CN110358534A - A kind of preparation method that carbon quantum dot combined oxidation is cuprous - Google Patents
A kind of preparation method that carbon quantum dot combined oxidation is cuprous Download PDFInfo
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- CN110358534A CN110358534A CN201910574792.6A CN201910574792A CN110358534A CN 110358534 A CN110358534 A CN 110358534A CN 201910574792 A CN201910574792 A CN 201910574792A CN 110358534 A CN110358534 A CN 110358534A
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 230000003647 oxidation Effects 0.000 title claims abstract description 17
- 238000007254 oxidation reaction Methods 0.000 title claims abstract description 17
- BERDEBHAJNAUOM-UHFFFAOYSA-N copper(I) oxide Inorganic materials [Cu]O[Cu] BERDEBHAJNAUOM-UHFFFAOYSA-N 0.000 claims abstract description 29
- 229940112669 cuprous oxide Drugs 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 15
- 150000001879 copper Chemical class 0.000 claims abstract description 13
- 239000012266 salt solution Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 49
- 229910052799 carbon Inorganic materials 0.000 claims description 49
- 239000000243 solution Substances 0.000 claims description 48
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- 230000001376 precipitating effect Effects 0.000 claims description 29
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 18
- 238000013019 agitation Methods 0.000 claims description 17
- 238000001035 drying Methods 0.000 claims description 16
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 15
- 239000008103 glucose Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 13
- 229910021641 deionized water Inorganic materials 0.000 claims description 13
- AEJIMXVJZFYIHN-UHFFFAOYSA-N copper;dihydrate Chemical compound O.O.[Cu] AEJIMXVJZFYIHN-UHFFFAOYSA-N 0.000 claims description 10
- 238000011049 filling Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 239000008236 heating water Substances 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000000502 dialysis Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- ZIALXKMBHWELGF-UHFFFAOYSA-N [Na].[Cu] Chemical compound [Na].[Cu] ZIALXKMBHWELGF-UHFFFAOYSA-N 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- JXSRRBVHLUJJFC-UHFFFAOYSA-N 7-amino-2-methylsulfanyl-[1,2,4]triazolo[1,5-a]pyrimidine-6-carbonitrile Chemical compound N1=CC(C#N)=C(N)N2N=C(SC)N=C21 JXSRRBVHLUJJFC-UHFFFAOYSA-N 0.000 claims description 2
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 2
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims description 2
- 238000007710 freezing Methods 0.000 claims description 2
- 230000008014 freezing Effects 0.000 claims description 2
- 229910052760 oxygen Inorganic materials 0.000 claims description 2
- 239000001301 oxygen Substances 0.000 claims description 2
- BEGBSFPALGFMJI-UHFFFAOYSA-N ethene;sodium Chemical group [Na].C=C BEGBSFPALGFMJI-UHFFFAOYSA-N 0.000 claims 1
- KRFJLUBVMFXRPN-UHFFFAOYSA-N cuprous oxide Chemical compound [O-2].[Cu+].[Cu+] KRFJLUBVMFXRPN-UHFFFAOYSA-N 0.000 abstract description 11
- 239000002245 particle Substances 0.000 abstract description 6
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 206010001497 Agitation Diseases 0.000 description 15
- 239000011449 brick Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 244000189799 Asimina triloba Species 0.000 description 1
- 235000006264 Asimina triloba Nutrition 0.000 description 1
- 235000009467 Carica papaya Nutrition 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000037237 body shape Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000013486 operation strategy Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
Abstract
The invention discloses a kind of preparation methods that carbon quantum dot combined oxidation is cuprous, belong to technical field of composite preparation.The method of the invention is on the basis of preparing carbon quantum dot by hydrothermal reaction kettle, copper salt solution is mixed with carbon quantum dot using molecular mixing method, make copper salt solution decomposition, then forming core, cuprous oxide of the oxidation generation containing carbon quantum dot, obtains cuprous oxide-carbon quantum dot composite powder.The particle size for the carbon quantum dot that the method for the invention is prepared is substantially in 10nm hereinafter, and being uniformly distributed and being embedded on cuprous oxide particle.
