CN105417573B - One kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles - Google Patents

One kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles Download PDF

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Publication number
CN105417573B
CN105417573B CN201510909222.XA CN201510909222A CN105417573B CN 105417573 B CN105417573 B CN 105417573B CN 201510909222 A CN201510909222 A CN 201510909222A CN 105417573 B CN105417573 B CN 105417573B
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China
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solution
lauroylamidopropyl betaine
nanoparticles
prepares
lauroylamidopropyl
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CN201510909222.XA
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CN105417573A (en
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殷广明
郑建华
王哲
辛建娇
王文波
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Qiqihar University
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Qiqihar University
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G3/00—Compounds of copper
    • C01G3/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/16—Pore diameter
    • C01P2006/17—Pore diameter distribution

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing Of Micro-Capsules (AREA)
  • Manufacture Of Metal Powder And Suspensions Thereof (AREA)

Abstract

One kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, the invention belongs to the preparation field of inorganic nano material, and in particular to Cu2The preparation method of O nanoparticles.The present invention is to solve existing Cu2The single technical problem of product structure that the preparation method of O microballoons obtains.This method：First, lauroylamidopropyl betaine solution is prepared；2nd, pH is adjusted after acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution again, or first adjusts the pH of lauroylamidopropyl betaine solution, then acetic acid copper solution is added dropwise, obtains mixed liquor；3rd, reaction is stirred after ascorbic acid solution is added dropwise, then separates, obtain Cu after drying2O nanoparticles.The construction unit of the microballoon is that class is needle-shaped or spherical nanoparticles, and has mesoporous or hollow structure, can be used as solar cell, optics, biology sensor and electrode anode material etc..

