CN101905331B - Method for extracting nano-silver in aqueous phase by using ionic liquid - Google Patents
Method for extracting nano-silver in aqueous phase by using ionic liquid Download PDFInfo
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- CN101905331B CN101905331B CN2010102614512A CN201010261451A CN101905331B CN 101905331 B CN101905331 B CN 101905331B CN 2010102614512 A CN2010102614512 A CN 2010102614512A CN 201010261451 A CN201010261451 A CN 201010261451A CN 101905331 B CN101905331 B CN 101905331B
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Abstract
The invention discloses a method for extracting nano-silver in an aqueous phase by using ionic liquid, which relates to a nano-silver. The method for extracting the nano-silver in the aqueous phase by using the ionic liquid comprises the following steps of: adding plant leaf dry powder into water; shaking the mixture in a shaking table; cooling the mixture to the room temperature, and then performing vacuum filtration to obtain plant leaf leachate; mixing the plant leaf leachate with alkaline solution and silver salt precursor solution to obtain a nano-silver sol after reaction; and adding a phase transfer agent into the nano-silver sol, and adding water-insoluble ionic liquid into the mixture to ensure that nano-silver particles can be extracted into an ionic liquid phase after shaking. The method is quick, simple and convenient, has a mild condition, can obtain the nano-silver particles in the ionic liquid, and has a good application prospect.
Description
Technical field
The present invention relates to a kind of Nano Silver, especially relate to a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver.
Background technology
Nano-Ag particles is with its unique optics and electrical properties, small-size effect, skin effect, quantum effect, is widely used in fields such as catalysis, antibiotic, electronic circuits at present.Simultaneously, it also has suitable application prospect in fields such as SERS (SERS), novel hydrogen storage material, composite electrode, low temperature Heat Conduction Materials.The biological reducing method is a kind of method that is used to prepare nano-Ag particles that development in recent years is got up; This method has plurality of advantages, like biomass starting material wide material sources, environmental friendliness and renewable, reduction process mild condition, need not add other chemical reducing agent, the nano particle good stability that obtained or the like.And wherein, plant reduction method is especially because the wide material sources of its living beings and simple have the value of industry development more.
At present, the preparation of nano-Ag particles is mainly all carried out at aqueous phase.But along with the difference of application scenario, People more and more needs the various nano-Ag particles that are dispersed in the nonaqueous phase solvent.And will realize this goal, generally through two approach: the one, directly in the nonaqueous phase solvent, prepare nano-Ag particles; Another is earlier to prepare nano-Ag particles at aqueous phase, again with its phase transfer in the nonaqueous phase solvent.Compared to preparing nano-Ag particles at aqueous phase; The research of preparation nano-Ag particles also is not very ripe in the nonaqueous phase solvent; And the characteristic and the rule difference of preparation nano-Ag particles is bigger in different solvents, and therefore, article one approach has significant limitation on using.Compare, earlier prepare nano-Ag particles at aqueous phase, with the method for its phase transfer in the target nonaqueous phase solvent, simple again, have extensive applicability.
Ionic liquid (IL) is also referred to as ionic liquid at room temperature (RTIL), but has characteristics such as stability height, easy purifying reuse, is liquid under the room temperature, and vapour pressure is extremely low, and atmosphere pollution is not described as green solvent.In recent years, ionic liquid has been obtained certain progress in the research in fields such as electrochemistry, nano material preparation, organic synthesis, catalysis, extract and separate.And in the extract and separate field, ionic liquid can be advantageously applied to liquid-liquid extraction, liquid-phase micro-extraction, SPME, supercritical CO as extraction phase
2Fields such as extraction.In recent years existing lot of documents has reported that the variety classes ionic liquid replaces traditional volatile organic solvent and is used for liquid-liquid extraction organic matter (J.Chem.Commum., 1998,16,1765; J.Chem.Eng.Data, 2004,49,1422; J.Anal.Chem., 2006,78,1774.), metal ion (J.Chem.Soc., Dalton Trans, 1999,1201; Sep.Sci.Technol., 2001,36,785.) and nano-scale particle such as nanometer copper (Environ.Sci.Technol., 2006,40,4761).
Summary of the invention
The object of the present invention is to provide a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver.
