CN101869989A - Method for preparing water dispersible metal nano-particles - Google Patents
Method for preparing water dispersible metal nano-particles Download PDFInfo
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- CN101869989A CN101869989A CN201010193339A CN201010193339A CN101869989A CN 101869989 A CN101869989 A CN 101869989A CN 201010193339 A CN201010193339 A CN 201010193339A CN 201010193339 A CN201010193339 A CN 201010193339A CN 101869989 A CN101869989 A CN 101869989A
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Abstract
The invention discloses a method for preparing water dispersible metal nano-particles. The method comprises the following steps of: adding metal ions or metal ion complex into nano cellulose dispersion; reducing the metal ions with a reducer under a certain temperature condition; curing the reduced metal ions in reaction liquid for a period of time; and separating the mixed solution by centrifuging and washing the separated product to obtain the water dispersible metal nano-particles. The prepared water dispersible metal nano-particles can be applied in the fields of biology, physics, chemistry, medicine and the like.
Description
Technical field
The present invention relates to a kind of preparation method of water dispersible metal nano-particles, affiliated technical field is the crossing domain of subjects such as material, biology, chemistry.
Technical background
Because the needs of sustainable development and environmental protection; in the past few decades; be subjected to domestic and international researcher and manufacturing enterprise more and more payes attention to based on the biodegradation material of natural reproducible resource, the preparation of nano-cellulose and use and also obtained extensive studies.Nano-cellulose has biocompatibility, biodegradable, advantage such as the preparation method is simple, is normally made by the acid-catalyzed hydrolysis method by native cellulose.Cellulosic chemical constitution be by D-glucopyranose ring each other with β-1, the 4-glycosidic bond connects the linear macromolecule form.1 primary hydroxyl and 2 secondary hydroxyls are arranged in the glucose unit in the cellulosic molecule, and this makes cellulose have good chemical reactivity, and to the suction-operated of metal ion, so nano-cellulose can be used as good dispersant and stabilizing agent.
Metal nanoparticle had obtained application more and more widely in fields such as biology, physics, chemistry, medical science in the last few years.Usually use petrochemical industry based surfactants or high molecular polymer to prepare metal nanoparticle as dispersant and stabilizing agent.Patent CN101497134 and CN101497133 are that dispersant and stabilizing agent prepare noble metal nano particles with the polyethylene glycol; Patent CN1623889 is that protective agent prepares metal nanoparticle with the heteroaromatic compound; Patent CN101070141, CN1986418 and CN101386069 use different types of petroleum chemicals to prepare metal nanoparticle respectively.The metal nanoparticle aqueous dispersion performance of the method for above-mentioned patent report or complex process or preparation is relatively poor.
Exhausted day by day along with petroleum resources sought stabilizing agent and the dispersant that alternative petroleum chemicals are used to prepare metal nanoparticle and had great importance.
Summary of the invention
Prepare the shortcoming of metal nano ion processes complexity, water dispersible difference for what solve that prior art exists with petroleum chemicals, the present invention proposes a kind of preparation method of water dispersible metal nano-particles, the nano-cellulose that uses natural reproducible is as dispersant and stabilizing agent, and technology is simple, water dispersible good.
Technical scheme of the present invention is: a kind of preparation method of water dispersible metal nano-particles, it according to the mass ratio of metal ion or metal ion match and nano-cellulose 1: 300～1: 3 ratio, it is in 0.01%～5% the nano-cellulose dispersion liquid that metal ion or metal ion match are joined mass concentration, mix, under 30～90 ℃, add reducing agent reducing metal ion, and slaking under this temperature, then, centrifugation, washing obtain water dispersible metal nano-particles.
Described nano-cellulose is to be prepared from in cotton fiber, flaxen fiber, wood pulp cellulose, bamboo fibre or the microcrystalline cellulose any one.
Described metal ion or metal ion match are any one in gold, platinum, copper, lead, the nickel, or the ionic complex of gold, platinum, copper, lead, nickel.
Described reducing agent is any one in hydrazine hydrate, sodium borohydride, sodium hypophosphite, natrium citricum or the ascorbic acid.
