CN102371358A - Aqueous-phase preparation method for re-dispersible nano-copper particles - Google Patents
Aqueous-phase preparation method for re-dispersible nano-copper particles Download PDFInfo
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- 229910052802 copper Inorganic materials 0.000 title claims abstract description 44
- 239000010949 copper Substances 0.000 title claims abstract description 44
- 239000002245 particle Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000008346 aqueous phase Substances 0.000 title claims abstract description 6
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 claims abstract description 10
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000003381 stabilizer Substances 0.000 claims abstract description 8
- 239000003223 protective agent Substances 0.000 claims abstract description 7
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 5
- 238000009835 boiling Methods 0.000 claims abstract description 5
- 239000003960 organic solvent Substances 0.000 claims abstract description 5
- 150000001879 copper Chemical class 0.000 claims abstract 7
- 239000002244 precipitate Substances 0.000 claims abstract 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract 2
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 6
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims description 6
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical group OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims description 4
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 4
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 4
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 4
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 239000004310 lactic acid Substances 0.000 claims description 3
- 235000014655 lactic acid Nutrition 0.000 claims description 3
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 claims description 2
- IKHGUXGNUITLKF-XPULMUKRSA-N acetaldehyde Chemical compound [14CH]([14CH3])=O IKHGUXGNUITLKF-XPULMUKRSA-N 0.000 claims description 2
- ARUVKPQLZAKDPS-UHFFFAOYSA-L copper(II) sulfate Chemical compound [Cu+2].[O-][S+2]([O-])([O-])[O-] ARUVKPQLZAKDPS-UHFFFAOYSA-L 0.000 claims description 2
- DYROSKSLMAPFBZ-UHFFFAOYSA-L copper;2-hydroxypropanoate Chemical compound [Cu+2].CC(O)C([O-])=O.CC(O)C([O-])=O DYROSKSLMAPFBZ-UHFFFAOYSA-L 0.000 claims description 2
- 239000006185 dispersion Substances 0.000 claims description 2
- 239000012046 mixed solvent Substances 0.000 claims description 2
- 229910001379 sodium hypophosphite Inorganic materials 0.000 claims description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 claims 2
- 229910000365 copper sulfate Inorganic materials 0.000 claims 1
- OPQARKPSCNTWTJ-UHFFFAOYSA-L copper(ii) acetate Chemical compound [Cu+2].CC([O-])=O.CC([O-])=O OPQARKPSCNTWTJ-UHFFFAOYSA-L 0.000 claims 1
- 238000000354 decomposition reaction Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 13
- 239000000243 solution Substances 0.000 abstract description 13
- 239000011259 mixed solution Substances 0.000 abstract description 3
- 238000010438 heat treatment Methods 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- MCSXGCZMEPXKIW-UHFFFAOYSA-N 3-hydroxy-4-[(4-methyl-2-nitrophenyl)diazenyl]-N-(3-nitrophenyl)naphthalene-2-carboxamide Chemical compound Cc1ccc(N=Nc2c(O)c(cc3ccccc23)C(=O)Nc2cccc(c2)[N+]([O-])=O)c(c1)[N+]([O-])=O MCSXGCZMEPXKIW-UHFFFAOYSA-N 0.000 abstract 1
- YSVZGWAJIHWNQK-UHFFFAOYSA-N [3-(hydroxymethyl)-2-bicyclo[2.2.1]heptanyl]methanol Chemical compound C1CC2C(CO)C(CO)C1C2 YSVZGWAJIHWNQK-UHFFFAOYSA-N 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000013049 sediment Substances 0.000 description 3
- 238000005406 washing Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000002045 lasting effect Effects 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000013013 elastic material Substances 0.000 description 1
- 238000005868 electrolysis reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 230000009931 harmful effect Effects 0.000 description 1
- 238000009766 low-temperature sintering Methods 0.000 description 1
- 238000003701 mechanical milling Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000012279 sodium borohydride Substances 0.000 description 1
- 229910000033 sodium borohydride Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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Abstract
