CN1672836A - Water soluble nano metal particle and its prepn process - Google Patents
Water soluble nano metal particle and its prepn process Download PDFInfo
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- CN1672836A CN1672836A CN 200410010149 CN200410010149A CN1672836A CN 1672836 A CN1672836 A CN 1672836A CN 200410010149 CN200410010149 CN 200410010149 CN 200410010149 A CN200410010149 A CN 200410010149A CN 1672836 A CN1672836 A CN 1672836A
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Abstract
The present invention relates to water soluble nanometer metal particle and its preparation process. Water soluble organic compound as modifying agent is made to react with metal surface, and the organic compound as modifying agent has the amount of 5-75 wt%. The present invention prepares nanometer metal particle through complexing reduction process, the nanometer metal particle has small size, homogeneous distribution and excellent dispersivity in water and effectively controllable particle size, and the modifying agent makes the metal particle possess excellent dispersivity and high chemical stability in water. The prepared organic compound modified nanometer metal particle may be used widely in paint, textile, photoelectronic material, catalysis, medicine and other fields.
Description
Technical field
The present invention relates to a kind of metallic nano-particle, relate in particular to a kind of water-soluble metal nanoparticle, the invention still further relates to a kind of preparation method of this water-soluble metal nanoparticle simultaneously.
Background technology
Metal nano material all has broad application prospects in fields such as coating, textile, photoelectric material, catalysis, drug materials as one of nano material important branch, is subjected to paying close attention to widely.At present, the method for preparing nano metal material has multiple, mainly contains sedimentation, electrode method, steams the method, mechanical milling method etc. of crossing.But said method is because required experiment condition strictness, the loaded down with trivial details complexity of process, and energy consumption is big and be difficult for applying, and the nano metal material that makes with said method is not soluble in water, and the dispersive property in water is not good.
Summary of the invention
For addressing the above problem, the object of the present invention is to provide a kind of water-soluble metal nanoparticle.
Simultaneously, the present invention also aims to provide a kind of preparation method of this organic matter modified metal nanoparticle.
In order to achieve the above object, technical program of the present invention lies in providing a kind of water-soluble metal nanoparticle, water-soluble organic compounds interacts as dressing agent and metal surface, and wherein, organic compound modified dose percentage by weight is 5-75%.
Described organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 4-20 carbon atom.
Described organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 10-20 carbon atom.
Described metal can be copper, silver, gold, platinum etc., and metal precursor is a soluble metallic salt.
The mol ratio of organic compound and metal ion is 1: 0.2-10; The concentration of soluble metallic salt in medium is 10-1000mmol/L.
Simultaneously, technical program of the present invention also lies in providing a kind of preparation method of water-soluble metal nanoparticle, this method may further comprise the steps: metal ion forms complex compound earlier, metal precursor is a soluble metallic salt, adding water-soluble organic compounds then, drip reducing agent again, is reaction 0.5-24 hour under 20-80 ℃ the condition in temperature, wherein reaction medium is water or alcohol-water system, can form the metal nanoparticle that the surface contains organic compound.
Organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 4-20 carbon atom.
Reducing agent can be water miscible nitrate, acetate, halide salt or sulfate.
The mol ratio of metal ion and reducing agent is 1: 0.3-5.
Reaction medium can be water or alcohol-water system.
Since the present invention be with the complexing reducing process prepare have particle diameter little, be evenly distributed and the water-soluble metal nanoparticle of good dispersion arranged in water, the formed nano level metal particle of dressing agent and metal complex can be controlled the size of nanoparticle effectively; Simultaneously, dressing agent can make metal particle have good dispersiveness and chemical stability again in water; The organic compound modified metallic nano-particle prepared with method of the present invention can be widely used in fields such as coating, textile, photoelectric material, catalysis, drug material.
Description of drawings
Fig. 1 is the infrared spectrogram of silver nano-grain among the present invention;
Fig. 2 is the XRD figure of silver nano-grain among the present invention;
Fig. 3 is the TEM Electronic Speculum figure of silver nano-grain among the present invention;
Fig. 4 is the infrared spectrogram of copper nano particles among the present invention;
Fig. 5 is the XRD figure of copper nano particles among the present invention;
Fig. 6 is the TEM Electronic Speculum figure of copper nano particles among the present invention;
Fig. 7 is the infrared spectrogram of gold nano grain among the present invention;
Fig. 8 is the XRD figure of gold nano grain among the present invention;
Fig. 9 is the TEM Electronic Speculum figure of gold nano grain among the present invention.
The specific embodiment
Embodiment 1
Get the beaker that 0.1mol/L liquor argenti nitratis ophthalmicus 20ml places 100ml, till the ammoniacal liquor that adds 0.6mol/L then becomes water white transparency to solution, the polyvinylpyrrolidone that adds 0.35g again in solution makes its dissolving, solution is transferred in the there-necked flask, under stirring, the dropping volume is 20ml, concentration is the tan-liquor of 0.01mol/L, under stirring at room, react 45min, leave standstill, filter, precipitate and obtain the pressed powder of black, be polyvinyl pyrrolidon modified silver nano-grain with distilled water washing, vacuum drying.
