CN102557112A - Method for preparing nano CdS particles by using switchable surfactant micelle - Google Patents
Method for preparing nano CdS particles by using switchable surfactant micelle Download PDFInfo
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- CN102557112A CN102557112A CN201010578050XA CN201010578050A CN102557112A CN 102557112 A CN102557112 A CN 102557112A CN 201010578050X A CN201010578050X A CN 201010578050XA CN 201010578050 A CN201010578050 A CN 201010578050A CN 102557112 A CN102557112 A CN 102557112A
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Abstract
The invention discloses a method for preparing nano CdS particles with the characteristics of simple operation, convenient separation and convenient recovery, which is characterized in that an alkyl amidino bicarbonate surfactant possessing a switchable characteristic is prepared to a micelle solution, nano CdS particles are prepared in the micelle solution, the alkyl amidino bicarbonate losses the surface activity after the processes of heating and introducing nitrogen after the reaction is finished, the solution is automatically laminated, and the processes of centrifugation and washing are simply carried out to obtain the nano CdS particles. According to the invention, the original tedious recovery and separation processes can be substantially simplified during the nano particles preparation, and the method of the invention possesses wide application prospect during the nano particles preparation.
Description
Technical field
The present invention relates to a kind of method for preparing the nano-tube/CdS particle, especially utilize the switching mode surfactant micelle to prepare the method for nano-tube/CdS particle.At first with switching mode tensio-active agent preparation micella; Preparation nano-tube/CdS particle in this system reacts the end post-heating and also feeds nitrogen then, and the switching mode tensio-active agent loses surfactivity; The automatic breakdown of emulsion layering of micella obtains the nano-tube/CdS particle through simple spinning.
Background technology
The nano-tube/CdS particle is owing to have quantum size effect, surface effects, and macro quanta tunnel effect makes its physico-chemical property that shows a series of excellences and second nonlinear optic characteristic, has huge application potential at aspects such as light, electricity, magnetic, catalysis.
As with data by MoM and MEI such as sol-gel method, micella, prepared with microemulsion reactor nanoparticle have advantages such as equipment is simple, experiment condition is gentle, size of particles is controlled, therefore be nanoparticle synthetic in crucial technology.But methods such as micella can run into the Separation and Recovery problem in the nanoparticle preparation: breakdown of emulsion difficulty, SURFACTANT ADSORPTION reclaim difficulty etc. at nanoparticle surface, tensio-active agent.Adopt traditional breaking method can not solve the separation problem of tensio-active agent in system, and tensio-active agent uses directly discharging of back, not only waste resource, environment is also produced a series of influence.
People such as Jessop are in Science (Science, 2006,313,958; CA2527144) reported a kind of switching mode long-chain amidino groups supercarbonate tensio-active agent on.Acid amidine is not have surface-active oil-soluble compounds, and it can form under water and carbonic acid gas effect has surface-active acid amidine supercarbonate; And when in this salt, feeding nitrogen or heating, reversed reaction then takes place, regenerating does not have surface-active acid amidine.This tensio-active agent can be applied in roily oil or the letex polymerization, does not see its report in the nano-tube/CdS particle.
The objective of the invention is in order to solve in the method that conventional surfactant prepares micella synthesis of nano CdS particle the problem of separating, recycling of tensio-active agent and nanoparticle in the last handling process, and a kind of method of utilizing switch surfactant micelle synthesis of nano CdS that provides.
Summary of the invention
The present invention to be having the alkyl amidine supercarbonate tensio-active agent preparation micellar solution of switching characteristic, and this type of micellar system effective breakdown of emulsion when switching mode tensio-active agent from " surfactivity is arranged " to " no surfactivity " becomes profit two phases, feeding CO
2After can form micella again.It is applied in nanoparticle when preparing; Can obtain nanoparticle through simple spinning; Owing to reduce greatly when the adsorption of " losing " surface-active acid amidine on nanoparticle is than " surfactivity state " behind the breakdown of emulsion, can remove the compound of particle surface absorption through simple washing.Therefore this method can will be simplified breakdown of emulsion originally loaded down with trivial details in the nanoparticle preparation greatly, removes tensio-active agent, reclaim processes such as separations, and it will have broad application prospects in nanoparticle prepares.
