CN104016400B - Grade cuprous oxide particle and synthetic method thereof - Google Patents
Grade cuprous oxide particle and synthetic method thereof Download PDFInfo
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Abstract
The invention belongs to the synthesis technical field of Red copper oxide, be specifically related to a kind of grade cuprous oxide particle and synthetic method thereof.By Cu
2+the reaction system that solution is formed is made through reduction reaction, under this reaction system is in alkaline condition, and contains Cu in reaction system
2+be reduced into Cu
+and be used as nucleation template to form the biomolecules of grade cuprous oxide particle, the juice of described biomolecules for being formed by vegetables or fruit.All contain the biomolecules such as protein, amino acid, VITAMIN and polysaccharide element in Fructus Citri grandis juice, juice of white turnip, containing atoms such as electronegative O, N in these molecules, they can attract Cu
2+, nucleation site is provided, and regulating and controlling effect is played to the process of growth of cuprous oxide crystal, and the vitamins C etc. in juice with reductibility can be reduced into univalent copper ion bivalent cupric ion in the basic conditions, form Red copper oxide.
Description
Technical field
The invention belongs to the synthesis technical field of Red copper oxide, be specifically related to a kind of grade cuprous oxide particle and synthetic method thereof.
Background technology
After second industrial revolution, industrial development is rapid, and especially chemical engineering industry, prospect is considerable.While bringing huge economic benefit, environmental pollution also becomes one of the problem of 21 century headache the most gradually.Comply with the epoch and raw photocatalysis technology has brought hope undoubtedly.Announce Cu from Ikeda first time in 1998
2o can after generation of hydrogen by dissociation of water and oxygen as photocatalyst, Cu
2o is taken seriously as the performance of photocatalyst and becomes the focus studied in the world.
Red copper oxide, oxide compound, copper is wherein monovalence, is generally red brown solid, and the organic solvent such as water-soluble and alcohol, is easily oxidized to cupric in acid condition, in liquor ammoniae fortis, easily forms colourless title complex hardly.Red copper oxide is a kind of important p-type semiconductor material, and its energy level difference is about 2.2eV, is compared to TiO
23.2eV, much lower, electron-hole pair can be produced under the radiation of sunlight completely, cause light-catalyzed reaction.And diameter is better at the catalytic effect of the Red copper oxide of nanoparticle level, because it has quantum size effect, make its valence band and conduction level become discrete energy levels, energy gap will broaden, and valence band current potential can become corrigendum, and conduction band price can become more negative.In other words be exactly that Nano semiconductor particles has stronger oxidation capacity and reducing power, therefore a lot of expert thinks that nano cuprous oxide can replace the photodissociation catalyzer that titanium dioxide becomes a new generation.
Red copper oxide, except being widely used in photodissociation catalyzer, also has application prospect in antifouling, sterilant, eelctro-catalyst etc.
The preparation about grade cuprous oxide known at present, mainly contain solid-phase synthesis, hydrothermal method, sedimentation etc., the inadequate environmental protection of ubiquity agents useful for same, cannot to regulate and control Red copper oxide size and pattern, because the grade cuprous oxide of more small scale cannot be obtained to such an extent as to cannot play the technological deficiencies such as its chemical property better.
Summary of the invention
For problems of the prior art, an object of the present invention is the synthetic method providing a kind of grade cuprous oxide particle, this synthetic method is by introducing biomolecules, realization carries out Effective Regulation to the size of cuprous oxide particle during synthesis and pattern, and obtains the less grade cuprous oxide particle of yardstick.
For achieving the above object, present invention employs following technical scheme: a kind of synthetic method of grade cuprous oxide particle, by Cu
2+the reaction system that solution is formed is made through reduction reaction, under this reaction system is in alkaline condition, and contains Cu in reaction system
2+be reduced into Cu
+and be used as nucleation template to form the biomolecules of grade cuprous oxide particle, the juice of described biomolecules for being formed by vegetables or fruit.
As grade cuprous oxide particle synthetic method further preferably, described juice is Fructus Citri grandis juice and/or juice of white turnip.
