Preparation of nanosized copper (I) compounds
View Patent ↗A method of making nanosized copper (I) compounds, in particular, copper (I) halides, pseudohalides, and cyanocuprate complexes, in reverse micelles or microemulsions is disclosed herein. The method of the invention comprises (a) dissolving a copper (II) compound in the polar phase of a first reverse micelle or microemulsion, (b) dissolving a copper (II) to copper (I) reducing agent or a pseudohalide salt in the polar phase of a second sample of the same reverse micelle or microemulsion, (c) mixing the two reverse micelle/microemulsions samples to form nanometer sized copper (I) compounds and (d) recovering said nanometer sized copper (I) compounds. The present invention is also directed to the resultant nanosized copper (I) compounds, such as copper (I) chloride, copper (I) cyanide, and potassium cyanocuprate complexes having an average particle size of about 0.1 to 600 nanometers.
1. A method of preparing nanosized copper (I) cyanide comprising the steps of:
providing a first microemulsion having a polar phase to surfactant molar ratio of less than about 30 comprising: a low or non-polar continuous phase comprising a surfactant, and a discontinuous polar phase comprising a copper (II) precursor wherein the discontinuous polar phase comprises nanosized droplets of the copper (II) precursor;
providing a second microemulsion having a polar phase to surfactant molar ratio of less than about 30 comprising: a low or non-polar continuous phase comprising a surfactant, and a discontinuous polar phase comprising a cyanide salt soluble in the polar phase wherein the discontinuous polar phase comprises nanosized droplets of the cyanide salt;
combining the first and second microemulsions to form copper (II) cyanide;
thermally decomposing the copper (II) cyanide to copper (I) cyanide; and
collecting the nanosized copper (I) cyanide having an average particle size of less than 100 nanometers.
2. The method of claim 1 wherein the non-polar phase comprises a compound selected from the group consisting of an alkane, an alkylated benzene and a cyclic siloxane.
3. The method of claim 1 wherein the non-polar phase comprises a cyclic siloxane having the general formula (RR′SiO) n wherein R and R′ are independently selected from the group consisting of methyl, ethyl, phenyl and phenethyl, and n is 3 to 30.
4. The method of claim 1 wherein the non-polar phase comprises a cyclic siloxane having the formula (RR′SiO) n wherein R and R′ are both methyl and n is 4.
5. The method of claim 1 wherein the surfactant is a non-ionic surfactant comprising an alkylphenolalkoxylate.
6. The method of claim 1 wherein the surfactant is a cationic surfactant comprising an alkyl ammonium salt.
7. The method of claim 6 wherein the cationic surfactant is hexadecyltrimethylammonium bromide.
8. The method of claim 1 wherein the surfactant is an anionic surfactant selected from the group consisting of sodium dodecylsulfate and sodium bis(2-ethylhexyl)sulfosuccinate.
9. The method of claim 1 wherein the surfactant is a zwitterionic surfactant selected from the group consisting of 3-(dimethyldodecyl-ammonium)propane sulfonate and cetyltrimethylammonium p-toluene sulfonate.
10. The method of claim 1 wherein the copper (II) precursor comprises CuCl 2 in an aqueous solution.
11. The method of claim 1 wherein the cyanide salt is KCN.