CN1766008A - The preparation method of nano copper composition protected by organic monomolecular layer - Google Patents
The preparation method of nano copper composition protected by organic monomolecular layer Download PDFInfo
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- CN1766008A CN1766008A CN 200410090209 CN200410090209A CN1766008A CN 1766008 A CN1766008 A CN 1766008A CN 200410090209 CN200410090209 CN 200410090209 CN 200410090209 A CN200410090209 A CN 200410090209A CN 1766008 A CN1766008 A CN 1766008A
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- monomolecular layer
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- copper composition
- organic monomolecular
- nano copper
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Abstract
The invention discloses a kind of preparation method of nano copper composition protected by organic monomolecular layer.This preparation method is with common mantoquita, the aqueous solution of cation quaternary ammonium salt type surfactant, mixes with the benzole soln of sulfocompound, passes through NaBH
4The aqueous solution carry out chemical reduction, single step reaction generates nano copper composition protected by organic monomolecular layer, the nano particle diameter that makes little (2-10nm), is evenly distributed, and good dispersiveness is arranged in non-polar solvent; The present invention has raw material and is easy to get, and apparatus and process is simple, need not heating, and is fast efficient, and characteristics such as productive rate height are fit to large-scale commercial production.
Description
Technical field
The present invention relates to a kind of preparation method of nano copper composition protected by organic monomolecular layer.
Background technology
Copper nanometer materials and mixture thereof are little owing to having size, specific surface area reaches characteristics such as quantum size effect and macro quanta tunnel effect greatly, make it light, electricity, magnetic and chemical aspect represented novel characteristic, the research of therefore relevant in recent years preparation, performance and the application to the copper nano material at home and abroad is subjected to paying close attention to widely always.Wherein protected by organic monomolecular layer nano particle (MPC) is different from traditional colloid and with the nano particle of other method preparation; it normally uses organic molecule as part; condensed phase and organic molecule pass through the supramolecular system that covalently or non-covalently of bonding assembling forms, and wherein the character of each component remains unaffected substantially.MPC can separate from solvent and disperse repeatedly, can not produce irreversible reunion and decomposition.The present preparation method of MPC carries out in organic phase, and its condition harshness and productive rate are lower.So development process is simple, the preparation method of the protected by organic monomolecular layer copper nano-complex of higher yields, prepares protected by organic monomolecular layer copper nano-complex for suitability for industrialized production, has important significance for theories and practical value.
Summary of the invention
The objective of the invention is to overcome existence condition harshness in the MPC technology of preparing in the past, deficiency that productive rate is lower, provide that a kind of technology is simple, the preparation method of the nano copper composition protected by organic monomolecular layer of higher yields.
The present invention can realize by following measure:
A kind of preparation method of nano copper composition protected by organic monomolecular layer is characterized in that this method specifically may further comprise the steps:
A, soluble copper salt, cation quaternary ammonium salt type surfactant are dissolved in the water, mix with the benzole soln of sulfocompound again, add NaBH
4The aqueous solution, stirring at room reaction 1-4 hour; Soluble copper salt is selected from copper sulfate; Cation quaternary ammonium salt type surfactant is selected from a kind of in Trimethyllaurylammonium bromide, the cetyl trimethylammonium bromide; Sulfocompound is selected from a kind of in lauryl mercaptan, double hexadecyl phosphorodithioic acid, the two dodecyl phosphorodithioic acid;
B, will react back liquid standing separation, get upper organic phase, after the underpressure distillation, 80 ℃ of oven dry of vacuum, the gained brown solid is nano copper composition.
The mol ratio of mantoquita and sulfocompound is 1: 0.5～3 among the present invention.
The mol ratio of mantoquita and cation quaternary ammonium salt type surfactant is 1: 0.3～2.5 among the present invention.
Compare with the technology of preparing of existing nano copper composition protected by organic monomolecular layer, this preparation method has characteristics such as raw material is cheap and easy to get, easy, cost is low, productive rate height, is fit to large-scale industrial production; Prepared nano copper composition protected by organic monomolecular layer particle diameter is even, and it is stable in the air, can stable dispersion in industrial non-polar organic solvents such as multiple lubricant base and benzene, sherwood oil, thereby have the wide industrial purposes.
Description of drawings
Fig. 1 is for being the transmission electron micrograph of the prepared nano copper composition protected by organic monomolecular layer of raw material with the lauryl mercaptan, and wherein scale length is 50nm.
Fig. 2 is for being the ED electron diffraction ring of the prepared nano copper composition protected by organic monomolecular layer of raw material with the lauryl mercaptan.
Fig. 3 is that wherein scale length is 50nm with the transmission electron micrograph of the prepared nano copper composition protected by organic monomolecular layer of two dodecyl phosphorodithioic acid raw materials.
Fig. 4 is for being the transmission electron micrograph of the prepared nano copper composition protected by organic monomolecular layer of raw material with the double hexadecyl phosphorodithioic acid, and wherein scale length is 100nm.
Embodiment
Embodiment 1:
Get 0.6M Cu
2SO
4.5H
2O solution 15ml adds the Trimethyllaurylammonium bromide of 0.05mol, stirs and makes its dissolving, and is stand-by;
The benzole soln 50ml that gets the 0.3M lauryl mercaptan adds in the above-mentioned solution, adds 1MNaBH
4Aqueous solution 60ml, react and tell organic phase after 2 hours, underpressure distillation, 80 ℃ of oven dry of vacuum.