As the further improvement of the synthetic method of grade cuprous oxide particle, by juice, alkali lye and Cu
2+solution mixing and stirring, Cu
2+and the mol ratio between the OH-in alkali lye is 1:2 ~ 4, in 30 ~ 60 DEG C of reaction 0.1 ~ 1h; Cool, hocket centrifugation and carrying out washing treatment, dry obtained grade cuprous oxide particle.
As the further improvement of the synthetic method of grade cuprous oxide particle, described Cu
2+solution is copper-bath, and described alkali lye is sodium hydroxide solution.
As the further improvement of the synthetic method of grade cuprous oxide particle, the preparation method of described juice is: shaddock and/or white turnip are cleaned peeling, the pulp that 50 ~ 200g removes the peel is put into mortar, hockets and grind and filter at least one times, obtain juice.
The biomolecules such as protein, amino acid, VITAMIN, polysaccharide element and carotene are all contained in Fructus Citri grandis juice, juice of white turnip.Containing atoms such as electronegative O, N in these molecules, they can attract Cu
2+, nucleation site is provided, and regulating and controlling effect is played to the process of growth of cuprous oxide crystal, and the vitamins C, amino acid etc. in juice with reductibility can be reduced into univalent copper ion bivalent cupric ion in the basic conditions, form Red copper oxide.
In order to inquire into the mechanism that cuprous oxide particle is formed in vegetable and fruit juice, existing infrared spectrum characterization is carried out to two kinds of vegetable and fruit juice, with the organic components that initial analysis is contained in them.Dropped on a small amount of KBr solid by prepare according to aforesaid method two kinds of juice, dry rear compressing tablet, carry out examination of infrared spectrum, infrared spectrogram refers to Fig. 1 a ~ 1b.By analysis chart 1a ~ 1b and documents and materials, can find out the mainly vitamins C with reductibility, bivalent cupric ion is reduced into monovalence by vitamins C in the basic conditions.Meanwhile, the amino acid and protein containing some reductibilities in juice, has a certain impact to the formation of Red copper oxide.In addition, in juice, there is a large amount of biomolecules, act as the effect of soft template, make reduzate Red copper oxide define the spherical of nano-scale or spherical particle.
Another object of the present invention is to provide two kinds of grade cuprous oxide particles prepared according to aforesaid method, this grade cuprous oxide particle is less due to yardstick, therefore can play better effect in the field such as photodissociation catalyzer, antifouling, sterilant, eelctro-catalyst.
When juice is chosen as Fructus Citri grandis juice, described grade cuprous oxide particle is diametrically 100 ~ 500nm, the inner spherical or spherical particle shape for hollow structure, and surface that is spherical or spherical particle has the circular opening that diameter is 50 ~ 100nm.
When juice is chosen as juice of white turnip, described grade cuprous oxide particle is diametrically the spherical grain shape of 0.5 ~ 1 μm.
Grade cuprous oxide particle of the present invention and synthetic method thereof, beneficial effect compared with prior art shows:
1), known by using scanning electronic microscope, infrared spectrometer, transmission electron microscope and X-ray diffractometer to carry out sign respectively to obtained grade cuprous oxide particle, biomolecules plays a part regulation and control to the size of cuprous oxide particle and pattern, containing atoms such as electronegative O, N in these molecules, they can attract Cu
2+, nucleation site is provided, and regulating and controlling effect is played to the process of growth of cuprous oxide crystal, and the vitamins C etc. in juice with reductibility can be reduced into univalent copper ion bivalent cupric ion in the basic conditions, form Red copper oxide.
2) when, juice is chosen as Fructus Citri grandis juice, the grade cuprous oxide particle of synthesis is diametrically 100 ~ 500nm, the inner spherical or spherical particle shape for hollow structure, and surface that is spherical or spherical particle has the circular opening that diameter is 50 ~ 100nm.When juice is chosen as juice of white turnip, the grade cuprous oxide particle of synthesis is diametrically the spherical grain shape of 0.5 ~ 1 μm.It can thus be appreciated that, by adding vegetable and fruit juice, can realize during synthesis carrying out Effective Regulation to the size of cuprous oxide particle and pattern, and obtaining the less grade cuprous oxide particle of yardstick.And then enable it play better effect in photodissociation catalyzer, antifouling, the known art such as sterilant, eelctro-catalyst, and numerous new opplication will certainly be caused in other known and unknown fields.