Get the beaker that 0.1mol/L liquor argenti nitratis ophthalmicus 20ml places 100ml, add then till 0.6mol/L ammoniacal liquor becomes water white transparency to solution, the dodecyl sodium sulfate that adds 0.82g again in solution makes its dissolving; Solution is transferred in the there-necked flask, under stirring, the dropping volume is 20ml, concentration is the tan-liquor of 0.01mol/L, stirring reaction 45min at ambient temperature, leave standstill, filter, precipitate the pressed powder that obtains black with distilled water washing, vacuum drying, be the silver nano-grain that dodecyl sodium sulfate is modified.
The performance parameter of the organic compound modified silver nano-grain that embodiment 1 is prepared is as follows:
The infrared spectrogram of the silver nano-grain that prepared organic is compound-modified (with the test of AVATAR360FT-IR infrared spectrometer) as Fig. 1, has figure as can be known: 1651.06cm
-1The absorption band at place is that carbonylic stretching vibration causes, 1455.43cm
-1, 1420.12cm
-1, 1398.21cm
-1Absorption band belong to the C-H flexural vibrations, more than the analysis showed that and contain PVP (being polyvinylpyrrolidone) in the sample.Because PVP's is water-soluble stronger, if it is not modified at the surface of Nano Silver, PVP can be gone by washing and can not get its infrared ray characteristic spectrum in the sample washing process.Hence one can see that, and PVP and Nano Silver are not simple mixing, but and the surface of Nano Silver stronger suction-operated has taken place.
By x-ray diffraction pattern, be that 2 θ values of sample and 2 θ's XRD figure (see figure 2) (with X ' Pert Pro ' X-ray diffractometer test) on the accurate card of silver label are consistent as can be known, the obvious broadening of while diffraction maximum, this shows that the purpose product that we prepare is not oxidized silver-colored nano microcrystalline, and has face-centred cubic structure.
Can see that from transmission electron microscope (JEM-2010 transmission electron microscope) photo (see figure 3) made Nano Silver is spherical in shape, particle is more even, and particle diameter does not have obvious agglomeration about 10nm.
Dispersed experiment shows that sample has good dispersiveness in water, and this has proved that PVP has been modified at the surface of Nano Silver, thereby has changed silver-colored surface characteristic, makes it that good dispersiveness be arranged in water.
Embodiment 3
The copper-bath 20ml that gets 0.1mol/L places the beaker of 100ml, the ammoniacal liquor that adds 0.6mol/L then, till becoming water white transparency to solution, the polyvinylpyrrolidone that adds 0.35g again in solution makes its dissolving, solution is transferred in the there-necked flask, under stirring, the dropping volume is 20ml, concentration is the hydrazine hydrate aqueous solution of 0.6mol/L, stirring reaction 45min under 50 ℃ temperature conditions leaves standstill, filters, precipitates with distilled water washing, vacuum drying and promptly obtain polyvinyl pyrrolidon modified copper nano particles.
Embodiment 4
The copper-bath 20ml that gets 0.1mol/L places the beaker of 100ml, add 0.6mol/L ammoniacal liquor then, till becoming water white transparency to solution, the dodecyl sodium sulfate that adds 0.82g again in solution makes its dissolving, solution is transferred in the there-necked flask, under stirring, the dropping volume is 20ml, concentration is the hydrazine hydrate aqueous solution of 0.6mol/L, stirring reaction 45min under 50 ℃ temperature conditions leaves standstill, filters, precipitates and obtains the copper nano particles that dodecyl sodium sulfate is modified with distilled water washing, vacuum drying.
The performance parameter of the organic compound modified copper nano particles that embodiment 3 is prepared is as follows:
The infrared spectrogram of the copper nano particles that prepared organic is compound-modified (with the test of AVATAR360FT-IR infrared spectrometer) as Fig. 4, has figure as can be known: 1654.87cm
-1The absorption band at place is that carbonylic stretching vibration causes, 1454.43cm
-1, 1421.76cm
-1, 1374.50cm
-1Absorption band belong to the C-H flexural vibrations, more than the analysis showed that and contain PVP (polyvinylpyrrolidone) in the sample.Because PVP's is water-soluble stronger, if it is not modified at the surface of nanometer copper, PVP can be gone by washing and can not get its infrared ray characteristic spectrum in the sample washing process.Hence one can see that, and PVP and nanometer copper are not simple mixing, but and the surface of nanometer copper stronger suction-operated has taken place.
By x-ray diffraction pattern, be that 2 θ values of sample and 2 θ's XRD figure (with X ' Pert Pro ' X-ray diffractometer test) on the copper standard card are consistent as can be known, the obvious broadening of while diffraction maximum, this shows that the purpose product that we prepare is not oxidized copper nano microcrystalline.