Description
Technical field
The present invention relates to a kind of preparation methods that carbon quantum dot combined oxidation is cuprous, belong to composite material technology of preparing neck
Domain.
Background technique
With the development and progress of society, the demand to material also becomes more and more diversified.Pursuing more preferable performance
And while beautiful appearance, it is also desirable to production cost energy relative reduction；Only production cost reduces, and operation strategies are
It can preferably be widened.
Carbon quantum dot, synthesis technology is simple, and cost is very low, herbage, pawpaw, this series green energy such as glucose is all
Can synthesize carbon quantum dot, and with and a series of researchs have shown that the toxicity of carbon quantum dot can be ignored, there is bio-compatible
Property, it has good stability, the unique advantages such as good conductivity.Therefore a kind of new cuprous composite powder of carbon quantum dot combined oxidation is probed into out
The method at end has certain theory directive significance whether for functional material or structural material.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods that carbon quantum dot combined oxidation is cuprous, specifically include following step
It is rapid:
(1) mantoquita, carbon quantum dot are separately added into the container for filling deionized water, the mass ratio of mantoquita and water be 1:50 ~
100, the mass ratio of carbon quantum dot and water is 1:600 ~ 1000, and carbon quantum dot solution is slowly dropped in copper salt solution, continues to stir
After mixing 5 ~ 10min, heating water bath obtains carbon quantum dot-mantoquita mixed liquor to 70 DEG C ~ 85 DEG C, wherein carbon quantum dot and mantoquita
Mass ratio is 1:390 ~ 1560.
(2) NaOH solution that mass fraction is 40% ~ 50% is prepared, NaOH solution is slowly dropped into the carbon that step (1) obtains
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in nanotube-mantoquita mixed solution；Carbon quantum dot-in the process
Kocide SD precipitating is always held at heating and magnetic agitation in the water-bath that temperature is 70 ~ 85 DEG C, so that Kocide SD precipitates
Forming core is complete.
(3) it prepares mass fraction and is 50% ~ 60% glucose solution, while glucose solution is slowly dropped into step (2)
In obtained carbon quantum dot-Kocide SD precipitating, it is always held at progress magnetic force in the water-bath that temperature is 70 ~ 85 DEG C and is stirred
It mixes, until solution colour becomes brick-red precipitating, obtains uniformly mixed carbon quantum dot-cuprous oxide mixed liquor, filter
Carbon quantum dot-cuprous oxide composite powder is obtained after drying.
Preferably, step (1) the of the present invention carbon quantum dot the preparation method comprises the following steps: citric acid and ethylene glycol are dissolved in dress
Have in the polytetrafluoroethyllining lining of deionized water, polytetrafluoroethyllining lining is placed in stainless steel cauldron, is heated to 100 ~ 150
DEG C, 300 ~ 360min is persistently kept the temperature, is then cooled to room temperature, the solution in taking-up reaction kettle, 6000 ~ 9000r/min centrifugation 20 ~
30min, then supernatant 10 ~ 12h of dialysis treatment that centrifugal treating is obtained, obtain powder formed carbon quantum dot after freeze-drying.
Preferably, the vacuum degree of freezing dry process of the present invention is less than 1Pa, and condenser temperature is -60 DEG C ~ -40 DEG C.
Preferably, present invention mantoquita as described in step (1) is copper acetate, copper stearate, copper sulphate, copper nitrate, second two
One or more of amine tetraacethyl sodium copper, EDTA copper sodium are configured according to arbitrary proportion and are formed.
Preferably, drying temperature is 60 ~ 70 DEG C in step (3) of the present invention, and drying time is 10 ~ 15h.
The beneficial effects of the present invention are:
(1) the method for the invention preparation carbon quantum dot-cuprous oxide composite material and preparation method thereof is simple, easy to operate, and carbon
Quantum point grain diameter is uniformly (such as Fig. 1)；The carbon quantum dot being prepared-cuprous oxide composite powder is substantially at nanoscale thin
Grain, without other field trashes.
(2) cost is relatively low for cuprous oxide composite material for the method for the invention preparation carbon quantum dot-.
Detailed description of the invention
Fig. 1 is the carbon quantum dot appearance structure prepared in embodiment 1.
