CN101905899B - Method for preparing ordered nano cuprous oxide polycrystalline powder - Google Patents
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Abstract
The invention discloses a method for preparing ordered nano cuprous oxide polycrystalline powder. The method comprises the following steps of: (1) dissolving copper salt into water to obtain copper salt solution, preparing sodium dodecyl sulfate-reducing agent-alcohol solution, then mixing the two kinds of solution, and preserving heat of the mixed solution for later use; (2) dissolving precipitant into water to obtain precipitant solution, and then adding alcohol into the precipitant solution to form precipitant-alcohol-water mixed solution; (3) preheating and dissolving the mixed solution prepared in the step (2), quickly adding the mixed solution into a flask in the step (1), heating the mixed solution to a reflux temperature, and refluxing and reacting the mixed solution for 7 to 48 hours; and (4) standing the obtained product, and washing and drying the sediment to obtain the ordered nano cuprous oxide polycrystalline powder product. The obtained cuprous oxide powder is high ordered (namely space symmetry) nano laminar polycrystalline structural pure cuprous oxide, the adopted low-toxicity sodium dodecyl sulfate surfactant is favorable for non-toxic production and environmental protection, and the raw materials are common chemical reagents and are cheap and easily obtained.
Description
Technical field
Technical scheme of the present invention relates to the lower valency oxide compound of copper, specifically a kind of preparation method of ordered nano cuprous oxide polycrystalline powder.
Background technology
Red copper oxide is a kind of important inorganic oxide, and copper atom by 88.1% and 11.9% Sauerstoffatom are formed.It is the lower valency oxide compound of copper, and English name is Cuprous oxide or Copper (I) Oxide.Molecular formula is Cu
2O, molecular weight are 143.09, density 6.0g/cm
3, fusing point is 1235 ℃.Red copper oxide is generally red or orange-yellow octahedral isometric system crystalline powder, because the difference of preparation method and particle size, can show as multiple colors such as Huang, orange, red or purple.
Red copper oxide is having potential to use as a kind of p type, semiconductor material with unique light, magnetism characteristic aspect solar energy converting, electronics, magnetic storing unit, bio-sensing and the catalysis.The Red copper oxide band gap width is 2.1eV, and exciton can transmit in monocrystalline continuously, makes it have higher specific absorbance, becomes the important materials of making photovoltaic converter.In addition, because quantum size effect, along with reducing of particle diameter, Red copper oxide shows peculiar optics, electricity and photoelectrochemistry character and catalytic activity, discovers Cu recently
2The submicron particles of O can be used for the negative material of lithium cell; The Red copper oxide of submicron order has special photocatalytic activity, can under the visible light effect, generate hydrogen and oxygen by photodissociation water, and this provides important thinking for the exploitation of following hydrogen energy source.
Red copper oxide has been used to prepare ship bottom anti-fouling paint at present, to kill rudimentary marine animal, hull below the sea line and hull bottom is shielded; As pottery and enamelled tinting material, the staining agent of red glass; In also producing as the organosilicon resin, the hydrogenation synthetic catalyzer of monochloro methane and silica flour.In addition, also be used for making various mantoquitas, analytical reagent, sterilant and be used for rectification in electrical equipment industry and electroplate.Therefore, research Red copper oxide has very important practical sense.
In recent years, a lot of work are devoted to control synthetic Cu
2O micron and nanocrystalline structure.The preparation method mainly contains several kinds of hydrothermal method, liquid phase method and electrochemical processes etc.Simultaneously, for the Cu of different-shape
2The O nanocrystal also has report, like nano wire, nanometer rod, nanocubes and nanometer octahedron etc.