Can see that from transmission electron microscope (JEM-2010 transmission electron microscope) photo (see figure 6) made nanometer copper is spherical in shape, particle is more even, does not have obvious agglomeration.
Dispersed experiment shows that sample has good dispersiveness in water, and this has proved that PVP has been modified at the surface of nanometer copper, thereby has changed the surface characteristic of copper, makes it that good dispersiveness be arranged in water.
Embodiment 5
Get the beaker that 0.01mol/L gold solution chlorate 20ml places 100ml, add then till 0.6mol/L ammoniacal liquor becomes water white transparency to solution, the polyvinylpyrrolidone that adds 0.82g again in solution makes its dissolving, solution is transferred in the there-necked flask, under stirring, drip the NaBH4 aqueous solution of 20ml 0.01mol/L, under 35 ℃ of stirrings, react 45min, leave standstill, filter, precipitate with distilled water washing, vacuum drying and promptly obtain polyvinyl pyrrolidon modified gold nano grain.
Embodiment 6
Get the beaker that 0.01mol/L gold solution chlorate 20ml places 100ml, add 0.6mol/L ammoniacal liquor 20ml then, the dodecyl sodium sulfate that adds 0.82g again in solution makes its dissolving, solution is transferred in the there-necked flask, under stirring, drip the NaBH4 aqueous solution of 20ml 0.01mol/L, under 35 ℃ of stirrings, react 45min, leave standstill, filter, precipitate the gold nano grain that obtains the dodecyl sodium sulfate modification with distilled water washing, vacuum drying.
By x-ray diffraction pattern, be that 2 θ values of sample and 2 θ's XRD figure (with X ' Pert Pro ' X-ray diffractometer test) on the goldstandard card are consistent as can be known, the obvious broadening of while diffraction maximum, this shows that the purpose product that we prepare is not oxidized gold nano crystallite, sees Fig. 8.
Can see that from transmission electron microscope (JEM-2010 transmission electron microscope) photo (see figure 9) made nm of gold is spherical in shape, particle is more even, does not have obvious agglomeration.
Dispersed experiment shows that sample has good dispersiveness in water, and this has proved organic compound modified on the surface of nm of gold, thereby has changed golden surface characteristic, makes it that good dispersiveness be arranged in water.
Claims (10)
1, a kind of water-soluble metal nanoparticle, it is characterized in that: water-soluble organic compounds interacts as dressing agent and metal surface, and wherein, organic compound modified dose percentage by weight is 5-75%.
2, water-soluble metal nanoparticle according to claim 1 is characterized in that: described organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 4-20 carbon atom.
3, water-soluble metal nanoparticle according to claim 2 is characterized in that: described organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 10-20 carbon atom.
4, water-soluble metal nanoparticle according to claim 1 is characterized in that: described metal can be copper, silver, gold, platinum etc., and metal precursor is a soluble metallic salt.
5, water-soluble metal nanoparticle according to claim 1 is characterized in that: the mol ratio of organic compound and metal ion is 1: 0.2-10; The concentration of soluble metallic salt in medium is 10-1000mmol/L.
6, a kind of preparation method of water-soluble metal nanoparticle, it is characterized in that: this method may further comprise the steps: metal ion forms complex compound earlier, metal precursor is a soluble metallic salt, add water-soluble organic compounds then, drip reducing agent again, be reaction 0.5-24 hour under 20-80 ℃ the condition in temperature, wherein reaction medium is water or alcohol-water system, can form the metal nanoparticle that the surface contains organic compound.
7, the preparation method of water-soluble nano particulate according to claim 6 is characterized in that: organic compound is straight chain or the cycloalkyl water-soluble organic compounds that contains 4-20 carbon atom.
8, the preparation method of water-soluble metal nanoparticle according to claim 6 is characterized in that: reducing agent can be water miscible nitrate, acetate, halide salt or sulfate.
9, water-soluble metal method for preparing Nano fine grains according to claim 6 is characterized in that: the mol ratio of metal ion and reducing agent is 1: 0.3-5.
10, water-soluble metal method for preparing Nano fine grains according to claim 6 is characterized in that: reaction medium can be water or alcohol-water system.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103264167A (en) * | 2013-06-09 | 2013-08-28 | 南通众诚生物技术有限公司 | Surface modification nanometer copper particle and preparation method thereof |
| CN103624265A (en) * | 2012-08-21 | 2014-03-12 | 国家纳米科学中心 | Gold nanoparticles and preparation method thereof |
-
2004
- 2004-03-22 CN CN 200410010149 patent/CN1672836A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102202815A (en) * | 2008-05-16 | 2011-09-28 | 维鲁泰克技术股份有限公司 | Green synthesis of nanometals using plant extracts and use thereof |
| CN103624265A (en) * | 2012-08-21 | 2014-03-12 | 国家纳米科学中心 | Gold nanoparticles and preparation method thereof |
| CN103264167A (en) * | 2013-06-09 | 2013-08-28 | 南通众诚生物技术有限公司 | Surface modification nanometer copper particle and preparation method thereof |
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