Fig. 2 is the shape appearance figure of cuprous oxide in comparative example 1.
Fig. 3 is the shape appearance figure that carbon quantum dot combined oxidation is cuprous in embodiment 2.
Specific embodiment
Invention is further described in detail in the following with reference to the drawings and specific embodiments, but protection scope of the present invention is simultaneously
It is not limited to the content.
Embodiment 1
The cuprous preparation method of carbon quantum dot combined oxidation described in the present embodiment, specifically includes the following steps:
(1) preparation of carbon quantum dot: citric acid and ethylene glycol are dissolved in the polytetrafluoroethyllining lining equipped with deionized water, will
Polytetrafluoroethyllining lining is placed in stainless steel cauldron, and 150 DEG C are heated in drying box, is cooled to after persistently keeping the temperature 360min
Room temperature, takes out the solution in reaction kettle, and 9000r/min is centrifuged 20min, then the supernatant dialysis treatment that centrifugal treating is obtained
12h；Freeze-drying (vacuum degree is less than 1Pa, and condenser temperature is 55 DEG C) obtains powder formed carbon quantum dot, as shown in Figure 1.
(2) by mantoquita, carbon quantum dot is separately added into the container for filling deionized water, and the mass ratio of mantoquita and water is 1:
50, the mass ratio of carbon quantum dot and water is then carbon quantum dot solution is slowly dripped copper salt solution magnetic agitation 1h by 1:600
Into copper salt solution, wherein the mass ratio of carbon quantum dot and mantoquita is 1:1560, is continued after stirring 10min, heating water bath to 80
DEG C, obtain carbon quantum dot-mantoquita mixed liquor.
(3) configuration quality score is 40% NaOH solution, while NaOH solution is slowly dropped into the carbon nanotube-in (2)
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in mantoquita mixed solution；Carbon quantum dot-Kocide SD in the process
Precipitating is always held at heating and magnetic agitation 10min in the water-bath that temperature is 80 DEG C, so that Kocide SD precipitating forming core is complete
Entirely.
(4) configuration quality score is 50% glucose solution, while glucose solution is slowly dropped into the carbon amounts in (3)
In sub- point-Kocide SD precipitating, it is kept always to 80 DEG C of progress magnetic agitations in water-bath, until solution colour becomes brick
Red precipitate obtains uniformly mixed carbon quantum dot-cuprous oxide mixed liquor；It filters and is placed in drying box dry
15h obtains carbon quantum dot-cuprous oxide composite powder.
It is uniform in size that the present embodiment is prepared carbon quantum dot-cuprous oxide composite powder, is tightly combined between particle, pine
It is small to fill density, pattern tends to completely, generate without impurity, cube face has seldom kick, i.e., on cuprous oxide particle
The carbon quantum dot of attachment is seldom, is difficult to observe.
Embodiment 2
The cuprous preparation method of carbon quantum dot combined oxidation described in the present embodiment, specifically includes the following steps:
(1) preparation of carbon quantum dot: citric acid and ethylene glycol are dissolved in the polytetrafluoroethyllining lining equipped with deionized water, will
Polytetrafluoroethyllining lining is placed in stainless steel cauldron, is heated to 100 DEG C in drying box, is cooled to room after persistently keeping the temperature 360min
Temperature, takes out the solution in reaction kettle, and 9000r/min is centrifuged 20min, then the supernatant dialysis treatment that centrifugal treating is obtained
12h, freeze-drying (vacuum degree is less than 1Pa, and condenser temperature is -50 DEG C) obtain powder formed carbon quantum dot.
(2) by mantoquita, carbon quantum dot is separately added into the container for filling deionized water, and the mass ratio of mantoquita and water is 1:
100, the mass ratio of carbon quantum dot and water is then carbon quantum dot solution is delayed copper salt solution magnetic agitation 0.5h by 1:1000
Slowly it drops in copper salt solution, wherein the mass ratio of carbon quantum dot and mantoquita is 1:780, is continued after stirring 5min, heating water bath is extremely
70 DEG C, obtain carbon quantum dot-mantoquita mixed liquor.
(3) configuration quality score is 50% NaOH solution, while NaOH solution is slowly dropped into the carbon nanotube-in (2)
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in mantoquita mixed solution；Carbon quantum dot-Kocide SD in the process
Precipitating is always held at heating and magnetic agitation 10min in the water-bath that temperature is 70 DEG C, so that Kocide SD precipitating forming core is complete
Entirely.