Because the raw material and the equipment that adopt are not quite similar, liquid phase method is produced Cu
2The technology of O has a variety of.People such as Wei adopt hydrothermal method in 140 ℃ NaOH and ethanolic soln, to reduce CuSO
4Synthesized Cu
2The O nanometer rod (WEI M, LUN N, MA X.A simple solvothermal reduction route to copper and cuprous oxide [J] .Mater Lett, 2007,61:2147-2150.).People such as Chen adopt oil/water microemulsion method in the presence of nonionogenic tenside, to control reduction Cu
2+Prepared nanometer Cu
2O (CHEN Q, SHEN X, GAO H.Formation of nanoparticles inwater-in-oil microemulsions controlled by the yield of hydrated electron:the controlledreduction of Cu
2+[J] .J Colloid Interface Sci, 2007,308:491-499.).People such as Luo adopt liquid phase reduction in the presence of nonionogenic tenside Triton X-100, reduce CuCl with glucose
2Method prepared Cu
2O nanometer monocrystalline pipe (LUO F, WU D, GAO L.Shape-controlled synthesis of Cu
2O nanocrystalsassisted by Triton X-100 [J] .J Cryst Growth, 2005,285:534-540.).Wang etc. are that template has been synthesized the item catenate one dimension Cu that cetyl trimethylammonium bromide (CTAB) coats with the DNA chain
2O nanostructure (WANG L, WEI G, OU B.Electrostatic assembly of Cu
2O nanoparticles on DNA templates [J] .ApplSurf Sci, 2006,252:2711-2716.).Yu Ying etc. utilize the tensio-active agent cetyl trimethylammonium bromide to be soft template, have prepared uniform nanometer Cu with chemical precipitation method
2O whisker (ZHANG H, GOODNER D M, BEDZYK M J.Formation and kinetics study of cuprous oxide nanodots on LaAlO
3(001) [J] .Chem Phys Lett, 2004,395 (4-6): 296-301.).Borgohain etc. make negative electrode with copper electrode in electrolyzer, platinum electrode is made anode, CH
3The additional proportion of CN and THF is 4: 1, and supporting electrolyte four n-octyl bromination ammonia (TOAB) have obtained pure Cu as stablizer
2O nanocrystalline (BORGOHAIN K, MURASE N, MAHAMUNI S.Synthesis and properties of Cu
2O quantum particles [J] .J Appl Phys, 2002,92 (3): 1292-1297.).These methods all can not obtain the Red copper oxide of ordered laminar nano structure.
Summary of the invention
Technical problem to be solved by this invention is: the preparation method that a kind of ordered laminar nano structure cuprous oxide polycrystalline powder is provided; Adopting the AS sodium laurylsulfonate is template; In alcohol-water or terepthaloyl moietie-aqueous systems with circumfluence method preparation have high-sequential, the cuprous oxide polycrystalline powder of the symmetry of having living space nanometer laminated structure, better crystallinity degree, to overcome the defective that existing method can not obtain ordered laminar nano structure Red copper oxide.
The present invention solves this technical problem the technical scheme that is adopted:
A kind of preparation method of ordered nano cuprous oxide polycrystalline powder the steps include:
(1) mantoquita is soluble in water; Make the copper salt solution that concentration is 0.000667 mole of copper ion/ml water, in addition sodium laurylsulfonate and reductive agent are dissolved in the alcohol, make sodium laurylsulfonate-reductive agent-alcoholic solution; Its concentration is that every milliliter of alcohol contains 0.025～0.2 gram sodium laurylsulfonate and 0.0155～0.135 gram reductive agent; With its preheating dissolving, get 30 parts of copper salt solutions and mix with 20 parts of sodium laurylsulfonate-reductive agent-alcoholic solutions then, adding has in the flask of reflux; Stir heat preservation for standby use;
Described reductive agent is glucose, S-WAT or Hydrazine Hydrate 80;
(2) precipitation agent is dissolved in the water, making concentration is the precipitant solution of 0.053～0.112 gram precipitation agent/ml water, gets 30 parts, adds 1～100 part alcohol again, is mixed with precipitation agent-alcohol-water mixed liquid, for use;
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 7～48 hours stops to stir and heating;
(4) will go up the step products therefrom again and at room temperature leave standstill 0～15 hour, and obtain brick-red deposition, washing then again through suction filtration, with the brick-red deposition oven dry of gained, obtains the product ordered nano cuprous oxide polycrystalline powder.
The umber of said components is volume parts, and used volume unit is identical in each step.
Mantoquita described in the top step (1) is cupric chloride, copper sulfate or neutralized verdigris;
Alcohol described in top step (1) and (2) is ethanol or terepthaloyl moietie.
When the reductive agent in the top step (1) was glucose, reductive agent was 0.09～0.135 gram glucose/milliliter alcohol with the proportioning of alcohol;
When the reductive agent in the top step (1) was S-WAT, reductive agent was pure with proportioning 0.063～0.0945 gram S-WAT/milliliter of alcohol
When the reductive agent in the top step (1) was Hydrazine Hydrate 80, reductive agent was pure with proportioning 0.0155～0.0235 gram Hydrazine Hydrate 80 (massfraction the is 80%)/milliliter of alcohol.