3), synthesis technique has simple to operation, the feature such as scientific and efficient, starting material are inexpensive, preparation cost is low, environmental protection, very easily in the commercial applications of industrialized production and grade cuprous oxide particle.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, optimal way of the present invention is described in further detail.
Fig. 1 a ~ 1b is the result using the Fourier transform infrared spectrometer that model is AVATAR-380 type to characterize to two kinds of vegetable and fruit juice.Fig. 1 a ~ Fig. 1 b is followed successively by the infrared spectrogram of Fructus Citri grandis juice, juice of white turnip.
Fig. 2 a1 ~ 2b2 is the result using the scanning electron microscope that model is S-3400 to characterize to obtained target product.Fig. 2 a1 is for adding the SEM figure of target product synthesized by Fructus Citri grandis juice, and Fig. 2 a2 is the SEM figure of the high magnification figure of Fig. 2 a1, Fig. 2 b1 target product synthesized by interpolation juice of white turnip, and Fig. 2 b2 is the high magnification figure of Fig. 2 b1.
Fig. 3 a ~ 3b is the result using the X-ray diffractometer that model is D8ADVANCE to characterize to obtained target product.Fig. 3 a ~ Fig. 3 b is followed successively by the X-ray diffractogram adding target product synthesized by Fructus Citri grandis juice, juice of white turnip.
Fig. 4 a ~ 4b is the result using the Fourier transform infrared spectrometer that model is AVATAR-380 type to characterize to obtained target product.Fig. 4 a ~ 4b is followed successively by the infrared spectrogram of adding target product synthesized by Fructus Citri grandis juice, juice of white turnip.
Fig. 5 a ~ 5d is transmission electron microscope and electron-diffraction diagram to adding target product synthesized by Fructus Citri grandis juice.Fig. 5 a ~ Fig. 5 c is respectively the transmission electron microscope picture of different multiplying, and Fig. 5 d is selected area electron diffraction figure.
Embodiment
Embodiment 1
Adopt Fructus Citri grandis juice synthesis nano cuprous oxide particle
1, the producing of Fructus Citri grandis juice
Get the fresh shaddock one that market is bought, peeling, leaves and takes pulp for subsequent use.Take 100g grapefruit flesh to grind several times in mortar, then grinding product is carried out suction filtration and obtain shaddock juice, pour in Erlenmeyer flask and save backup.
2, the preparation of solution
1., accurately take anhydrous cupric sulfate solid 12.8480g to dissolve in beaker, and in 250mL volumetric flask constant volume, be mixed with the copper-bath of 0.2mol/L.
2., accurately take NaOH solid 3.997g to dissolve in beaker, and in 250mL volumetric flask constant volume, be mixed with the NaOH solution of 0.4moL/L.
3, the synthesis of grade cuprous oxide particle
Get 75mL0.2mol/L copper-bath in 250mL large beaker, add 75mL shaddock juice wherein, then the sodium hydroxide solution of 75mL0.4mol/L is added, then magneton is added, be placed in magnetic stirring apparatus and stir, and temperature is transferred to 60 DEG C, rotating speed be transferred to 14 turns/min, 25min after, stop stirring, after taking out solution cool to room temperature, carry out centrifugal with whizzer, rotating speed is transferred to 3000 turns/min, centrifugal 10min, afterwards supernatant liquid is poured out, add ethanol in proper amount washing precipitation, until supernatant becomes colorless.Finally precipitation is put in an oven (80 DEG C) to dry.