(4) configuration quality score is 50% glucose solution, while glucose solution is slowly dropped into the carbon amounts in (3)
In sub- point-Kocide SD precipitating, it is kept always to 70 DEG C of progress magnetic agitations in water-bath, until solution colour becomes brick
Red precipitate obtains uniformly mixed carbon quantum dot-cuprous oxide mixed liquor；It filters and is placed in drying box dry
12h obtains carbon quantum dot-cuprous oxide composite powder；Composite powder shape appearance figure is shown in attached drawing 3.
As shown in figure 3, to be prepared micron level carbon quantum dot-cuprous oxide composite powder uniform in size for the present embodiment,
And carbon quantum dot is more uniform to be deposited on cube cuprous oxide, and composite powder pattern is complete, and apparent density is small, not miscellaneous
Matter generates.
Embodiment 3
The cuprous preparation method of carbon quantum dot combined oxidation described in the present embodiment, specifically includes the following steps:
(1) preparation of carbon quantum dot: citric acid and ethylene glycol are dissolved in the polytetrafluoroethyllining lining equipped with deionized water, will
Polytetrafluoroethyllining lining is placed in stainless steel cauldron, is heated to 120 DEG C in drying box, is cooled to room after persistently keeping the temperature 300min
Temperature takes out the solution in reaction kettle, and 7000r/min is centrifuged 25min, then the supernatant dialysis treatment 11h that centrifugal treating is obtained,
Freeze-drying (vacuum degree is less than 1Pa, and condenser temperature is -40 DEG C) obtains powder formed carbon quantum dot.
(2) by mantoquita, carbon quantum dot is separately added into the container for filling deionized water, and the mass ratio of mantoquita and water is 1:
70, the mass ratio of carbon quantum dot and water is 1:800, then that carbon quantum dot solution is slow by copper salt solution magnetic agitation 0.5h
It drops in copper salt solution, wherein the mass ratio of carbon quantum dot and mantoquita is 1:520, is continued after stirring 5min, heating water bath to 85
DEG C, obtain carbon quantum dot-mantoquita mixed liquor.
(3) configuration quality score is 40% NaOH solution, while NaOH solution is slowly dropped into the carbon nanotube-in (2)
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in mantoquita mixed solution；Carbon quantum dot-Kocide SD in the process
Precipitating is always held at heating and magnetic agitation 20min in the water-bath that temperature is 85 DEG C, so that Kocide SD precipitating forming core is complete
Entirely.
(4) configuration quality score is 50% glucose solution, while glucose solution is slowly dropped into the carbon amounts in (3)
In sub- point-Kocide SD precipitating, it is kept always to 85 DEG C of progress magnetic agitations in water-bath, until solution colour becomes brick
Red precipitate obtains uniformly mixed carbon quantum dot-cuprous oxide mixed liquor；It filters and is placed in drying box dry
10h obtains carbon quantum dot-cuprous oxide composite powder.
The present embodiment is prepared that carbon quantum dot-cuprous oxide composite powder is uniform in size, and cube structure is more complete
And there is a little little particle protrusion on surface, that is, has a little carbon quantum dot attachment thereon, apparent density is small, generates without impurity.
Embodiment 4
The cuprous preparation method of carbon quantum dot combined oxidation described in the present embodiment, specifically includes the following steps:
(1) preparation of carbon quantum dot: citric acid and ethylene glycol are dissolved in the polytetrafluoroethyllining lining equipped with deionized water, will
Polytetrafluoroethyllining lining is placed in stainless steel cauldron, is heated to 130 DEG C in drying box, is cooled to room after persistently keeping the temperature 320min
Temperature takes out the solution in reaction kettle, and 6000r/min is centrifuged 30min, then the supernatant dialysis treatment 10h that centrifugal treating is obtained,
Freeze-drying (vacuum degree is less than 1Pa, and condenser temperature is -60 DEG C) obtains powder formed carbon quantum dot.