Precipitation agent described in the top step (2) is sodium hydroxide or Pottasium Hydroxide;
When the precipitation agent described in the top step (2) was sodium hydroxide, the concentration of precipitant solution was 0.053～0.08 gram sodium hydroxide/ml water;
When the precipitation agent described in the top step (2) was Pottasium Hydroxide, the concentration of precipitant solution was 0.075～0.112 gram Pottasium Hydroxide/ml water;
The invention has the beneficial effects as follows:
1. the resulting ordered nano cuprous oxide polycrystalline powder of the inventive method is that to have the pure zirconia of nano lamellar polycrystalline structure of high-sequential (being spatial symmetry) cuprous, and promptly the cuprous nano wafer of two-dimensional growth forms along its normal direction ordered arrangement.The repeat cycle of this laminate structure is about 2.75 nanometers, and the degree of order of the nanostructure of the resulting ordered nano cuprous oxide polycrystalline powder of the inventive method (spatial symmetry) is very high.As shown in Figure 1; The medium and small angle part of XRD spectra (2 θ=0～10 °) exist 3 sharply, the characteristic small-angle diffraction of layered nano-structure clearly; XRD spectra small-angle diffraction representative among this and patent of invention " preparation method of the ordered nano hydroxyl apatite polycrystal powder " CN101058416A be same class formation; Be about 2.75 nanometers through the repeat cycle that calculates this laminate structure, diffraction peak shows that product is that cubic phase oxygenization is cuprous to wide-angle part (2 θ=10～80 °), and diffraction peak is very clear, sharp-pointed; Explain that Red copper oxide percent crystallinity is fine, and do not have the diffraction peak of other dephasigns to occur.
The Red copper oxide of ordered laminar nano structure is spatially assembled by nano-sheet Red copper oxide structural unit in order, has character and catalytic activitys such as peculiar light, electricity, magnetic.In addition, open layered nano-structure provides parallel cuprous oxide crystal and open duct alternately, for the preparation nano composite material provides brand-new experiment porch.
2. in the inventive method, adopt the low AS sodium laurylsulfonate of toxicity, help toxicological harmless production and environment protection.
3. the raw material cupric chloride, copper sulfate, the neutralized verdigris that adopt of the present invention; Glucose (C
6H
12O
6), S-WAT (Na
2SO
3), Hydrazine Hydrate 80 (massfraction is 80%); Sodium hydroxide (NaOH), Pottasium Hydroxide (KOH); Ethanol, terepthaloyl moietie; Sodium laurylsulfonate (SDS) all belongs to general chemistry reagent, and is cheap and easy to get.
Description of drawings
Below in conjunction with accompanying drawing and embodiment the present invention is further specified.
Fig. 1 is the XRD spectra of embodiment 1 laminate Red copper oxide powder.
Fig. 2 is the stereoscan photograph of embodiment 1 laminate Red copper oxide powder.
Embodiment
Embodiment 1
(1) the 0.02mol cupric chloride is dissolved in the beaker that fills 30mL water; In addition 1g sodium laurylsulfonate and 2.4g glucose are dissolved in and make sodium laurylsulfonate glucose ethanolic soln mixed solution in the beaker that fills the 20mL ethanolic soln; Then its preheating dissolving back is mixed; Adding has in the flask of reflux, stirs heat preservation for standby use.
(2) with the 1.6g dissolution of sodium hydroxide in 30mL water, add 10mL ethanol again, be mixed with sodium hydroxide-second-water alcohol mixed solution, for use.
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 48h stops to stir and heating.
(4) will go up the step products therefrom again and at room temperature leave standstill 15h, obtain brick-red deposition, then it washed three times with deionized water; Again through suction filtration; Brick-red being deposited in 60 ℃ the vacuum drying oven of gained dried, and the time is 2.5h, obtains product ordered nano cuprous oxide polycrystalline powder 1.15g.
Through the XRD test, the product ordered nano cuprous oxide polycrystalline powder is the nano lamellar Red copper oxide of high-sequential (being spatial symmetry).Small-angle diffraction peak (100) among Fig. 1, (200), (300) explain that there is high-sequential (being spatial symmetry) layered nano-structure in the product ordered nano cuprous oxide polycrystalline powder; Wide-angle diffraction peak among Fig. 1 shows that the product ordered nano cuprous oxide polycrystalline powder is the cuprous crystal of pure zirconia, does not contain other dephasign; These diffraction peaks are clear, sharp-pointed simultaneously, explain that the percent crystallinity of this nano cuprous oxide is fine.