Metal nanoparticle involved in the present invention refers to the small single metal nanoparticle of particle diameter in 1～100 nanometer, and this metal nanoparticle is difficult for oxidation by air at ambient temperature, and good stable is arranged.
Beneficial effect:
1. the present invention prepares water dispersible metal nano-particles with natural biomass resource nano-cellulose as dispersant and stabilizing agent, and the preparation method is simple, and the metal nanoparticle yardstick is adjustable, has good dispersiveness and stable in water.The method applied in the present invention is simple, cost is low, workable, need not special instrument and equipment.
2. the nano-cellulose of the present invention preparation has characteristics such as disperseing stable homogeneous in good biocompatibility, biodegradable, the water, is particularly useful for the application in biological and medical field.
Description of drawings
Fig. 1 is the micro-structure diagram of the water-dispersion type golden nanometer particle of preparation;
Fig. 2 is the micro-structure diagram of the water-dispersion type nickel nano particle of preparation;
Fig. 3 is the micro-structure diagram of the water-dispersion type copper nano-particle of preparation;
Fig. 4 is the micro-structure diagram of the plumbous nano particle of water-dispersion type of preparation;
Fig. 5 is the micro-structure diagram of the water-dispersion type nano platinum particle of preparation.
The specific embodiment
Following examples are to give an example for more of the present invention, are not limitation of the invention.
The nano-cellulose that uses is laboratory self-control (putting down in writing among preparation method's referenced patent application CN101509209), and other raw materials are all commercially available.
A kind of preparation method of water dispersible metal nano-particles: (1) preparation of nano cellulose aqueous dispersions, the mass concentration of nano-cellulose is between 0.01%～5%; (2) a certain amount of metal ion or metal ion match are joined in the nano-cellulose dispersion liquid, metal ion or metal ion match and cellulosic mass ratio are between 1: 300～1: 3, and mechanical agitation mixes; (3) under 30～90 ℃ of temperature conditions, add reducing agent reducing metal ion, and slaking 10 minutes～2 days under this reaction temperature condition.(4) dispersion liquid after the slaking is carried out centrifugation, washing 1～6 time, obtain water dispersible metal nano-particles.
Above-mentioned nano-cellulose can be with cotton fiber, flaxen fiber, wood pulp cellulose, bamboo fibre or microcrystalline cellulose, the metal ion that adds can be any one metal ion or its complex in gold, platinum, copper, lead or the nickel, the reducing agent that uses can be any one in hydrazine hydrate, sodium borohydride, sodium hypophosphite, natrium citricum or the ascorbic acid, and the consumption of reducing agent is 1.2～5 times of amount of metal ion species.
Embodiment 1:
Configuration 30 gram mass concentration are 0.5% the nano-cellulose suspension by the absorbent cotton preparation in the flask, add the HAuCl of 5 milliliters of 0.1mol/L
4Solution, warming-in-water to 60 ℃ insulation, condensing reflux, and magnetic agitation after 60 minutes, drips the 1mL hydrazine hydrate, slaking 2 hours, the centrifugation golden nanometer particle to product washing 6 times, obtains the water-dispersion type golden nanometer particle, as shown in Figure 1, particle diameter is at 5 ± 2nm, and dispersed as can be seen fine from the figure, the dispersion liquid of preparation 1%wt leaves standstill no obvious sedimentation after month in water.
Embodiment 2:
The nano-cellulose suspension of configuration 600 gram 1%wt in the flask by flax preparation, the Ni (NO of 40 milliliters of 0.5mol/L of adding
3)
3Solution, NaOH transfer solution to alkalescent, warming-in-water to 90 ℃ insulation, condensing reflux, and lasting mechanical agitation drip the 30mL hydrazine hydrate after 30 minutes, slaking 4 hours, the centrifugation nickel nano particle to product washing 3 times, obtains the water-dispersion type nickel nano particle, as shown in Figure 2, particle diameter is below 5nm, and is dispersed as can be seen fine from the figure, and the dispersion liquid of preparation 1%wt leaves standstill no obvious sedimentation after month in water.