(2) by mantoquita, carbon quantum dot is separately added into the container for filling deionized water, and the mass ratio of mantoquita and water is 1:
80, the mass ratio of carbon quantum dot and water is 1:900, then that carbon quantum dot solution is slow by copper salt solution magnetic agitation 0.5h
It drops in copper salt solution, wherein the mass ratio of carbon quantum dot and mantoquita is 1:390, is continued after stirring 5min, heating water bath to 80
DEG C, obtain carbon quantum dot-mantoquita mixed liquor.
(3) configuration quality score is 40% NaOH solution, while NaOH solution is slowly dropped into the carbon nanotube-in (2)
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in mantoquita mixed solution；Carbon quantum dot-Kocide SD in the process
Precipitating is always held at heating and magnetic agitation 15min in the water-bath that temperature is 80 DEG C, so that Kocide SD precipitating forming core is complete
Entirely.
(4) configuration quality score is 50% glucose solution, while glucose solution is slowly dropped into the carbon amounts in (3)
In sub- point-Kocide SD precipitating, it is kept always to 80 DEG C of progress magnetic agitations in water-bath, until solution colour becomes brick
Red precipitate obtains uniformly mixed carbon quantum dot-cuprous oxide mixed liquor；It filters and is placed in drying box dry
15h obtains carbon quantum dot-cuprous oxide composite powder.
It is small that the present embodiment is prepared carbon quantum dot-cuprous oxide composite powder apparent density, generates without impurity, cube
The cuprous oxide particle surface of body shape has a large amount of kick, i.e., surface has a large amount of carbon quantum dot to adhere to, and composite powder
It is uniform in size.
Comparative example 1
The cuprous preparation method of carbon quantum dot combined oxidation described in the present embodiment, specifically includes the following steps:
(1) mantoquita is added in the container for filling deionized water, the mass ratio of mantoquita and water is 1:50, and copper salt solution magnetic force is stirred
0.5h is mixed, heating water bath obtains mantoquita mixed liquor to 80 DEG C.
(2) NaOH solution that configuration quality score is 40%, while NaOH solution is slowly dropped into the mantoquita in (1) and is mixed
Uniform Kocide SD precipitating is obtained in solution；Kocide SD precipitating is always held at the water-bath that temperature is 80 DEG C in the process
Heating and magnetic agitation 10min in pot, so that Kocide SD precipitating forming core is complete.
(3) configuration quality score is 50% glucose solution, while glucose solution is slowly dropped into the hydrogen-oxygen in (2)
Change in copper precipitating, it is kept in water-bath always to 80 DEG C of progress magnetic agitations, until solution colour becomes brick-red precipitating
, obtain uniform cuprous oxide mixed liquor；It filters and is placed in drying box dry 15h and obtain cuprous oxide powder；Its
Shape appearance figure is shown in attached drawing 2.
After can be seen that addition carbon quantum dot by the comparison with comparative example 1, cube cuprous oxide surface becomes
It is coarse, there are some tiny protrusions, these protrusions are exactly the carbon quantum dot added, also, after addition carbon quantum dot, cuprous oxide
Size is more uniform, and structure is also more complete.This is beneficial to some relevant physicochemical performances.Also, technique letter
It is single, special equipment is not needed, therefore the technology is feasible.
Claims (5)
1. a kind of preparation method that carbon quantum dot combined oxidation is cuprous, which is characterized in that specifically includes the following steps:
(1) mantoquita, carbon quantum dot are separately added into the container for filling deionized water, the mass ratio of mantoquita and water be 1:50 ~
100, the mass ratio of carbon quantum dot and water is 1:600 ~ 1000, and carbon quantum dot solution is slowly dropped in copper salt solution, continues to stir
After mixing 5 ~ 10min, heating water bath obtains carbon quantum dot-mantoquita mixed liquor to 70 DEG C ~ 85 DEG C, wherein carbon quantum dot and mantoquita
Mass ratio is 1:390 ~ 1560；
(2) NaOH solution that mass fraction is 40% ~ 50% is prepared, NaOH solution is slowly dropped into the carbon nanometer that step (1) obtains
Uniformly mixed carbon quantum dot-Kocide SD precipitating is obtained in pipe-mantoquita mixed solution；Carbon quantum dot-hydrogen-oxygen in the process
Change copper precipitating and be always held at heating and magnetic agitation in the water-bath that temperature is 70 ~ 85 DEG C, so that Kocide SD precipitates forming core
Completely；
(3) it prepares mass fraction and is 50% ~ 60% glucose solution, while glucose solution is slowly dropped into step (2) and is obtained
Carbon quantum dot-Kocide SD precipitating in, being always held at temperature is to carry out magnetic agitation in 70 ~ 85 DEG C of water-bath,
Until solution colour becomes brick-red precipitating, uniformly mixed carbon quantum dot-cuprous oxide mixed liquor is obtained, filters drying
After obtain carbon quantum dot-cuprous oxide composite powder.