Fig. 1 is the transmission electron micrograph of prepared nano copper composition protected by organic monomolecular layer, can see that prepared nano particle diameter is even, does not have and reunites, particle diameter 2-4nm.Figure two is prepared nano particle electron-diffraction diagram, contains the copper of face-centered cubic crystalline form in the prepared as seen from the figure protected by organic monomolecular layer nano-complex.
Embodiment 2:
Get 0.6M Cu
2SO
4.5H
2O solution 15ml adds the cetyl trimethylammonium bromide of 0.05mol, stirs and makes its dissolving, and is stand-by;
The benzole soln 50ml that gets 0.3M double hexadecyl phosphorodithioic acid adds in the above-mentioned solution, adds 1M NaBH
4Aqueous solution 60ml, react and tell organic phase after 2 hours, underpressure distillation, 80 ℃ of oven dry of vacuum.
Fig. 3 is the transmission electron micrograph of prepared nano copper composition protected by organic monomolecular layer, can see that prepared nano particle diameter is even, does not have and reunites, particle diameter 4-7nm.
Embodiment 3:
Get 0.6M Cu
2SO
4.5H
2O solution 15ml adds the cetyl trimethylammonium bromide of 0.05mol, stirs and makes its dissolving, and is stand-by;
The benzole soln 50ml that gets the two dodecyl phosphorodithioic acid of 0.3M adds in the above-mentioned solution, adds 1M NaBH
4Aqueous solution 60ml, react and tell organic phase after 2 hours, underpressure distillation, 80 ℃ of oven dry of vacuum.
Fig. 4 is the transmission electron micrograph of prepared nano copper composition protected by organic monomolecular layer, can see that prepared nano particle diameter is even, does not have and reunites, particle diameter 7-10nm.
Claims (3)
1, a kind of preparation method of nano copper composition protected by organic monomolecular layer is characterized in that this method specifically may further comprise the steps:
A, soluble copper salt, cation quaternary ammonium salt type surfactant are dissolved in the water, mix with the benzole soln of sulfocompound again, add NaBH
4The aqueous solution, stirring at room reaction 1-4 hour; Soluble copper salt is selected from copper sulfate; Cation quaternary ammonium salt type surfactant is selected from a kind of in Trimethyllaurylammonium bromide, the cetyl trimethylammonium bromide; Sulfocompound is selected from a kind of in lauryl mercaptan, double hexadecyl phosphorodithioic acid, the two dodecyl phosphorodithioic acid;
B, will react back liquid standing separation, get upper organic phase, after the underpressure distillation, 80 ℃ of oven dry of vacuum, the gained brown solid is nano copper composition.
2, as the said method of claim 1, the mol ratio that it is characterized in that mantoquita and sulfocompound is 1: 0.5～3.
3, as the said method of claim 1, the mol ratio that it is characterized in that mantoquita and cation quaternary ammonium salt type surfactant is 1: 0.3～2.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN 200410090209 CN1766008A (en) | 2004-10-26 | 2004-10-26 | The preparation method of nano copper composition protected by organic monomolecular layer |
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| CN 200410090209 CN1766008A (en) | 2004-10-26 | 2004-10-26 | The preparation method of nano copper composition protected by organic monomolecular layer |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883894B (en) * | 2006-06-13 | 2010-06-16 | 上海大不同木业科技有限公司 | Mixture containing nano copper compound and process for preparing same |
| CN102791404A (en) * | 2010-03-24 | 2012-11-21 | Dic株式会社 | Complex of organic compound and copper nanoparticles, complex of organic compound and copper oxide (I) nanoparticles, and processes for production of the complexes |
| CN103755610A (en) * | 2014-01-13 | 2014-04-30 | 上海交通大学 | Thiol metal nanoparticle compound |
| WO2021012754A1 (en) * | 2019-07-23 | 2021-01-28 | 富兰克科技（深圳）股份有限公司 | Preparation method of self-dispersing nano copper with long organice carbon chain, nano copper preparation and application thereof |
-
2004
- 2004-10-26 CN CN 200410090209 patent/CN1766008A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1883894B (en) * | 2006-06-13 | 2010-06-16 | 上海大不同木业科技有限公司 | Mixture containing nano copper compound and process for preparing same |
| CN102791404A (en) * | 2010-03-24 | 2012-11-21 | Dic株式会社 | Complex of organic compound and copper nanoparticles, complex of organic compound and copper oxide (I) nanoparticles, and processes for production of the complexes |
| CN102791404B (en) * | 2010-03-24 | 2014-07-09 | Dic株式会社 | Complex of organic compound and copper nanoparticles, complex of organic compound and copper oxide (I) nanoparticles, and processes for production of the complexes |
| CN103755610A (en) * | 2014-01-13 | 2014-04-30 | 上海交通大学 | Thiol metal nanoparticle compound |
| WO2021012754A1 (en) * | 2019-07-23 | 2021-01-28 | 富兰克科技（深圳）股份有限公司 | Preparation method of self-dispersing nano copper with long organice carbon chain, nano copper preparation and application thereof |
| CN112296345A (en) * | 2019-07-23 | 2021-02-02 | 富兰克科技（深圳）股份有限公司 | Preparation method of self-dispersible nano-copper with long organic carbon chain, nano-copper preparation and application thereof |
| CN112296345B (en) * | 2019-07-23 | 2022-02-18 | 富兰克科技（深圳）股份有限公司 | Preparation method of self-dispersible nano-copper with long organic carbon chain, nano-copper preparation and application thereof |
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