Embodiment 3:
The nano-cellulose suspension of configuration 100 gram 2%wt in the flask by the wood pulp preparation, the CuSO of 10 milliliters of 0.2mol/L of adding
4Solution, warming-in-water to 40 ℃ insulation, condensing reflux, and magnetic agitation, drip 10mL sodium borohydride solution (0.01mol/L), slaking 12 hours, centrifugation copper nano-particle after 90 minutes, to product washing 3 times, obtain the water-dispersion type copper nano-particle, as shown in Figure 3, particle diameter is between 20～50nm, dispersed as can be seen fine from the figure, the dispersion liquid of preparation 1%wt leaves standstill no obvious sedimentation after month in water.
Embodiment 4:
The nano-cellulose suspension of configuration 50 gram 4%wt in the flask by the bamboo fibre preparation, the Pb (NO of 5 milliliters of 0.02mol/L of adding
3)
2Solution, warming-in-water to 30 ℃ insulation, and magnetic agitation, Dropwise 5 mL sodium hypophosphite solution (0.01mol/L) after 30 minutes, slaking 3 hours, the plumbous nano particle of centrifugation to product washing 5 times, obtains the plumbous nano particle of water-dispersion type, as shown in Figure 4, particle diameter is about 10nm, and dispersiveness is better as can be seen from figure, and the dispersion liquid of preparation 1%wt leaves standstill no obvious sedimentation after month in water.
Embodiment 5:
Configuration 150 gram mass concentration are the nano-cellulose suspension by the microcrystalline cellulose preparation of 0.01%wt in the flask, add the H of 5 milliliters of 0.1mol/L
2PtCl
6Solution, warming-in-water to 90 ℃ insulation, condensing reflux, and magnetic agitation after 60 minutes, drips 10mL ascorbic acid solution (0.5mol/L), slaking 20 minutes, the centrifugation nano platinum particle to product washing 6 times, obtains the water-dispersion type nano platinum particle, as shown in Figure 5, particle diameter is about 10nm, and dispersiveness is better as can be seen from figure, and the dispersion liquid of preparation 1%wt leaves standstill no obvious sedimentation after month in water.
Claims (4)
1. the preparation method of a water dispersible metal nano-particles, it is characterized in that, it according to the mass ratio of metal ion or metal ion match and nano-cellulose 1: 300～1: 3 ratio, it is in 0.01%～5% the nano-cellulose dispersion liquid that metal ion or metal ion match are joined mass concentration, mix, under 30～90 ℃, add reducing agent reducing metal ion, and slaking under this temperature, then, centrifugation, washing obtain water dispersible metal nano-particles.
2. the preparation method of water dispersible metal nano-particles according to claim 1 is characterized in that, described nano-cellulose is to be prepared from in cotton fiber, flaxen fiber, wood pulp cellulose, bamboo fibre or the microcrystalline cellulose any one.
3. the preparation method of water dispersible metal nano-particles according to claim 1, it is characterized in that, described metal ion or metal ion match are any one in gold, platinum, copper, lead, the nickel, or the ionic complex of gold, platinum, copper, lead, nickel.
