimentional porous graphene/cuprous oxide composite material is catalyzed the generation chemiluminescence of hydrogen peroxide oxidation luminol
Catalysis Principles figure.
Fig. 8 is the chemiluminescence light that two-dimentional porous graphene/cuprous oxide composite material is catalyzed hydrogen peroxide oxidation luminol
Spectrogram（A）And H2O2Canonical plotting（B）.
Fig. 9 is the detection principle diagram of NADH.
Figure 10 is two-dimentional porous graphene/cuprous oxide composite material-hydrogen peroxide-luminol after various concentration NADH is added
System chemistry luminescent spectrum figure（A）And the canonical plotting of NADH（B）.
Specific embodiment
Below by specific embodiment to the preparation method of porous graphene/cuprous oxide composite material of the invention two-dimentional,
Catalysis and detection performance are described further.
Embodiment 1
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 2.5 g/L in water.Take the oxidation of 2.5 g/L
8.0 mL of graphene dispersing solution, 15 min of room temperature ultrasound.2.0 g Copper dichloride dihydrates are weighed, are dissolved in above-mentioned dispersion liquid, room
10 min of warm ultrasound.It filters, then mixture is placed on after being dried in 60 DEG C of baking oven, is placed in 430 DEG C of Muffle furnace, fire
2 min are burnt, i.e., it can be seen that the porous graphene appearance of brick-red cuprous oxide covering, as crude product；Crude product ultrapure water
Washing 5 times ethanol washing 3 times, removes impurity and dry to get two-dimentional porous graphene/cuprous oxide composite material.The two dimension
Porous graphene/cuprous oxide composite material chemiluminescence catalytic performance and result shown in Fig. 9 fit like a glove.
Embodiment 2
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 1.0 g/L in water.Take the oxidation of 1.0 g/L
10.0 mL of graphene dispersing solution, 10 min of room temperature ultrasound.2.5 g Copper dichloride dihydrates are weighed, are dissolved in above-mentioned dispersion liquid,
15 min of room temperature ultrasound.It filters, then mixture is placed on after being dried in 50 DEG C of baking oven, is placed in 450 DEG C of Muffle furnace,
Burn 1 min, i.e., it can be seen that the porous graphene appearance of brick-red cuprous oxide covering, as crude product；Crude product is with ultrapure
Water washing 5 times, ethanol washing 3 times, remove impurity and dry to get two-dimentional porous graphene/cuprous oxide composite material.This two
Result shown in dimension porous graphene/cuprous oxide composite material chemiluminescence catalytic performance and embodiment 1 is coincide substantially.
Embodiment 3
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 1.0 g/L in water.Take the oxidation of 1.0 g/L
50.0 mL of graphene dispersing solution, 20 min of room temperature ultrasound.16.0 g Copper dichloride dihydrates are weighed, are dissolved in above-mentioned dispersion liquid,
30 min of room temperature ultrasound.It filters, then mixture is placed in 60 DEG C of baking oven and is dried in the Muffle furnace for being placed on 420 DEG C,
Burn 5 min, i.e., it can be seen that the porous graphene appearance of brick-red cuprous oxide covering, as crude product；Crude product is with ultrapure
Water washing 10 times, ethanol washing 3 times, remove impurity and dry to get two-dimentional porous graphene/cuprous oxide composite material.It should
Two-dimentional porous graphene/cuprous oxide composite material chemiluminescence catalytic performance is compared with the result of embodiment 1, catalytic performance
Slightly reduce.
Embodiment 4
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 5.0 g/L in water.Take graphene oxide point
2.0 mL of dispersion liquid, 5 min of room temperature ultrasound；1.6 g Copper dichloride dihydrates are weighed, are dissolved in above-mentioned dispersion liquid, room temperature ultrasound 20
min；It filters, then mixture is placed in 40 DEG C of baking oven after drying and is lighted with alcolhol burner, burnt repeatedly to brick-red oxidation
The porous graphene of cuprous covering occurs being crude product；Crude product ethanol washing 3 times, removes impurity with milli-Q water 5 times
And it is dry to get two-dimentional porous graphene/cuprous oxide composite material.Two dimension porous graphene/cuprous oxide the composite material
Chemiluminescence catalytic performance compared with the result of embodiment 1, catalytic performance significantly reduce.