Observed the product ordered nano cuprous oxide polycrystalline powder through the SEM test again.Fig. 2 is the SEM photo of product ordered nano cuprous oxide polycrystalline powder, can find out that this powder is particulate state, and particle diameter is about 100～400nm.
Embodiment 2, example 3, example 4, example 5
The time of refluxing is changed the operation in the step (3) among the embodiment 1 into 7h, 12h, 24h, 36h respectively, other operations is all identical with embodiment 1, obtains product with embodiment 1.
Embodiment 6
With step (1) C among the embodiment 1
6H
12O
6Consumption change 1.8g into, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 7
With step (1) C among the embodiment 1
6H
12O
6Consumption change 2.7g into, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 8
Change the consumption of step (1) SDS among the embodiment 1 into 0.5g, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 9
Change the consumption of step (1) SDS among the embodiment 1 into 4g, other steps obtain product with embodiment 1 with embodiment 1.
Change the consumption of step (2) NaOH among the embodiment 1 into 2.4g, other steps obtain product with embodiment 1,1.23g with embodiment 1.
Embodiment 11
(1) 0.02mol copper sulfate is dissolved in the beaker that fills 30mL water; In addition 1g sodium laurylsulfonate and 2.4g glucose are dissolved in and make sodium laurylsulfonate glucose ethanolic soln mixed solution in the beaker that fills the 20mL ethanolic soln; Then its preheating dissolving back is mixed; Adding has in the flask of reflux, stirs heat preservation for standby use.
(2) 2.24g KOH is dissolved in the 30mL water, adds 10mL ethanol again, be mixed with potassium hydroxide-ethanol-water mixed liquid, for use.
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 48h stops to stir and heating.
(4) will go up the step products therefrom again and at room temperature leave standstill 15h, obtain brick-red deposition, then it washed three times with deionized water; Again through suction filtration; Brick-red being deposited in 60 ℃ the vacuum drying oven of gained dried, and the time is 2.5h, obtains product ordered nano cuprous oxide polycrystalline powder 1.16g.
Embodiment 12
Change the consumption of step (2) KOH among the embodiment 11 into 3.36g, other steps obtain product with embodiment 11,1.22g with embodiment 11.
Embodiment 13
Change step (1) cupric chloride among the embodiment 1 into neutralized verdigris, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 14
Change step (2) consumption of ethanol among the embodiment 1 into 40mL, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 15
Change step (2) consumption of ethanol among the embodiment 11 into 40mL, other steps obtain product with embodiment 11 with embodiment 11.
Embodiment 16
Change step (2) consumption of ethanol among the embodiment 13 into 40mL, other steps obtain product with embodiment 13 with embodiment 13.
Embodiment 17
Change step (1) glucose and consumption thereof among the embodiment 1 into the 1.26g S-WAT, other steps obtain product with embodiment 1 with embodiment 1.
Embodiment 18
With step (1) Na among the embodiment 17
2SO
3Consumption change 1.89g into, other steps obtain product with embodiment 17 with embodiment 17.
Embodiment 19
Changing step (2) glucose and consumption thereof among the embodiment 1 into the 0.31g massfraction is 80% Hydrazine Hydrate 80, and other steps obtain product with embodiment 1 with embodiment 1.
Change the consumption of step (1) Hydrazine Hydrate 80 among the embodiment 19 into 0.47g, other steps obtain product with embodiment 19 with embodiment 19.
Embodiment 21
(1) the 0.02mol cupric chloride is dissolved in the beaker that fills 30mL water; In addition 1g sodium laurylsulfonate and 2.4g glucose are dissolved in and make sodium laurylsulfonate glucose ethanolic soln mixed solution in the beaker that fills the 20mL ethanolic soln; Then its preheating dissolving back is mixed; Adding has in the flask of reflux, stirs heat preservation for standby use.
(2) with the 1.6g dissolution of sodium hydroxide in 30mL water, add 100mL ethanol again, be mixed with sodium hydroxide-alcohol-water mixed solution, for use.
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 48h stops to stir and heating.
(4) will go up the step products therefrom again and at room temperature leave standstill 0h, obtain brick-red deposition, then it washed three times with deionized water; Again through suction filtration; Brick-red being deposited in 60 ℃ the vacuum drying oven of gained dried, and the time is 2.5h, obtains product ordered nano cuprous oxide polycrystalline powder 1.21g.
Embodiment 22
(1) the 0.02mol cupric chloride is dissolved in the beaker that fills 30mL water; In addition 1g sodium laurylsulfonate and 2.4g glucose are dissolved in and make sodium laurylsulfonate glucose ethanolic soln mixed solution in the beaker that fills the 20mL ethanolic soln; Then its preheating dissolving back is mixed; Adding has in the flask of reflux, stirs heat preservation for standby use.