The switch list surface-active agent that the present invention adopted is: N '-alkyl-N, N-dimethyl-ethanamidine base supercarbonate (I) and N, N '-two alkyl-ethanamidine base supercarbonate (II).
R is the straight or branched alkyl of 12-16 carbon atom among following formula I and the II, specifically can be selected from the following material one or more: n-dodecane, two dodecyls, n-tetradecane, two tetradecanes, n-hexadecane, two n-Hexadecanes.
The present invention at first utilizes switch list surface-active agent I or II preparation micellar system.Compound method mainly contains two kinds:
(1) 0.5g-1.5g switch list surface-active agent is joined in the mixed solution of 0-2g n-hexyl alcohol, 2-15g normal heptane, at room temperature sonic oscillation 30min forms inverse micellar solution;
(2) 0.5g-1.5g switch list surface-active agent is joined in the 2-15g water, at room temperature sonic oscillation 30min forms micellar solution;
The present invention utilizes the micellar solution of preparation to prepare the nano-tube/CdS particle.Formed micellar solution is divided into two parts of A, B, the Cd (NO of A solubilising 0.02-0.2g 0.05mol/L
3)
2Solution, the Na of B solubilising 0.02-0.2g 0.05mol/L
2The S aqueous solution, sonic oscillation 30min slowly is added drop-wise to A among the B more respectively, sonic oscillation reaction 1h;
The present invention adds 0-1g Dodecyl Mercaptan, 0-20g normal heptane in system after the nano-tube/CdS particle preparation finishes; Be warming up to 65 ℃, and in system, lead to nitrogen, alkyl amidine supercarbonate I or II lose surfactivity; The automatic breakdown of emulsion of solution; Can obtain the nano-tube/CdS particle through simple spinning, use ethanol and deionized water washing sediment 2-3 time respectively, vacuum-drying promptly gets the nano-tube/CdS particle.Collect the acid amidine in the normal heptane, feed CO
2, make alkyl amidine supercarbonate I or II again, realize the tensio-active agent recycling.
Advantage of the present invention is:
(1) compound method of CdS nanoparticle of the present invention need not main equipment, and operational safety, easy, easy going are convenient to control the size pattern and the performance of nano-tube/CdS, and favorable repeatability is easy to large-scale industrialization production, can realize the pollution-free industry of energy-saving and emission-reduction.
(2) reaction conditions of the present invention is gentle, can carry out the synthetic of nano-tube/CdS under the room temperature; No obnoxious flavour produces in the reaction process, and reaction does not need loaded down with trivial details breakdown of emulsion, separation, washing operation after finishing.
(3) the present invention prepares the nano-tube/CdS particle in the micella of switch list surface-active agent, and the nano-tube/CdS that synthesizes is a monocrystalline, sphere, and size distribution is even, and diameter is 4-10nm, meets the size range that the CdS quantum confined effect is manifested.
Description of drawings
Fig. 1 is the transmission electron microscope picture (TEM) of embodiment 1 synthetic nano-tube/CdS; Fig. 2 is the high-resolution-ration transmission electric-lens figure (HRTEM) of embodiment 1 synthetic nano-tube/CdS; Fig. 3 is the uv absorption spectrum of embodiment 1 synthetic nano-tube/CdS, and Fig. 4 is the fluorescence emission spectrum of embodiment 1 synthetic nano-tube/CdS.
Embodiment
Through specific embodiment the present invention is done further description below, but the present invention should not only limit to these embodiment.The switch list surface-active agent likes that available from ladder is uncommon (Shanghai) changes into industrial development ltd, and other reagent are available from Shanghai traditional Chinese medicines reagent group.
