CN102531041A - Method for preparing nano cadmium dating sulphide (CdS) particles with switching mode surfactant micro-emulsion - Google Patents
Method for preparing nano cadmium dating sulphide (CdS) particles with switching mode surfactant micro-emulsion Download PDFInfo
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- CN102531041A CN102531041A CN2010105820032A CN201010582003A CN102531041A CN 102531041 A CN102531041 A CN 102531041A CN 2010105820032 A CN2010105820032 A CN 2010105820032A CN 201010582003 A CN201010582003 A CN 201010582003A CN 102531041 A CN102531041 A CN 102531041A
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Abstract
The invention discloses a method for preparing nano cadmium dating sulphide (CdS), which is simple in operation and convenient in separation and recovery. The method is characterized in that an alkyl guanyl dicarbonate surfactant with switching characteristics is used for preparing micro-emulsion, and nano CdS particles are prepared in the micro-emulsion. After reaction is finished, by heating and leading in the air, alkyl guanyl dicarbonate is enabled to lose surface activity, the micro-emulsion automatically breaks the emulsion and is layered, and nano CdS particles are obtained through simple centrifugation and washing. The method can greatly simplify previous tedious processes such as recovery and separation during preparation of nano particles and has broad application prospects in preparation of nano particles.
Description
Technical field
The present invention relates to a kind of method for preparing the nano-tube/CdS particle, especially utilize switching mode tensio-active agent microemulsion to prepare the method for nano-tube/CdS particle.At first with switching mode tensio-active agent preparation microemulsion; Preparation nano-tube/CdS particle in this system reacts and finishes post-heating and bubbling air then, and the switching mode tensio-active agent loses surfactivity; The automatic breakdown of emulsion layering of micro emulsion 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, the prepared with microemulsion reactor nanoparticle has advantages such as equipment is simple, experiment condition is gentle, size of particles is controlled, therefore be nanoparticle synthetic in crucial technology.But the micro emulsion method 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 for the problem of separating, recycling of tensio-active agent in the last handling process in the method that solves conventional surfactant micro emulsion method synthesis of nano CdS particle with nanoparticle, and a kind of method of utilizing switch list surface-active agent micro emulsion synthesis of nano CdS that provides.
Summary of the invention
The present invention is to have the alkyl amidine supercarbonate tensio-active agent preparation microemulsion of switching characteristic; It is stable that this type of microemulsion system keeps when the switching mode tensio-active agent " has surfactivity "; When the switching mode tensio-active agent loses surfactivity, the automatic breakdown of emulsion of micro emulsion becomes profit two phases.It is applied in nanoparticle when preparing; Only need to 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, and N '-two alkyl-ethanamidine base supercarbonate, structural formula is following:
R is the straight or branched alkyl of 12-16 carbon atom in the following formula, 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 preparation micellar system.Compound method is following:
5-25g switch list surface-active agent is added in the 15mL oil phase, and add 2mL to the 5mL deionized water, 1mL is to 5mL alcohol, in stirring at room to transparent system.
Above-mentioned oil phase is selected saturated alkane or toluene for use, specifically can be selected from the following material one or more: normal heptane, normal hexane, toluene.
Above-mentioned alcohol selects for use the straight or branched alkyl alcohol of 2-8 carbon atom specifically can be selected from the following material one or more: ethanol, n-propyl alcohol, Virahol, propyl carbinol, n-hexyl alcohol, n-Octanol
The present invention utilizes the micro emulsion of preparation to prepare the nano-tube/CdS particle.Formed micro emulsion is divided into two parts of A, B, and A solubilising 0.02g is to the 0.05mol/L Cd (NO of 2g
3)
2Solution, B solubilising 0.02g is to the 0.05mol/L Na of 2g
2The S aqueous solution stirs 30min respectively, A slowly is added drop-wise among the B stirring at room reaction 1h again;
The present invention is after the nano-tube/CdS particle preparation finishes; System is warming up to 65 ℃, and in system blowing air, the alkyl amidine supercarbonate loses surfactivity; The automatic breakdown of emulsion of micro emulsion; 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 the alkyl amidine supercarbonate 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 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 micro emulsion 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.
Description of drawings
Fig. 1 is the transmission electron microscope picture (TEM) 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 10g N, N '-dodecyl-ethanamidine base supercarbonate joins in the 15mL normal heptane, adds 5mL deionized water and 2g propyl carbinol, stirs 30 minutes under the room temperature, forms the microemulsion of stable transparent; Formed microemulsion is divided into two parts of A, B, the Cd (NO of A solubilising 0.1g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.1g0.05mol/L
2The S aqueous solution, stirring at room is 30 minutes respectively, A slowly is added drop-wise among the B room temperature reaction 1h again; It is faint yellow that system gradually becomes, and the faint yellow microemulsion that will generate the CdS nanoparticle after reaction finishes is warming up to 65 ℃, and in system blowing air gas 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 '-dodecyl-ethanamidine base supercarbonate.