Embodiment 2
Adopt juice of white turnip synthesis nano cuprous oxide particle
1, the producing of juice of white turnip
Get the fresh white turnip one that market is bought, peeling, leaves and takes pulp for subsequent use.Take 200g white turnip pulp to grind several times in mortar, then grinding product is carried out suction filtration and obtain white turnip juice, pour in Erlenmeyer flask and save backup.
2, the preparation of solution
1., accurately take anhydrous cupric sulfate solid 25.6960g to dissolve in beaker, and in 250mL volumetric flask constant volume, be mixed with the copper-bath of 0.2mol/L.
2., accurately take NaOH solid 7.9940g to dissolve in beaker, and in 250mL volumetric flask constant volume, be mixed with the NaOH solution of 0.8mol/L.
3, the synthesis of grade cuprous oxide particle
Get 10mL0.2mol/L copper-bath in 250mL large beaker, add 20mL white turnip juice wherein, then the sodium hydroxide solution of 10mL0.4mol/L is added, then magneton is added, be placed in magnetic stirring apparatus and stir, and temperature is transferred to 30 DEG C, rotating speed be transferred to 14 turns/min, 25min after, stop stirring, after taking out solution cool to room temperature, carry out centrifugal with whizzer, rotating speed is transferred to 5000 turns/min, centrifugal 20min, afterwards supernatant liquid is poured out, add ethanol in proper amount washing precipitation, until supernatant becomes colorless.Finally precipitation is put in an oven (80 DEG C) to dry.
One, the performance characterization of the grade cuprous oxide particle of embodiment 1 ~ 2 preparation:
1, the scanning electron microscope analysis of grade cuprous oxide particle
Fig. 2 a1 ~ 2b2 is the result using the scanning electron microscope that model is S-3400 to characterize to obtained target product.Fig. 2 a1 is for adding the SEM figure of target product synthesized by Fructus Citri grandis juice, and Fig. 2 a2 is the SEM figure of the high magnification figure of Fig. 2 a1, Fig. 2 b1 target product synthesized by interpolation juice of white turnip, and Fig. 2 b2 is the high magnification figure of Fig. 2 b1.
As can be seen from Fig. 2 a1, the Red copper oxide particle obtained in shaddock juice is spherical or spherical particle, and distribution is comparatively even, grain diameter 100 ~ 500nm.As can be seen from Fig. 2 a2, the surface ratio of product grain is more coarse, and carefully identification can find that large spheroid is that the small-particle being tens nanometers by particle diameter assembles.The surface of some spheroid has diameter to be the circular opening of 50 ~ 100nm, can inference section spheroid may be hollow structure.
As can be seen from Fig. 2 b1, in white turnip liquid, products therefrom is spheroidal particle, and dispersion is relatively more even, and particle diameter is at about 0.5 ~ 1 μm.As can be seen from Fig. 2 b2, the surface ratio of product grain is more coarse.
2, the X diffraction analysis of grade cuprous oxide particle
Fig. 3 a ~ 3b is the result using the X-ray diffractometer that model is D8ADVANCE to characterize to obtained target product.Fig. 3 a ~ Fig. 3 b is followed successively by the X-ray diffractogram adding target product synthesized by Fructus Citri grandis juice, juice of white turnip.
As can be seen from Fig. 3 a, the product of Fructus Citri grandis juice synthesis is occurred five diffraction peaks near 29.70 °, 36.61 °, 42.51 °, 61.66 ° and 73.91 ° at 2 θ, reference standard card (JCPDS74-1230) can find, correspond respectively to the characteristic diffraction peak in (110), (111), (200) of isometric system Red copper oxide, (220) and (311) face, wherein the diffraction peak intensity in (111) face is the highest, proves that product is Red copper oxide.
As can be seen from Fig. 3 b, the product that the product of juice of white turnip synthesis and Fructus Citri grandis juice synthesize closely, there is (110), (111), (200) of isometric system Red copper oxide, the characteristic diffraction peak in (220) and (311) face equally, proved that products therefrom is also Red copper oxide.
Therefore, as shown in Figure 3, the product that prepared by embodiment 1 ~ 2 is Red copper oxide.