本发明属于纳米材料技术领域，具体为一种可再分散的纳米铜粒子的水相制备方法。本发明将铜盐和混合的有机保护剂溶解于水或者水和有机溶剂的混合溶液中，在氨水和还原剂作用下，得到深红色溶液，将溶液离心得到沉淀，沉淀物在甲醇中超声洗涤，得到纳米铜粒子。经过清洗的铜纳米粒子能在低沸点稳定剂的帮助下，再分散于溶剂中，纳米铜粒径小于30nm。本发明方法工艺简单，不需加热，成本低；使用水作溶剂，更环保；适合大规模的制备纳米铜粒子。
The invention belongs to the technical field of nanometer materials, in particular to an aqueous phase preparation method of redispersible nanometer copper particles. In the present invention, the copper salt and the mixed organic protective agent are dissolved in water or a mixed solution of water and an organic solvent, under the action of ammonia water and a reducing agent, a deep red solution is obtained, the solution is centrifuged to obtain a precipitate, and the precipitate is ultrasonically washed in methanol , to obtain copper nanoparticles. The cleaned copper nanoparticles can be redispersed in a solvent with the help of a low boiling point stabilizer, and the diameter of the nano copper particles is less than 30nm. The method of the invention has simple process, does not need heating, and has low cost; uses water as a solvent, is more environmentally friendly; and is suitable for large-scale preparation of nanometer copper particles.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of aqueous phase preparation method of redispersible nanometer copper particle.
Background technology
Nanometer copper surface-active is big, has excellent catalytic performance and bactericidal property; Nanometer copper has the ultra ductility of moulding, and this mechanical property provides advantage for the elastic material of making under the normal temperature; Nanometer copper has high electric conductivity, operational stability and chilling process ability in addition, thereby in fields such as electrically conductive ink, conducting resinls good application prospects is arranged.At present, the method for preparing nanometer copper particle mainly contains chemical reduction method, electrolysis, mechanical milling method, steam condensation method, arc plasma process etc.With respect to gold and Nano silver grain; The nanometer copper activity is higher; Be prone to oxidizedly, thereby the surface protection for preparing in the process at nanometer copper particle is extremely important, but a large amount of stabilizing agents can bring harmful effect to the low-temperature sintering performance and the electric conductivity of nanometer copper particle; Therefore, selection of stabilizers and removing method have significant effects for the preparation and the application of nanometer copper particle.Chinese patent 200610104573.4 discloses a kind of preparation method of stabilized nano copper particle: it uses copper nitrate as presoma; Softex kw and sulfur compound are stabilizing agent, and sodium borohydride is a reducing agent, in the solution of second alcohol and water, has synthesized copper nano-particle; Owing to add sulfur compound; And use chloroform extraction, the preparation process is complicated, and product purity is not high.Chinese patent 200910054883.3 discloses a kind of preparation method of nanometer copper particle; Use mantoquita, stabilizing agent and reducing agent, synthesized copper nano-particle under the condition that in organic solvent, heats, be reflected in the organic solvent and carry out; Need heating; The process relative complex needs to use ethanol and acetone repeatedly to clean, and can cause the oxidation of nanometer copper in the process.
Summary of the invention
The objective of the invention is to overcome the too loaded down with trivial details deficiency of aforementioned nanometer copper particle preparation technology, the short-cut method of the redispersible nanometer copper particle of a kind of preparation of water is provided.
The redispersible nanometer copper particle aqueous phase preparation method that the present invention proposes, concrete steps are following:
(1) mantoquita and organic protective agent are dissolved in the solvent, at room temperature stirred 15-25 minute, add ammoniacal liquor, solution becomes dark blue purple from blue stain, continues to stir 50-60 minute;
(2) feed nitrogen, protection dropwise adds reducing agent then, continues stirring reaction 30-40 minute, obtains dark red solution;
(3) with above-mentioned solution centrifugal, obtain deposition, sediment is supersound washing in methyl alcohol, promptly obtains nanometer copper particle.