Embodiment 1
This embodiment carries out according to the following steps: with 0.5gN '-hexadecyl-N, N-dimethyl-ethanamidine base supercarbonate (I), 1g n-hexyl alcohol, 9g normal heptane mixing sonic oscillation 30min form stable reverse micelle; Formed reverse micelle is divided into two parts of A, B, the Cd (NO of A solubilising 0.02g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.02g0.05mol/L
2The S aqueous solution, sonic oscillation is 30-60 minute respectively, A slowly is added drop-wise among the B sonic oscillation reaction 1h again; In the yellow solution that generates the CdS nanoparticle, drip the 0.03g Dodecyl Mercaptan, be warming up to 65 ℃, and in system, lead to nitrogen 1h; After treating the solution layering, extracting yellow leafing gains in depth of comprehension throw out is used ethanol and deionized water washing sediment 2-3 time respectively, and vacuum-drying promptly gets the nano-tube/CdS powder.Collect the acid amidine in the normal heptane, feed CO
2, make N '-hexadecyl-N again, N-dimethyl-ethanamidine base supercarbonate (I).
The nano-tube/CdS that this embodiment synthesizes is a monocrystalline, sphere, diameter is about 4nm, the amount of having confinement effect (like Fig. 3 and shown in Figure 4).Fig. 3 is the UV, visible light absorption spectrum of the synthetic CdS nanoparticle of this embodiment, and system has the absorption platform at the 380nm place.There are two kinds of emissions usually in the fluorescence spectrum of CdS nanoparticle; A kind of is the band edge emission, and a kind of is the surface state emission, and Fig. 4 is the fluorescence emission spectrum that this embodiment synthesizes the CdS nanoparticle; The 431nm place is the band edge emission of CdS nanoparticle, and the 527nm place is the surface state emission of CdS nanoparticle.Fig. 2 is the HRTEM figure of the synthetic CdS nanoparticle of this embodiment, and the spacing that can measure the CdS nanoparticle among the figure is 0.333nm.
This embodiment carries out according to the following steps: with 0.5g N, N '-hexadecyl-ethanamidine base supercarbonate (II), 0.5g n-hexyl alcohol, 12g normal heptane mixing sonic oscillation 30min form stable reverse micelle; Formed micella is divided into two parts of A, B, the Cd (NO of A solubilising 0.05g 0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.05g 0.05mol/L
2The S aqueous solution, sonic oscillation is 30-60 minute respectively, A slowly is added drop-wise among the B sonic oscillation reaction 1h again; In the yellow solution that generates the CdS nanoparticle, drip the 0.05g Dodecyl Mercaptan, be warming up to 65 ℃, and in system, lead to nitrogen 1h; After treating the solution layering, extracting yellow leafing gains in depth of comprehension throw out is used ethanol and deionized water washing sediment 2-3 time respectively, and vacuum-drying promptly gets the nano-tube/CdS powder.Collect the acid amidine in the normal heptane, feed CO
2, make N again, N '-hexadecyl-ethanamidine base supercarbonate (II).
Embodiment 3
This embodiment carries out according to the following steps: with 0.5gN '-dodecyl-N, N-dimethyl-ethanamidine base supercarbonate (I), 0.5g n-hexyl alcohol, 6g normal heptane mixing sonic oscillation 30min form stable reverse micelle; Formed reverse micelle is divided into two parts of A, B, the Cd (NO of A solubilising 0.01g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.01g0.05mol/L
2The S aqueous solution, sonic oscillation is 30-60 minute respectively, A slowly is added drop-wise among the B sonic oscillation reaction 1h again; In the yellow solution that generates the CdS nanoparticle, drip the 0.03g Dodecyl Mercaptan, be warming up to 65 ℃, and in system, lead to nitrogen 1h; After treating the solution layering, extracting yellow leafing gains in depth of comprehension throw out is used ethanol and deionized water washing sediment 2-3 time respectively, and vacuum-drying promptly gets the nano-tube/CdS powder.Collect the acid amidine in the normal heptane, feed CO
2, make N '-dodecyl-N again, N-dimethyl-ethanamidine base supercarbonate (I).