3, the Infrared spectroscopy of grade cuprous oxide particle
Fig. 4 a ~ 4b is the result using the Fourier transform infrared spectrometer that model is AVATAR-380 type to characterize to obtained target product.Fig. 4 a ~ Fig. 4 b is followed successively by the infrared spectrogram of adding target product synthesized by Fructus Citri grandis juice, juice of white turnip.
From Fig. 4 a ~ 4b, the product of two kinds of juice synthesis 3433 ~ 3448,2160,2073,1637,1414,1107 ~ 1111,617 ~ 619cm
-1there is infrared absorption peak at place, wherein 3433 ~ 3448,1637,1414cm
-1may be the absorption of the group such as hydroxyl, amino, amido linkage, carboxyl of the biomolecules such as amino acid, albumen, vitamins C at place, 617 ~ 619cm
-1may be the characteristic absorbance of Red copper oxide, this shows in products therefrom Red copper oxide containing the biomolecules in two kinds of vegetable and fruit juice.
Therefore, from Fig. 4 a ~ 4b, containing biomolecules in product Red copper oxide prepared by embodiment 1 ~ 2.
4, the transmission electron microscope of grade cuprous oxide prepared of embodiment 1 and electron diffraction
Fig. 5 a ~ 5d is transmission electron microscope and electron-diffraction diagram to adding target product synthesized by Fructus Citri grandis juice.Fig. 5 a ~ Fig. 5 c is respectively the TEM figure of different multiplying, and Fig. 5 d is selected area electron diffraction figure.
As can be seen from Fig. 5 a, the shape of product is spherical or class is spherical, particle diameter 100 ~ 500nm, and this is consistent with scanning electron microscopic observation result.In addition, be it can also be seen that by Fig. 5 b, in the middle of some particles, bright surrounding is dark, deducibility its be hollow structure.Can be found out by Fig. 5 c, the edge of particle is lighter, has illustrated that biomolecules is wrapped up.Selected area electron diffraction figure there is array of light spots (shown in Fig. 5 d), shown that in shaddock juice, gained Red copper oxide is single crystal structure.From Fig. 5 a ~ 5d, grade cuprous oxide prepared by embodiment 1 is the monocrystalline Red copper oxide that part has hollow structure.
Two, the research of reaction mechanism
1, the mensuration of Vitamin C content in Fructus Citri grandis juice, juice of white turnip
Get 20mL juice, 100mL distilled water, 15mL2mol ∕ L HAc solution, 15mL1% starch solution join the Erlenmeyer flask kind of 250mL.Use I
2standardized solution titration juice, parallel titration three times.I
2the consumption of standardized solution is respectively a mL, b mL, c mL, and average-volume is d=(a+b+c)/3.The Vc content of juice is: Vc%=C
i2v
i2× 176.12 ∕ 30.
By calculating, the Vitamin C content in Fructus Citri grandis juice, juice of white turnip is followed successively by 0.15,0.35mg/mL.
2, the Infrared spectroscopy of Fructus Citri grandis juice, juice of white turnip
Fig. 1 is the result using the Fourier transform infrared spectrometer that model is AVATAR-380 type to characterize to four kinds of vegetable and fruit juice.Fig. 1 a ~ Fig. 1 b is followed successively by the infrared spectrogram of Fructus Citri grandis juice, juice of white turnip.
As seen from Figure 1, two kinds of juice 3450 ~ 3458,2069 ~ 2071,1637 ~ 1639,1417,1136,642,621cm
-1infrared absorption peak is there is at place, the absorption of the group such as hydroxyl, amino, amido linkage, carboxyl of the biomolecules such as amino acid, albumen, vitamins C and polysaccharide element may be belonged to, this shows may contain various biomolecules in two kinds of juice, as amino acid, protein, VITAMIN and polysaccharide element etc.
3, reaction start and at the end of the specific conductivity of mixed solution and pH
Get two parts of 20mL0.2mol ∕ L copper-baths in 100mL small beaker, add 20mL shaddock juice wherein, fully stir with glass stick and make it mix, after several minutes, survey its pH and specific conductivity respectively.The copper sulfate getting 20mL0.2mol ∕ L is placed in 100mL small beaker, adds 20mL distilled water wherein, fully stirs and makes it mix, survey its specific conductivity and pH after several minutes with glass stick.The data obtained is as shown in table 1.