Embodiment 5
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 10.0 g/L in water.Take the oxygen of 10.0 g/L
1.0 mL of graphite alkene dispersion liquid, 5 min of room temperature ultrasound.4.0 g Copper dichloride dihydrates are weighed to be dissolved in 7 mL ultrapure waters, then
It is mixed with the dispersion liquid of above-mentioned graphene oxide, 30 min of room temperature ultrasound.It filters, then mixture is placed in 50 DEG C of baking oven
It is lighted after middle drying with alcolhol burner, the porous graphene covered to brick-red cuprous oxide that burns repeatedly occurs being crude product；
Crude product removes impurity and dry to get two-dimentional porous graphene/cuprous oxide with milli-Q water 5 times, ethanol washing 3 times
Composite material.The result phase of two dimension porous graphene/cuprous oxide composite material chemiluminescence catalytic performance and embodiment 3
Than catalytic performance slightly reduces.
Embodiment 6
Graphene oxide ultrasonic disperse is configured to the graphene oxide dispersion of 5.0 g/L in water.Take the oxidation of 5.0 g/L
2.0 mL of graphene dispersing solution, 5 min of room temperature ultrasound.2.0 g Copper dichloride dihydrates are weighed to be dissolved in 6 mL ultrapure waters, then with
The dispersion liquid of above-mentioned graphene oxide mixes, 5 min of room temperature ultrasound.It filters, then mixture is placed in 60 DEG C of baking oven and is dried
It is lighted after dry with alcolhol burner, the porous graphene covered to brick-red cuprous oxide that burns repeatedly occurs being crude product；It is thick to produce
Product are removed impurity and drying are compound to get two-dimentional porous graphene/cuprous oxide with milli-Q water 5 times, ethanol washing 3 times
Material.Two dimension porous graphene/cuprous oxide composite material chemiluminescence catalytic performance and result shown in embodiment 1 are basic
It coincide.
Through the foregoing embodiment it is found that during preparing composite material, Copper dichloride dihydrate and graphene oxide
Mass ratio should be controlled 100:1~800:In 1 range, and the optium concentration of Copper dichloride dihydrate is 250 g/L, and it is dense to be higher than this
Its catalytic performance will weaken after degree；Calcination temperature in Muffle furnace should control between 420 DEG C ~ 450 DEG C, in order to reach compared with
Good analytical effect, in the range as the temperature rises, burning time should gradually decrease.
Claims (6)
1. a kind of preparation method of two dimension porous graphene/cuprous oxide composite material, is that Copper dichloride dihydrate is added to oxygen
5 ~ 30 min of ultrasound in graphite alkene aqueous dispersions filter, obtain the mixture of copper chloride and graphene oxide；Again by mixture
It is placed in the porous graphite for being lighted after drying with alcolhol burner in 40 ~ 60 DEG C of baking oven and burning and covering to brick-red cuprous oxide repeatedly
There is obtaining crude product in alkene, or mixture is placed in dry be placed in Muffle furnace in 40 ~ 60 DEG C of baking oven and calcines to obtain crude product；
Crude product is washed to remove impurity, dry to get two-dimentional porous graphene/cuprous oxide composite material.
2. the preparation method of two dimension porous graphene/cuprous oxide composite material as described in claim 1, it is characterised in that：Institute
The concentration for stating graphene oxide dispersion is 1 ~ 10 g/L.
3. the preparation method of two dimension porous graphene/cuprous oxide composite material as described in claim 1, it is characterised in that：Two
The mass ratio of Hydrated copper chloride and graphene oxide is 100:1~800:1.
4. the preparation method of two dimension porous graphene/cuprous oxide composite material as described in claim 1, it is characterised in that：Institute
Stating the calcining in Muffle furnace is that the min of 1 min ~ 5 is heat-treated at 420 ~ 450 DEG C.
5. the preparation method of two dimension porous graphene/cuprous oxide composite material as described in claim 1, it is characterised in that：Institute
Stating washing is to be washed repeatedly with water and dehydrated alcohol.
6. two-dimentional porous graphene/cuprous oxide composite material of method preparation as described in claim 1 is used for as catalyst
It is catalyzed hydrogen peroxide oxidation luminol and generates chemiluminescence reaction.
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| CN115537959A (en) * | 2021-09-28 | 2022-12-30 | 江苏青昀新材料科技有限公司 | Composite material |
| CN114113057A (en) * | 2021-11-12 | 2022-03-01 | 山西大学 | Copper oxide nanorod-heme functionalized graphene and preparation method and application thereof |
| CN114113057B (en) * | 2021-11-12 | 2024-05-24 | 山西大学 | Copper oxide nanorod-heme functionalized graphene and preparation method and application thereof |
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