The present invention includes following steps:
1) leaves of plants dry powder is added in the entry, in shaking table, shake, be cooled to room temperature final vacuum suction filtration, get the leaves of plants leachate;
2) the leaves of plants leachate that step 1) is obtained mixes with alkaline solution and silver salt precursor solution, gets nano silver colloidal sol after the reaction;
3) in step 2) add phase transfer reagent in the nano silver colloidal sol that makes, add water-insoluble ionic liquid again, after the concussion, can with nano-Ag particles be extracted into ionic liquid mutually in.
In step 1), said leaves of plants can be fragrant camphor tree leaf etc.; Said temperature of in shaking table, shaking can be 30～60 ℃, and the time of shaking in the shaking table can be 2～10h.
In step 2) in, said alkaline solution can be NaOH etc.; Said silver salt precursor solution can be liquor argenti nitratis ophthalmicus etc.; Said reaction, at room temperature magnetic agitation is reacted 5～15h; Said plant extract concentration can be 0.1～20 with the mass concentration ratio of silver, and said alkaline solution molar concentration can be 1～40, preferred 2～20 with the molar concentration rate of silver.
In step 3), said phase transfer reagent can be softex kw (CTAB) etc., said phase transfer reagent and silver-colored mol ratio>=3; Said water-insoluble ionic liquid can be 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]) etc.; Volume ratio>=0.2 of said water-insoluble ionic liquid and nano silver colloidal sol.
The present invention utilizes water-insoluble ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), under the effect of phase transfer reagent softex kw (CTAB), with aqueous phase with the nano-Ag particles of plant reduction method preparation be extracted into ionic liquid mutually in.Technology of the present invention is simple, mild condition.Simultaneously, owing to nano-Ag particles and ionic liquid are in catalysis at present, there is huge application potential in fields such as organic synthesis.Therefore, obtain to have good using value at the nano-Ag particles of ionic liquid in mutually.
Description of drawings
Fig. 1 is embodiment 1,2, the supernatant UV-Vis spectral scan figure before and after 3 extractions.In Fig. 1, abscissa is wavelength wavelength Wavelength (nm), and ordinate is absorbance A bs; Curve a is for before extracting, and curve b is 1L=0.3ml, and curve c is 1L=0.6ml, and curve d is 1L=1.0ml.
Fig. 2 is embodiment 2,4, the supernatant UV-Vis spectral scan figure before and after 5 extractions.In Fig. 2, abscissa is wavelength wavelength Wavelength (nm), and ordinate is absorbance A bs; Curve a is for before extracting, and curve b is CTAB=0, and curve c is CTAB=0.3ml, and curve d is CTAB=0.5ml.
The specific embodiment
Through embodiment the present invention is described further below.
Embodiment 1
Get 2g virtue camphor tree leaf dried powder, add the 100mL deionized water, place shaking bath, 30 ℃ of temperature, rotating speed 180r/min, concussion 5h takes out and is cooled to room temperature, and vacuum filtration obtains the fragrant camphor tree leaf leachate of 20g/L.
Get the fragrant camphor tree leaf leachate that makes more than the 20mL, to wherein adding 200 μ L0.1MAgNO
3Solution, 400 μ L0.1MNaOH solution, the room temperature lower magnetic force stirs, and reaction 6h reacts completely, and obtains the silver sol that concentration is 1mM.
Get the above silver sol 3mL that makes in test tube, to the phase transfer reagent softex kw (CTAB) that wherein adds 0.5mL30mM, again to wherein adding 0.3mL ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), concuss 10s, can the Nano Silver of aqueous phase partly be extracted into ionic liquid mutually in.The UV-Vis spectral scan figure of water supernatant sees Fig. 1 before and after the extraction.
Embodiment 2
Get the nano silver colloidal sol that makes among the 3mL embodiment 1 in test tube, to the phase transfer reagent softex kw (CTAB) that wherein adds 0.5mL30mM, again to wherein adding 0.6mL ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), concuss 10s, can the Nano Silver of aqueous phase all be extracted into ionic liquid mutually in.The UV-Vis spectral scan figure of water supernatant sees Fig. 1 or Fig. 2 before and after the extraction.
Embodiment 3
Get the nano silver colloidal sol that makes among the 3mL embodiment 1 in test tube, to the phase transfer reagent softex kw (CTAB) that wherein adds 0.5mL30mM, again to wherein adding 1.0mL ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), concuss 10s, can the Nano Silver of aqueous phase all be extracted into ionic liquid mutually in.The UV-Vis spectral scan figure of water supernatant sees Fig. 1 before and after the extraction.