Embodiment 4
This embodiment carries out according to the following steps: with 1gN '-hexadecyl-N, N-dimethyl-ethanamidine base supercarbonate (I) sonic oscillation 30min in the 15g de-ionized forms stable micella; Formed micella is divided into two parts of A, B, and A adds the Cd (NO of 0.02g0.05mol/L
3)
2The aqueous solution, B adds the Na of 0.02g0.05mol/L
2The S aqueous solution, sonic oscillation is 30-60 minute respectively, A slowly is added drop-wise among the B sonic oscillation reaction 1h again; In the yellow solution that generates the CdS nanoparticle, drip the 0.03g Dodecyl Mercaptan, the 15g normal heptane is warming up to 65 ℃, and in system, leads to nitrogen 1h; After treating the solution layering, extracting yellow leafing gains in depth of comprehension throw out is used ethanol and deionized water washing sediment 2-3 time respectively, and vacuum-drying promptly gets the nano-tube/CdS powder.Collect the acid amidine in the normal heptane, feed CO
2, make N '-hexadecyl-N again, N-dimethyl-ethanamidine base supercarbonate (I).
Claims (5)
1. the method for the synthetic CdS nanoparticle of the micellar solution of utilizing the switching mode tensio-active agent, its characteristic exists: with the alkyl amidine supercarbonate is tensio-active agent preparation micellar solution; And in this micellar solution preparation nano-tube/CdS particle; After the nano-tube/CdS particle preparation finishes, in system, add Dodecyl Mercaptan and normal heptane, be warming up to 65 ℃; And in system logical nitrogen; The alkyl amidine supercarbonate loses surfactivity, and the automatic breakdown of emulsion of solution obtains the nano-tube/CdS particle through simple spinning.
2. the switching mode tensio-active agent preparation micellar solution of utilizing according to claim 1; It is characterized in that tensio-active agent is the N '-alkyl-N of monoalkyl chain; The N of N-dimethyl-ethanamidine base supercarbonate and two alkyl chains; N '-alkyl-ethanamidine base supercarbonate, alkyl are respectively the straight or branched alkyl of dodecyl, tetradecyl, pentadecyl, hexadecyl.
3. be the solution that the alkyl amidine supercarbonate forms in normal heptane or water according to claim 1 with 2 described micellar solutions.
4. according to the method for claim 1,2 and 3 described switching mode surfactant micelle synthesis of nano CdS, it is characterized in that switch list surface-active agent micellar solution is divided into two parts of A, B A solubilising Cd (NO
3)
2Solution, B solubilising Na
2The S aqueous solution slowly is added drop-wise to A among the B again, sonic oscillation reaction 1h.
5. according to the separation method of claim 1,2,3 and 4 described switching mode surfactant micelle synthesis of nano CdS, it is characterized in that after the nano-tube/CdS particle preparation finishes, in system, add Dodecyl Mercaptan and normal heptane; Be warming up to 65 ℃, and in system, lead to nitrogen, alkyl amidine supercarbonate tensio-active agent loses surfactivity; The automatic breakdown of emulsion of solution; Obtain the nano-tube/CdS particle through spinning, use ethanol and deionized water wash 2-3 time respectively, vacuum-drying promptly gets the nano-tube/CdS particle.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040101465A1 (en) * | 2000-10-13 | 2004-05-27 | Adams Edward William | Surface-modified semiconductive and metallic nanoparticles having enhanced dispersibility in aqueous media |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20040101465A1 (en) * | 2000-10-13 | 2004-05-27 | Adams Edward William | Surface-modified semiconductive and metallic nanoparticles having enhanced dispersibility in aqueous media |
Non-Patent Citations (4)
| Title |
|---|
| 《Science》 20060818 Yingxin Liu et al. "Switchable Surfactants" 958-960 1-5 第313卷, * |
| 《化学研究》 20070630 王莹等 "溶剂对反胶束法合成CdS纳米粒子粒径的影响" 10-11、15 1-5 第18卷, 第2期 * |
| YINGXIN LIU ET AL.: ""Switchable Surfactants"", 《SCIENCE》, vol. 313, 18 August 2006 (2006-08-18), pages 958 - 960 * |
| 王莹等: ""溶剂对反胶束法合成CdS纳米粒子粒径的影响"", 《化学研究》, vol. 18, no. 2, 30 June 2007 (2007-06-30) * |
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Application publication date: 20120711 |