Description

One kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles
Technical field
The invention belongs to the preparation field of inorganic nano material, and in particular to Cu2The preparation method of O nanoparticles
Background technology
Cuprous oxide (Cu2O be) a kind of important metal oxide, belong to p-type semiconductor material, solar cell, Optics, biology sensor and electrode anode material etc. are with a wide range of applications.Based on Cu2Application important O The nanometer Cu of value and special nature, different-shape and structure2O, the research of characterization and correlated performance is subject to that researcher's is extensive Concern.Wherein there is the Cu of hollow structure2The preparation method of O microballoons is more, such as《German applied chemistry》(Angewandte Chemic International Edition) the 1489-1492 pages of every 9 phase of volume 46 in 2007 disclose one kind with table Face lammonium bromide (CTAB) is templated synthesis nanometer Cu2The method of the more shell hollow spheres of O, Er Qiekong The ball wall of bulbus cordis is monocrystalline.The Chinese patent of Publication No. CN100486896 discloses one kind and utilizes aqueous phase cluster soft mold plates method Prepare monodispersed Cu2The method of the hollow sub-micro balls of O, this method are formed using polyvinylpyrrolidone and lauryl sodium sulfate Aqueous solution containing mantoquita is mixed, gone back after adjusting pH value with hydrazine hydrate as soft template by cluster with cluster soft mold plates aqueous solution Former agent, quickly reduction obtains Cu to copper ion2The hollow sub-micro spherocolloid solution of O.Reaction product is centrifuged, precipitation deionization Water and washes of absolute alcohol, obtain being self-assembly of by the cuprous nano particle of particle diameter about 11~22nm and have narrow particle diameter The monodispersed Cu of 400~550nm of diameter of distribution characteristics2The hollow sub-micro balls of O.But above-mentioned method can only obtain single structure Cu2O nanoparticles.
The content of the invention
The present invention is to solve the Cu of existing hollow structure2The product structure that the preparation method of O microballoons obtains is single Technical problem, and one kind is provided and prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles.
The present invention's prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, carries out according to the following steps：
First, it is 0.2%~0.3% by the concentration of lauroylamidopropyl betaine, lauroylamidopropyl betaine is added Into deionized water, 30~40min is stirred, obtains lauroylamidopropyl betaine solution；
2nd, acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, after being added dropwise, stirring 30~ 40min, it is 10.0~10.5 then to adjust pH with NaOH solution, obtains mixed liquor；Or adjust lauramide with NaOH solution Propyl betaine solution for 10.0~10.5, then acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, dripped After adding, 30~40min is stirred, obtains mixed liquor；
3rd, ascorbic acid solution is added drop-wise to 40~60min of stirring reaction in mixed liquor, obtains suspension；Wherein acetic acid The molar ratio of copper and ascorbic acid is 1：(2~2.5)；Suspension is centrifuged, solid formation water and ethanol therein Washed, then dried respectively, obtain Cu2O nanoparticles.
For the present invention under the comprehensive function of lauroylamidopropyl betaine and other compositions, obtain high dispersive has duct The Cu of structure2O microballoons, and the characteristics of lauroylamidopropyl betaine is in different liquids environment is utilized, by varying raw material Addition order, with regard to two kinds of different Cu of construction unit can be obtained2O nanoparticles, by lauroylamidopropyl betaine, acetic acid Copper, the order of NaOH add Cu prepared by raw material2The construction unit of O microballoons is acicular nanometer particle, and presses dodecanamide propyl Glycine betaine, NaOH, the order of copper acetate add Cu prepared by raw material2The construction unit of O microballoons is spherical nanoparticles, using phase Same raw material, can prepare two kinds of different structure units and be respectively provided with the Cu of pore passage structure2O nanoparticles.Preparation method letter Single, advantages of nontoxic raw materials, meets the requirement in terms of energy conservation and environmental protection.
Brief description of the drawings
Fig. 1 is Cu prepared by Examples 1 and 22The X-ray diffraction spectrogram of O nanoparticles；
Fig. 2 is Cu prepared by embodiment 12The stereoscan photograph of O nanoparticles；
Fig. 3 is Cu prepared by embodiment 12The transmission electron microscope photo of O nanoparticles；
Fig. 4 is Cu prepared by Examples 1 and 22The pore size distribution curve of O nanoparticles；
Fig. 5 is Cu prepared by embodiment 22The stereoscan photograph of O nanoparticles；
Fig. 6 is Cu prepared by embodiment 22The transmission electron microscope photo of O nanoparticles.
Embodiment
Embodiment one：Present embodiment prepares Cu using lauroylamidopropyl betaine2The side of O nanoparticles Method, carries out according to the following steps：
First, it is 0.2~0.3% by the concentration of lauroylamidopropyl betaine, lauroylamidopropyl betaine is added to In deionized water, 30~40min is stirred, obtains lauroylamidopropyl betaine solution；
2nd, acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, after being added dropwise, stirring 30~ 40min, it is 10.0~10.5 then to adjust pH with NaOH solution, obtains mixed liquor；Or adjust lauramide with NaOH solution Propyl betaine solution for 10.0~10.5, then acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, dripped After adding, 30~40min is stirred, obtains mixed liquor；