Embodiment 4
Get the nano silver colloidal sol that makes among the 3mL embodiment 1 in test tube, under the situation that does not add phase transfer reagent CTAB, to wherein adding 0.6mL ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), concuss 10s, can the Nano Silver of aqueous phase partly be extracted into ionic liquid mutually in.The UV-Vis spectral scan figure of water supernatant sees Fig. 2 before and after the extraction.
Embodiment 5
Get the nano silver colloidal sol that makes among the 3mL embodiment 1 in test tube, to the phase transfer reagent softex kw (CTAB) that wherein adds 0.3mL30mM, again to wherein adding 0.6mL ionic liquid 1-butyl 3-methylimidazole hexafluorophosphate ([Bmim] [PF
6]), concuss 10s, can the Nano Silver of aqueous phase all be extracted into ionic liquid mutually in.The UV-Vis spectral scan figure of water supernatant sees Fig. 2 before and after the extraction.
Claims (9)
1. method of utilizing ion liquid abstraction aqueous phase Nano Silver is characterized in that may further comprise the steps:
1) leaves of plants dry powder is added in the entry, in shaking table, shake, be cooled to room temperature final vacuum suction filtration, get the leaves of plants leachate; Said leaves of plants is fragrant camphor tree leaf;
2) the leaves of plants leachate that step 1) is obtained mixes with alkaline solution and silver salt precursor solution, gets nano silver colloidal sol after the reaction;
3) in step 2) add phase transfer reagent in the nano silver colloidal sol that makes, add water-insoluble ionic liquid again, after the concussion, can with nano-Ag particles be extracted into ionic liquid mutually in; Said phase transfer reagent is a softex kw; Said water-insoluble ionic liquid is a 1-butyl 3-methylimidazole hexafluorophosphate.
2. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 1) said temperature of in shaking table, shaking is 30～60 ℃, and the time of shaking in the shaking table is 2～10h.
3. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 2) in, said alkaline solution is NaOH.
4. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 2) in, said silver salt precursor solution is a liquor argenti nitratis ophthalmicus.
5. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 2) in, said reaction is a magnetic agitation at room temperature, reaction 5～15h.
6. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1; It is characterized in that in step 2) in; Said plant extract concentration is 0.1～20 with the mass concentration ratio of silver, and said alkaline solution molar concentration is 1～40 with the molar concentration rate of silver.
7. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 6 is characterized in that the said alkaline solution molar concentration and the molar concentration rate of silver are 2～20.
8. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 3), said phase transfer reagent and silver-colored mol ratio >=3.
9. a kind of method of utilizing ion liquid abstraction aqueous phase Nano Silver as claimed in claim 1 is characterized in that in step 3), volume ratio >=0.2 of said water-insoluble ionic liquid and nano silver colloidal sol.
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| CN103192091B (en) * | 2013-04-23 | 2015-04-08 | 湖南农业大学 | Method utilizing sloanea sinensis leaves for green synthesis of water-soluble nano-iron |
| CN104084593A (en) * | 2014-07-03 | 2014-10-08 | 北京工业大学 | Method for extracting nano-silver in ionic liquid separation and enrichment liquid |
| CN105040414B (en) * | 2015-05-25 | 2017-05-03 | 厦门大学 | Preparation method of sliver supporting fabric based on plant material and nanometer sliver synergetic antibacterial |
| CN106807935B (en) * | 2015-12-01 | 2019-11-12 | 中国科学院大连化学物理研究所 | A kind of activation method for the gold nano grain protected by organic ligand |
| CN105642911B (en) * | 2016-01-27 | 2018-05-04 | 陕西科技大学 | A kind of synthetic method of nanometer Ag |
| CN106513707B (en) * | 2016-12-07 | 2018-06-08 | 鲁东大学 | A kind of nano silver antibacterial agent and its preparation process using blueberry leaf extract biosynthesis |
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| CN100450677C (en) * | 2006-11-28 | 2009-01-14 | 厦门大学 | Plant reduction method for preparing silver Nano granules and gold Nano granules |
| CA2728987C (en) * | 2008-05-16 | 2018-12-04 | Verutek Technologies, Inc. | Green synthesis of nanometals using plant extracts and use thereof |
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