Embodiment 2
This embodiment carries out according to the following steps: with 10g N, N '-dodecyl-ethanamidine base supercarbonate joins in the 10mL toluene, adds 5mL deionized water and 1g propyl carbinol, stirs 30 minutes under the room temperature, forms the microemulsion of stable transparent; Formed microemulsion is divided into two parts of A, B, the Cd (NO of A solubilising 0.5g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.5g0.05mol/L
2The S aqueous solution, stirring at room is 30 minutes respectively, A slowly is added drop-wise among the B room temperature reaction 1h again; It is faint yellow that system gradually becomes, and the faint yellow microemulsion that will generate the CdS nanoparticle after reaction finishes is warming up to 65 ℃, and in system blowing air gas 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 '-dodecyl-ethanamidine base supercarbonate.
Embodiment 3
This embodiment carries out according to the following steps: with 10g N, N '-hexadecyl-ethanamidine base supercarbonate joins in the 15mL normal heptane, adds 5mL deionized water and 1g propyl carbinol, stirs 30 minutes under the room temperature, forms the microemulsion of stable transparent; Formed microemulsion is divided into two parts of A, B, the Cd (NO of A solubilising 1g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 1g0.05mol/L
2The S aqueous solution, stirring at room is 30 minutes respectively, A slowly is added drop-wise among the B room temperature reaction 1h again; It is yellow that system gradually becomes, and the faint yellow microemulsion that will generate the CdS nanoparticle after reaction finishes is warming up to 65 ℃, and in system blowing air gas 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.
Embodiment 4
This embodiment carries out according to the following steps: with 10g N, N '-tetradecyl-ethanamidine base supercarbonate joins in the 10mL toluene, adds 5mL deionized water and 1.5g propyl carbinol, stirs 30 minutes under the room temperature, forms the microemulsion of stable transparent; Formed microemulsion is divided into two parts of A, B, the Cd (NO of A solubilising 0.2g0.05mol/L
3)
2The aqueous solution, the Na of B solubilising 0.2g0.05mol/L
2The S aqueous solution, stirring at room is 30 minutes respectively, A slowly is added drop-wise among the B room temperature reaction 1h again; It is yellow that system gradually becomes, and the faint yellow microemulsion that will generate the CdS nanoparticle after reaction finishes is warming up to 65 ℃, and in system blowing air gas 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 '-tetradecyl-ethanamidine base supercarbonate.
Claims (5)
1. the method for the synthetic CdS nanoparticle of a switching mode tensio-active agent microemulsion, its characteristic exists: with the alkyl amidine supercarbonate is tensio-active agent preparation microemulsion, and in this microemulsion preparation nano-tube/CdS particle; After the nano-tube/CdS particle preparation finishes; System is warming up to 65 ℃, and bubbling air, the alkyl amidine supercarbonate loses surfactivity; The automatic breakdown of emulsion of solution obtains the nano-tube/CdS particle through simple spinning.
2. switching mode tensio-active agent according to claim 1 is the N of two alkyl chains, and N '-alkyl-ethanamidine base supercarbonate is characterized in that alkyl is respectively the straight or branched alkyl of dodecyl, tetradecyl, pentadecyl, hexadecyl.
3. be that the alkyl amidine supercarbonate adds the 15mL oil phase according to claim 1 and 2 described microemulsions, 2mL is to the 5mL deionized water, and 1mL is in 5mL alcohol; Form transparent micro emulsion in stirring at room; Above-mentioned oil phase can be a normal heptane, normal hexane, one or more in the toluene; Above-mentioned alcohol is selected the straight or branched alkyl alcohol of 2-8 carbon atom for use.
4. according to the method for claim 1,2 and 3 described switching mode tensio-active agent micro emulsion synthesis of nano CdS, it is characterized in that switch list surface-active agent microemulsion 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, 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, system being warming up to 65 ℃; And bubbling air; Alkyl amidine supercarbonate tensio-active agent loses surfactivity, and the automatic breakdown of emulsion of solution obtains 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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| CN2010105820032A CN102531041A (en) | 2010-12-10 | 2010-12-10 | Method for preparing nano cadmium dating sulphide (CdS) particles with switching mode surfactant micro-emulsion |
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| CN2010105820032A CN102531041A (en) | 2010-12-10 | 2010-12-10 | Method for preparing nano cadmium dating sulphide (CdS) particles with switching mode surfactant micro-emulsion |
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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 (7)
| Title |
|---|
| 《Science》 20060818 Yingxin Liu et al. "Switchable Surfactants" 第958-960页 1-5 第313卷, * |
| 《中国优秀硕士学位论文全文数据库 工程科技辑》 20080815 王琳 "含脒基开关型表面活性剂的合成及应用研究" B016-75，正文45、62页 2-5 , * |
| 《材料研究学报》 20040831 容敏智等 "原位表面修饰纳米CdS粒子的表面结构和光学性能" 第343-351页 1-5 第18卷, 第4期 * |
| YINGXIN LIU ET AL.: ""Switchable Surfactants"", 《SCIENCE》 * |
| 容敏智等: ""原位表面修饰纳米CdS粒子的表面结构和光学性能"", 《材料研究学报》 * |
| 王琳: ""含脒基开关型表面活性剂的合成及应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技І辑》 * |
| 王琳: ""含脒基开关型表面活性剂的合成及应用研究"", 《中国优秀硕士学位论文全文数据库 工程科技І辑》, 15 August 2008 (2008-08-15) * |
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Application publication date: 20120704 |