Among the present invention, the solvent of use is a water, or the mixture of water and ethanol, EGME etc. the organic solvent that can dissolve each other with water, and amount of solvent is the corresponding 50-100ml of every 0.01mol mantoquita.
Among the present invention, the mantoquita that uses is a kind of in the mantoquitas such as Schweinfurt green, copper lactate, copper nitrate, copper sulphate or several kinds mixture wherein.
Among the present invention; The reducing agent that uses can be organic reducing agents such as hydrazine hydrate, formaldehyde or acetaldehyde, perhaps is inorganic reducing agents such as sodium hypophosphite, and reducing agent itself is easier to water-soluble; More soluble in water or the methyl alcohol of product after it is oxidized, the mol ratio 2:1-4:1 of reducing agent and mantoquita.
Among the present invention, the protective agent that uses is the mixture of two kinds in the organic matters such as polyvinylpyrrolidone, softex kw, nation of department 80 or two or more compositions, can water-soluble and methyl alcohol.The mol ratio of used protective agent and mantoquita is 1:1-10:1.
Among the present invention, the nanometer copper particle that obtains, particle diameter is less than 30nm.
The copper nano-particle that obtains among the present invention is lower than at boiling points such as lactic acid, softex kws in the presence of 250 ℃ the stabilizing agent; Can be dispersed in the lower boiling mixed solvents such as ethanol, methyl alcohol, EGME again; Nanometer shot copper footpath after the dispersion is suitable for the application of multiple occasions such as electrically conductive ink less than 30nm.
The present invention has the following advantages:
1, technology is simple, need not heat, and the reaction time is short;
2, last handling process is easy, only uses washed with methanol just can remove the most of material that adds when synthesizing;
3, water is as solvent, and more environmental protection is fit to the preparation water-soluble conducting ink;
4, the copper nano-particle after the cleaning can be scattered in the solvent that contains stabilizing agent again, and the footpath of the nanometer shot copper after disperseing is fit to the application of multiple occasion less than 30nm.
Description of drawings
Fig. 1 is the transmission electron microscope photo (TEM) of nanometer copper particle.
Fig. 2 is the XRD figure of centrifugal, dry back nanometer copper particle.
The specific embodiment
The invention is further illustrated by the following examples.
Embodiment 1: the 0.01mol Schweinfurt green is dissolved in the 50ml water, adds 5g polyvinylpyrrolidone and 1g softex kw, after the stirring and dissolving; Continue to stir 20 minutes, add ammoniacal liquor then, solution becomes dark blue purple from blue stain; Continue to stir 50-60 minute, feed nitrogen protection, dropwise add the 10ml hydrazine hydrate again; Obtained dark red solution in lasting stirring reaction 30-40 minute afterwards; Solution centrifugal is obtained deposition, and sediment supersound washing 1 time in methyl alcohol promptly obtains nanometer copper particle.
Embodiment 2: the 0.01mol Schweinfurt green is dissolved in the mixed solution of 25ml water and 25ml ethanol, adds 5g polyvinylpyrrolidone and 1g softex kw, after the stirring and dissolving; Continue to stir 20 minutes, add ammoniacal liquor then, solution becomes dark blue purple from blue stain; Continue to stir 50-60 minute, feed nitrogen protection, dropwise add the 10ml hydrazine hydrate again; Obtained dark red solution in lasting stirring reaction 30-40 minute afterwards; Solution centrifugal is obtained deposition, and sediment supersound washing 1 time in methyl alcohol promptly obtains nanometer copper particle.