Table 1 copper sulfate mixes specific conductivity and the pH of front and back solution with fruit juice
| Solution composition | Specific conductivity μ s/cm | pH |
| 20mLCu 2++20mLH 2O | 7.34 | 3.34 |
| 20mLCu 2++ 20mL shaddock juice | 7.28 | 2.42 |
As can be seen from Table 1, the specific conductivity of copper sulfate solution is 7.34 μ s/cm, and the specific conductivity of the mixing solutions of cupric ion and shaddock juice only has 7.28 μ s/cm, can illustrate and there occurs interaction between some biomolecules in cupric ion and juice, thus cause the rate of migration of the removable ion in solution to reduce, also strong some biomolecules demonstrated in juice is that the growth of Red copper oxide particle provides template.From the change of pH, can find that these two kinds of solution are all acidic solutions, and bivalent cupric ion is easily reduced into elemental copper in an acidic solution, is unfavorable for the synthesis of Red copper oxide, the synthesis of the Red copper oxide further illustrated needs to complete under the condition of alkalescence.
In addition, characterize us also as can be seen from the infrared spectra of product above and transmission electron microscope, containing biomolecules in the Red copper oxide that two kinds of juice is obtained.And, the surface irregularity of products therefrom particle.Therefore, these cuprous oxide crystals may be that Jie formed by the approach of non-classical crystallization sees crystal.First, initial nano particle is formed in the solution by nucleation process, biomolecules in following vegetable and fruit juice changes size and the pattern of initial nano particle by modifying, there is directed gathering in a small amount of particle produced in solution under lower degree of supersaturation, nano particle subunit in polymer moves generation druse, and this process is along with the restructuring of the biomolecules in vegetable and fruit juice and desorption process.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.
Claims (3)
1. a synthetic method for grade cuprous oxide particle, by Cu
2+the reaction system that solution is formed is made through reduction reaction, it is characterized in that: under this reaction system is in alkaline condition, and contains Cu in reaction system
2+be reduced into Cu
+and be used as nucleation template to form the biomolecules of grade cuprous oxide particle, the juice of described biomolecules for being formed by vegetables or fruit;
Described juice is juice of white turnip;
By juice, alkali lye and Cu
2+solution mixing and stirring, Cu
2+with the OH in alkali lye
-between mol ratio be 1:2 ~ 4, in 30 ~ 60 DEG C reaction 0.1 ~ 1h; Cool, hocket centrifugation and carrying out washing treatment, dry obtained grade cuprous oxide particle;
Described grade cuprous oxide particle is diametrically the spherical grain shape of 0.5 ~ 1 μm.
2. the synthetic method of grade cuprous oxide particle according to claim 1, is characterized in that: described Cu
2+solution is copper-bath, and described alkali lye is sodium hydroxide solution.
3. the synthetic method of grade cuprous oxide particle according to claim 2, it is characterized in that: the preparation method of described juice is: white turnip is cleaned peeling, the pulp of peeling is put into mortar, hockets and grind and filter at least one times, obtain juice.
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| CN104609456B (en) * | 2014-12-31 | 2016-08-24 | 浙江理工大学 | A kind of preparation method of the C/N codope cuprous nanosphere of porous oxidation based on sericin |
| CN106966422B (en) * | 2017-04-01 | 2018-10-30 | 华南理工大学 | A kind of pair of spherical cuprous oxide microballoon and preparation method thereof |
| CN109603851A (en) * | 2018-12-29 | 2019-04-12 | 合肥学院 | A kind of preparation method and application of silver/cuprous oxide composite material |
| CN110354906A (en) * | 2019-08-27 | 2019-10-22 | 合肥学院 | A kind of Cu2O/ chitin composite membrane and preparation method thereof |
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| C06 | Publication | ||
| PB01 | Publication | ||
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