(2) with the 1.6g dissolution of sodium hydroxide in 30mL water, add 1mL ethanol again, be mixed with the sodium hydroxide alcohol mixeding liquid, for use.
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 48h stops to stir and heating.
(4) will go up the step products therefrom again and at room temperature leave standstill 3h, obtain brick-red deposition, then it washed three times with deionized water; Again through suction filtration; Brick-red being deposited in 60 ℃ the vacuum drying oven of gained dried, and the time is 2.5h, obtains product ordered nano cuprous oxide polycrystalline powder 1.14g.
Embodiment 23-44
Change step (1), (2) ethanol among the embodiment 1-22 into terepthaloyl moietie, other steps obtain product with embodiment 1-22 with embodiment 1-22.
Claims (8)
1. the preparation method of an ordered nano cuprous oxide polycrystalline powder, it is following to it is characterized by step:
(1) mantoquita is soluble in water; Make the copper salt solution that concentration is 0.000667 mole of copper ion/ml water, in addition sodium laurylsulfonate and reductive agent are dissolved in the alcohol, make sodium laurylsulfonate-reductive agent-alcoholic solution; Its concentration is that every milliliter of alcohol contains 0.025～0.2 gram sodium laurylsulfonate and 0.0155～0.135 gram reductive agent; With its preheating dissolving, get 30 parts of copper salt solutions and mix with 20 parts of sodium laurylsulfonate-reductive agent-alcoholic solutions then, adding has in the flask of reflux; Stir heat preservation for standby use;
Described reductive agent is glucose, S-WAT or Hydrazine Hydrate 80;
(2) precipitation agent is dissolved in the water, making concentration is the precipitant solution of 0.053～0.112 gram precipitation agent/ml water, gets 30 parts, adds 1～100 part alcohol again, is mixed with precipitation agent-pure mixed solution, for use;
(3) with liquid mixture prepared preheating dissolving in the step (2), join fast in the flask in the step (1), be warming up to reflux temperature under the nitrogen protection, back flow reaction 7～48 hours stops to stir and heating;
(4) will go up the step products therefrom again and at room temperature leave standstill 0～15 hour, and obtain brick-red deposition, washing then again through suction filtration, with the brick-red deposition oven dry of gained, obtains the product ordered nano cuprous oxide polycrystalline powder;
Wherein, the precipitation agent described in the step (2) is sodium hydroxide or Pottasium Hydroxide;
The umber of said components is volume parts, and used volume unit is identical in each step.
2. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, it is characterized by the mantoquita described in the step (1) is cupric chloride, copper sulfate or neutralized verdigris.
3. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, it is characterized by the alcohol described in step (1) and (2) is ethanol or terepthaloyl moietie.
4. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, when it is characterized by reductive agent in the step (1) and being glucose, reductive agent is that 0.09～0.135 gram glucose/milliliter is pure with the proportioning of alcohol.
5. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, when it is characterized by reductive agent in the step (1) and being S-WAT, reductive agent is pure with proportioning 0.063～0.0945 gram S-WAT/milliliter of alcohol.
6. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, when it is characterized by reductive agent in the step (1) and being Hydrazine Hydrate 80, reductive agent is pure with proportioning 0.0155～0.0235 gram Hydrazine Hydrate 80/milliliter of alcohol, and the massfraction of Hydrazine Hydrate 80 is 80%.
7. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, when it is characterized by the precipitation agent described in the step (2) and being sodium hydroxide, the concentration of precipitant solution is 0.053～0.08 gram sodium hydroxide/ml water.
8. the preparation method of ordered nano cuprous oxide polycrystalline powder according to claim 1, when it is characterized by the precipitation agent described in the step (2) and being Pottasium Hydroxide, the concentration of precipitant solution is 0.075～0.112 gram Pottasium Hydroxide/ml water.
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| CN106315662B (en) * | 2016-08-04 | 2018-04-17 | 浙江理工大学 | A kind of cuprous particle of porous oxidation and preparation method thereof |
| CN106698498B (en) * | 2016-11-18 | 2019-04-23 | 沈阳师范大学 | A kind of preparation method of nano cuprous oxide catalyst |
| CN111482175B (en) * | 2020-05-09 | 2022-10-28 | 中国科学技术大学 | Preparation method of copper/cuprous oxide heterojunction nanosheet catalyst |
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