Embodiment 3: get 0.3g through washed with methanol, dried copper nano-particle, join in the mixed solution of 50ml ethanol and 1ml lactic acid, ultrasonic 2-3 minute, copper nano-particle was dispersed in the solution, and particle diameter is less than 30nm.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102601383A (en) * | 2012-03-30 | 2012-07-25 | 电子科技大学 | Method for preparing ultrafine copper powder at room temperature |
| CN102898887A (en) * | 2012-10-12 | 2013-01-30 | 复旦大学 | Method for preparing organic copper salt ink and copper conductive film |
| CN103752844A (en) * | 2014-01-08 | 2014-04-30 | 洛阳理工学院 | Preparation method of nano spherical lead powder |
| CN104289727A (en) * | 2014-10-22 | 2015-01-21 | 苏州正业昌智能科技有限公司 | Method for preparing nano-silver by taking modified chitosan as reducing agent |
| CN107020389A (en) * | 2017-04-06 | 2017-08-08 | 江苏大学 | A kind of preparation method of high-dispersion nano copper |
| CN108079991A (en) * | 2017-12-26 | 2018-05-29 | 扬州大学 | A kind of preparation method and applications of the monodispersed loaded nano copper catalyst of standard |
| CN108315771A (en) * | 2018-02-11 | 2018-07-24 | 中国工程物理研究院材料研究所 | A kind of electrochemical preparation method of sub-nanometer size copper particle elctro-catalyst |
| CN110586952A (en) * | 2018-06-22 | 2019-12-20 | 天津理工大学 | Room temperature preparation method of nano metal powder and conductive ink thereof |
| CN112916864A (en) * | 2021-01-21 | 2021-06-08 | 范期奎 | Water-phase copper nanocrystal and preparation method and application thereof |
| CN114210972A (en) * | 2021-11-03 | 2022-03-22 | 中科检测技术服务(重庆)有限公司 | Novel nano copper welding material |
| CN116041749A (en) * | 2023-02-08 | 2023-05-02 | 高梵(浙江)信息技术有限公司 | Nano antibacterial and deodorant masterbatch for down jacket and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102601383A (en) * | 2012-03-30 | 2012-07-25 | 电子科技大学 | Method for preparing ultrafine copper powder at room temperature |
| CN102898887A (en) * | 2012-10-12 | 2013-01-30 | 复旦大学 | Method for preparing organic copper salt ink and copper conductive film |
| CN103752844A (en) * | 2014-01-08 | 2014-04-30 | 洛阳理工学院 | Preparation method of nano spherical lead powder |
| CN104289727A (en) * | 2014-10-22 | 2015-01-21 | 苏州正业昌智能科技有限公司 | Method for preparing nano-silver by taking modified chitosan as reducing agent |
| CN107020389A (en) * | 2017-04-06 | 2017-08-08 | 江苏大学 | A kind of preparation method of high-dispersion nano copper |
| CN108079991A (en) * | 2017-12-26 | 2018-05-29 | 扬州大学 | A kind of preparation method and applications of the monodispersed loaded nano copper catalyst of standard |
| CN108315771A (en) * | 2018-02-11 | 2018-07-24 | 中国工程物理研究院材料研究所 | A kind of electrochemical preparation method of sub-nanometer size copper particle elctro-catalyst |
| CN110586952A (en) * | 2018-06-22 | 2019-12-20 | 天津理工大学 | Room temperature preparation method of nano metal powder and conductive ink thereof |
| CN112916864A (en) * | 2021-01-21 | 2021-06-08 | 范期奎 | Water-phase copper nanocrystal and preparation method and application thereof |
| CN114210972A (en) * | 2021-11-03 | 2022-03-22 | 中科检测技术服务(重庆)有限公司 | Novel nano copper welding material |
| CN114210972B (en) * | 2021-11-03 | 2023-04-14 | 中科检测技术服务(重庆)有限公司 | Preparation method of novel nano copper welding material |
| CN116041749A (en) * | 2023-02-08 | 2023-05-02 | 高梵(浙江)信息技术有限公司 | Nano antibacterial and deodorant masterbatch for down jacket and preparation method thereof |
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Application publication date: 20120314 |