2. the cuprous preparation method of carbon quantum dot combined oxidation according to claim 1, it is characterised in that: step (1) is described
Carbon quantum dot the preparation method comprises the following steps: being dissolved in citric acid and ethylene glycol in the polytetrafluoroethyllining lining equipped with deionized water, will
Polytetrafluoroethyllining lining is placed in stainless steel cauldron, is heated to 100 ~ 150 DEG C, is persistently kept the temperature 300 ~ 360min, is then cooled down
To room temperature, the solution in reaction kettle is taken out, 6000 ~ 9000r/min is centrifuged 20 ~ 30min, then the supernatant that centrifugal treating is obtained
10 ~ 12h of dialysis treatment obtains powder formed carbon quantum dot after freeze-drying.
3. the preparation method that carbon quantum dot according to claim 2 strengthens Cu-base composites, it is characterised in that:
The vacuum degree of freezing dry process is less than 1Pa, and condenser temperature is -60 DEG C ~ -40 DEG C.
4. the cuprous preparation method of carbon quantum dot combined oxidation according to claim 1, it is characterised in that: institute in step (1)
The mantoquita stated be one of copper acetate, copper stearate, copper sulphate, copper nitrate, sodium ethylene diamine tetracetate copper, EDTA copper sodium or
A variety of configure according to arbitrary proportion of person forms.
5. the cuprous preparation method of carbon quantum dot combined oxidation according to claim 1, it is characterised in that: done in step (3)
Dry temperature is 60 ~ 70 DEG C, and drying time is 10 ~ 15h.
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| CN111607387A (en) * | 2020-01-03 | 2020-09-01 | 华南师范大学 | Photocatalytic microsphere motor based on carbon dots and preparation method and application thereof |
| CN112536034A (en) * | 2020-11-22 | 2021-03-23 | 重庆交通大学 | CQDS/CuO@Cu2Preparation method of O-micron balls |
| CN113186417A (en) * | 2021-03-19 | 2021-07-30 | 昆明理工大学 | Preparation method of graphene oxide-carbon quantum dot reinforced copper-based composite material |
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| CN111607387A (en) * | 2020-01-03 | 2020-09-01 | 华南师范大学 | Photocatalytic microsphere motor based on carbon dots and preparation method and application thereof |
| CN111607387B (en) * | 2020-01-03 | 2023-07-25 | 华南师范大学 | Photocatalytic microsphere motor based on carbon dots and preparation method and application thereof |
| CN111589444A (en) * | 2020-04-30 | 2020-08-28 | 昆明理工大学 | Noble metal quantum dot and preparation method and application thereof |
| CN112536034A (en) * | 2020-11-22 | 2021-03-23 | 重庆交通大学 | CQDS/CuO@Cu2Preparation method of O-micron balls |
| CN113186417A (en) * | 2021-03-19 | 2021-07-30 | 昆明理工大学 | Preparation method of graphene oxide-carbon quantum dot reinforced copper-based composite material |
| CN114958037A (en) * | 2022-05-30 | 2022-08-30 | 湖南金天铝业高科技股份有限公司 | Preparation method of carbon quantum dot coated carbonaceous material, composite material and application |
| CN114958037B (en) * | 2022-05-30 | 2023-09-05 | 湖南湘投轻材科技股份有限公司 | Preparation method of carbon quantum dot coated carbonaceous material, composite material and application |
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Application publication date: 20191022 |