4. the preparation method of water dispersible metal nano-particles according to claim 1 is characterized in that, described reducing agent is any one in hydrazine hydrate, sodium borohydride, sodium hypophosphite, natrium citricum or the ascorbic acid.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102493265A (en) * | 2011-12-14 | 2012-06-13 | 南京林业大学 | Method for preparing metal nano particle and cellulose fiber composite material |
| CN102737786A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Preparation method of cellulose nanofiber-based flexible transparent conductive membrane |
| CN103752844A (en) * | 2014-01-08 | 2014-04-30 | 洛阳理工学院 | Preparation method of nano spherical lead powder |
| CN104781081A (en) * | 2012-09-24 | 2015-07-15 | 纸和纤维研究所 | Coating composition of nano cellulose, its uses and a method for its manufacture |
| CN105033281A (en) * | 2015-08-27 | 2015-11-11 | 华南理工大学 | Simple and environment-friendly preparation method for gold nanoparticle solution |
| CN105367828A (en) * | 2015-12-03 | 2016-03-02 | 丁玉琴 | Preparation method for porphyra microcrystalline cellulose/nano platinum composite material |
| CN105899313A (en) * | 2013-11-01 | 2016-08-24 | 科学与工业研究理事会 | A process for the preparation of metal nanoparticles |
| CN107252703A (en) * | 2017-06-27 | 2017-10-17 | 南京林业大学 | It is a kind of to have efficiently except cellulose base catalyst of formaldehyde effect and preparation method thereof |
| CN110653379A (en) * | 2018-06-28 | 2020-01-07 | 宁波山功新材料科技有限公司 | Preparation method of degradable metal nanowires |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN101077528A (en) * | 2006-05-26 | 2007-11-28 | 徐健宏 | Process for manufactruing superfine nano noble metal solution |
| CN101352760A (en) * | 2007-07-23 | 2009-01-28 | 三星电机株式会社 | Method for manufacturing nickel nanoparticles |
| CN101450385A (en) * | 2008-12-30 | 2009-06-10 | 天津大学 | Nano silver colloid aqueous solution preparation method using sodium cellulose glycolate |
| CN101509209A (en) * | 2009-03-10 | 2009-08-19 | 中国林业科学研究院林产化学工业研究所 | Method of preparing clubbed nano-cellulose |
-
2010
- 2010-06-03 CN CN201010193339A patent/CN101869989A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1583332A (en) * | 2004-06-08 | 2005-02-23 | 陈丽琼 | Nanometer silver sol and preparing method thereof |
| CN101077528A (en) * | 2006-05-26 | 2007-11-28 | 徐健宏 | Process for manufactruing superfine nano noble metal solution |
| CN101352760A (en) * | 2007-07-23 | 2009-01-28 | 三星电机株式会社 | Method for manufacturing nickel nanoparticles |
| CN101450385A (en) * | 2008-12-30 | 2009-06-10 | 天津大学 | Nano silver colloid aqueous solution preparation method using sodium cellulose glycolate |
| CN101509209A (en) * | 2009-03-10 | 2009-08-19 | 中国林业科学研究院林产化学工业研究所 | Method of preparing clubbed nano-cellulose |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102493265A (en) * | 2011-12-14 | 2012-06-13 | 南京林业大学 | Method for preparing metal nano particle and cellulose fiber composite material |
| CN102493265B (en) * | 2011-12-14 | 2014-04-02 | 南京林业大学 | Method for preparing metal nano particle and cellulose fiber composite material |
| CN102737786A (en) * | 2012-06-28 | 2012-10-17 | 北京理工大学 | Preparation method of cellulose nanofiber-based flexible transparent conductive membrane |
| CN104781081A (en) * | 2012-09-24 | 2015-07-15 | 纸和纤维研究所 | Coating composition of nano cellulose, its uses and a method for its manufacture |
| CN105899313A (en) * | 2013-11-01 | 2016-08-24 | 科学与工业研究理事会 | A process for the preparation of metal nanoparticles |
| CN103752844A (en) * | 2014-01-08 | 2014-04-30 | 洛阳理工学院 | Preparation method of nano spherical lead powder |
| CN105033281A (en) * | 2015-08-27 | 2015-11-11 | 华南理工大学 | Simple and environment-friendly preparation method for gold nanoparticle solution |
| CN105033281B (en) * | 2015-08-27 | 2017-10-20 | 华南理工大学 | A kind of preparation method of simple environment protection type nanogold particle solution |
| CN105367828A (en) * | 2015-12-03 | 2016-03-02 | 丁玉琴 | Preparation method for porphyra microcrystalline cellulose/nano platinum composite material |
| CN107252703A (en) * | 2017-06-27 | 2017-10-17 | 南京林业大学 | It is a kind of to have efficiently except cellulose base catalyst of formaldehyde effect and preparation method thereof |
| CN110653379A (en) * | 2018-06-28 | 2020-01-07 | 宁波山功新材料科技有限公司 | Preparation method of degradable metal nanowires |
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Application publication date: 20101027 |