3rd, ascorbic acid solution is added drop-wise to 40~60min of stirring reaction in mixed liquor, obtains suspension；Wherein acetic acid The molar ratio of copper and ascorbic acid is 1：(2~2.5)；Suspension is centrifuged, solid formation water and ethanol therein Washed, then dried respectively, obtain Cu2O nanoparticles.
Embodiment two：The present embodiment is different from the first embodiment in that dodecanamide propyl in step 1 The concentration of glycine betaine is 0.25%.It is other identical with embodiment one.
Embodiment three：The present embodiment is different from the first and the second embodiment in that by copper acetate in step 2 Solution is added drop-wise in lauroylamidopropyl betaine solution, after being added dropwise, is stirred 35min, is then adjusted pH with NaOH solution For 10.2.It is other the same as one or two specific embodiments.
Embodiment four：By vinegar in step 2 unlike one of present embodiment and embodiment one to three Sour copper solution is added drop-wise in lauroylamidopropyl betaine solution, after being added dropwise, 35min is stirred, then with NaOH solution tune It is 10.5 to save pH.It is other identical with one of embodiment one to three.
Embodiment five：Used in step 2 unlike one of present embodiment and embodiment one to three The pH value that NaOH solution adjusts lauroylamidopropyl betaine solution is 10.5, then acetic acid copper solution is added dropwise, after being added dropwise, 35min is stirred, obtains mixed liquor.It is other identical with one of embodiment one to three.
Embodiment six：Step 3 moderate resistance unlike one of present embodiment and embodiment one to five is bad Hematic acid solution is added drop-wise to stirring reaction 50min in mixed liquor.It is other identical with one of embodiment one to five.
Embodiment seven：Step 3 copper acetate unlike one of present embodiment and embodiment one to six Molar ratio with ascorbic acid is 1：2.2.It is other identical with one of embodiment one to six.
Embodiment eight：Acetic acid in step 2 unlike one of present embodiment and embodiment one to seven The amount of the material of copper acetate and the ratio of the volume of lauroylamidopropyl betaine solution are 1mmol in copper solution：(300~350) mL.Other are identical with one of embodiment one to seven.
With following verification experimental verification beneficial effects of the present invention：
Embodiment 1：The present embodiment prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, by following Step carries out：
First, by 0.22mL mass percent concentrations be 35% lauroylamidopropyl betaine add fill 100mL go from In sub- water, 30min is stirred, obtains lauroylamidopropyl betaine solution；
2nd, it is 0.1molL by 3mL concentration- 1Acetic acid copper solution be added drop-wise in lauroylamidopropyl betaine solution, After being added dropwise, 30min is stirred, is then 0.5molL with concentration- 1NaOH solution adjust pH be 10.0, mixed Liquid；
3rd, it is 0.2molL by 3mL concentration- 1Ascorbic acid solution be added drop-wise in mixed liquor electromagnetic agitation and react 40min, obtains suspension；Suspension is centrifuged, solid formation therein is washed respectively with water and ethanol, then It is dry, obtain Cu2O nanoparticles.
Cu manufactured in the present embodiment2The XRD spectra of O nanoparticles as shown in fig. 1A, it will be seen from figure 1 that prepare Cu2O is in cubic phase crystal structure, and crystallinity is high.
Cu manufactured in the present embodiment2The stereoscan photograph of O nanoparticles is as shown in Fig. 2, transmission electron microscope photo such as Fig. 3 institutes Show, figure it is seen that Cu2A diameter of 170~220nm of O nanoparticles, from figure 3, it can be seen that Cu2The ball of O nanoparticles Wall is by the acicular Cu of class2O nano particles structure, its class can be seen more clearly from the partial enlarged view in the figure lower left corner Acicular nano particle, and Cu2There are duct for O nanoparticles.
Cu manufactured in the present embodiment2The pore size distribution curve of O nanoparticles as shown in a of Fig. 4, from fig. 4, it can be seen that Cu2O nanoparticles are mesoporous level there are duct.
Embodiment 2：The present embodiment prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, by following Step carries out：
First, by 0.22mL mass percent concentrations be 35% lauroylamidopropyl betaine add fill 100mL go from In sub- water, 30min is stirred, obtains lauroylamidopropyl betaine solution；
2nd, it is 0.5molL with concentration- 1NaOH solution the pH of lauroylamidopropyl betaine solution is adjusted to 10.0, it is then 0.1molL by 3mL concentration- 1Acetic acid copper solution be added drop-wise in lauroylamidopropyl betaine solution, drip After adding, 30min is stirred, obtains mixed liquor；
3rd, it is 0.2molL by 3mL concentration- 1Ascorbic acid solution be added drop-wise in mixed liquor electromagnetic agitation and react 40min, obtains suspension；Suspension is centrifuged, solid formation therein is washed respectively with water and ethanol, then It is dry, obtain Cu2O nanoparticles.
Cu manufactured in the present embodiment2The XRD spectra of O nanoparticles can be seen that system as shown in fig. ib, from the b of Fig. 1 Standby Cu2O is in cubic phase crystal structure, and crystallinity is high.
Cu manufactured in the present embodiment2The stereoscan photograph of O nanoparticles is as shown in figure 5, transmission electron microscope photo such as Fig. 6 institutes Show, from fig. 5, it can be seen that Cu2A diameter of 170~220nm of O nanoparticles, from fig. 6, it can be seen that Cu2The ball of O nanoparticles Wall is by spherical Cu2O nano particles structure, and Cu2O nanoparticles are hollow sphere.
Cu manufactured in the present embodiment2The pore size distribution curve of O nanoparticles, can from the b of Fig. 4 as shown in the b of Fig. 4 Go out, Cu2O nanoparticles are mesoporous level there are duct.

