Method of preparing cerium dioxide nanoparticles
View Patent ↗A method of making cerium dioxide nanoparticles includes: a) providing an aqueous reaction mixture having a source of cerous ion, a source of hydroxide ion, a nanoparticle stabilizer, and an oxidant at an initial temperature no higher than about 20° C.; b) mechanically shearing the mixture and causing it to pass through a perforated screen, thereby forming a suspension of cerium hydroxide nanoparticles; and c) raising the initial temperature to achieve oxidation of cerous ion to eerie ion and thereby form cerium dioxide nanoparticles having a mean diameter in the range of about 1 nm to about 15 nm. The cerium dioxide nanoparticles may be formed in a continuous process.
1. A process for making cerium dioxide nanoparticles comprising the steps of:
providing an aqueous reaction mixture comprising a source of cerous ion, a source of hydroxide ion, a water soluble nanoparticle stabilizer comprising an alkoxylated carboxylic acid, or salt thereof, and an oxidant; and
providing temperature conditions effective to enable oxidation of cerous ion to ceric ion, wherein said temperature conditions effective to enable oxidation of cerous ion to ceric ion comprise a temperature less than 100° C., thereby forming a product dispersion comprising cerium dioxide nanoparticles, wherein said nanoparticles are characterized by a crystalline cubic fluorite structure,
wherein said water soluble nanoparticle stabilizer comprises a compound of formula (Ia),
R—O—(CH 2 CH 2 O) n CHR 1 CO 2 Y (Ia)
wherein:
R represents a methyl group or an ethyl group;
R 1 represents hydrogen or an alkyl group;
Y represents H or a counterion; and
n is 0-5.
2. The process according to claim 1 , wherein R represents a methyl or ethyl group, R 1 represents hydrogen, and n is 1-2.
3. The process according to claim 2 , wherein R represents a methyl group.
4. The process according to claim 1 , wherein said water soluble nanoparticle stabilizer is 2-[2-(2-methoxyethoxy)ethoxy]acetic acid.
5. The process according to claim 1 , wherein said source of cerous ion comprises cerous nitrate.
6. The process according to claim 1 , wherein said temperature conditions effective to enable oxidation of cerous ion to ceric ion comprise a temperature from about 60° C. to about 90° C.
7. The process according to claim 1 , wherein the pH of said reaction mixture is less than or equal to 7.
8. The process according to claim 1 , wherein the pH of said reaction mixture is less than or equal to about 5.
9. The process according to claim 1 , wherein said oxidant is hydrogen peroxide or molecular oxygen.
10. The process according to claim 1 , further comprising the step:
mechanically shearing said reaction mixture and causing it to pass through a perforated screen.
11. A process for forming a homogeneous mixture containing cerium dioxide nanoparticles, at least water soluble one nanoparticle stabilizer, a surfactant, water, and a nonpolar solvent, said process comprising the steps of:
a) providing an aqueous mixture including stabilized cerium dioxide nanoparticles produced according to the process of claim 1 ;
b) concentrating said aqueous mixture including stabilized cerium dioxide nanoparticles to form an aqueous concentrate; and
c) combining said concentrate with said surfactant and said nonpolar solvent, thereby forming said homogeneous mixture,
wherein said water soluble nanoparticle stabilizer comprises a compound of formula (Ia),
R—O—(CH 2 CH 2 O) n CHR 1 CO 2 Y (Ia)
wherein:
R represents a methyl group or an ethyl group;
R 1 represents hydrogen or an alkyl group;
Y represents H or a counterion; and
n is 0-5.
12. The process according to claim 11 , wherein said water soluble nanoparticle stabilizer is 2-[2-(2-methoxyethoxy)ethoxy]acetic acid.
13. The process according to claim 11 , wherein said surfactant comprises an anionic surfactant selected from a fatty acid, sodium bis(2-ethyl-1-hexyl)sulfosuccinate, or combinations thereof.
14. The process according to claim 11 , wherein said concentrating said aqueous mixture is carried out using diafiltration to produce said aqueous concentrate.
15. The process according to claim 14 , wherein said aqueous concentrate is characterized by a conductivity of about 5 mS/cm or less.
16. The process according to claim 11 , further comprising the step of:
d) diluting one part of said homogeneous mixture with at least about 100 parts of a fuel.
17. The process according to claim 1 , wherein said product dispersion comprises cerium dioxide nanoparticles having a mean diameter in the range of about 1 nm to about 15 nm.
18. The process according to claim 1 , wherein n is 1 or 2.