Claims (8)

1. one kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, it is characterised in that this method is by following Step carries out：
First, it is 0.2%~0.3% by the concentration of lauroylamidopropyl betaine, lauroylamidopropyl betaine is added to In ionized water, 30~40min is stirred, obtains lauroylamidopropyl betaine solution；
2nd, acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, after being added dropwise, stirs 30~40min, so It is 10.0~10.5 to adjust pH value with NaOH solution afterwards, obtains mixed liquor；Or adjust dodecanamide propyl sweet tea with NaOH solution The pH value of dish aqueous slkali is 10.0~10.5, then acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution, is added dropwise After, 30~40min is stirred, obtains mixed liquor；
3rd, ascorbic acid solution is added drop-wise to 40~60min of stirring reaction in mixed liquor, obtains suspension；Wherein copper acetate with The molar ratio of ascorbic acid is 1：(2~2.5)；Suspension is centrifuged, solid formation water and ethanol difference therein Washed, then dried, obtain the Cu with mesoporous level pore passage structure2O nanoparticles.
2. one kind according to claim 1 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, it is special The concentration levied in the lauroylamidopropyl betaine in step 1 is 0.25%.
3. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution in step 2, after being added dropwise, stirring 35min, it is 10.2 then to adjust pH with NaOH solution.
4. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that acetic acid copper solution is added drop-wise in lauroylamidopropyl betaine solution in step 2, after being added dropwise, stirring 35min, it is 10.5 then to adjust pH with NaOH solution.
5. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that the pH value for adjusting lauroylamidopropyl betaine solution in step 2 with NaOH solution is 10.5, then acetic acid is added dropwise Copper solution, after being added dropwise, stirs 35min, obtains mixed liquor.
6. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that ascorbic acid solution is added drop-wise to stirring reaction 50min in mixed liquor in step 3.
7. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that the molar ratio of step 3 copper acetate and ascorbic acid is 1：2.2.
8. one kind according to claim 1 or 2 prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles, It is characterized in that in step 2 in acetic acid copper solution the amount of the material of copper acetate and lauroylamidopropyl betaine solution volume Ratio be 1mmol：(300~350) mL.
CN201510909222.XA 2015-12-10 2015-12-10 One kind prepares Cu using lauroylamidopropyl betaine2The method of O nanoparticles Expired - Fee Related CN105417573B (en)

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CN107321394A (en) * 2017-05-09 2017-11-07 安徽皖东化工有限公司 A kind of sewage disposal anion exchange resin preparation method
CN107185600A (en) * 2017-05-09 2017-09-22 安徽皖东化工有限公司 A kind of preparation technology of groundwater treatment macroporous anion exchange resin

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CN100486896C (en) * 2007-03-02 2009-05-13 江南大学 Method for preparing monodispersed copper-protoxide hollow microsphere by aqueous phase cluster soft mold plates process
CN101397137A (en) * 2007-09-27 2009-04-01 刘文红 Globular inorganic oxide material, synthetic method, modification method and use thereof
CN103204525B (en) * 2012-01-17 2017-04-05 上海杰事杰新材料(集团)股份有限公司 Application of the lactams as solvent in nano material preparation

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