Rapid method for production of cerium-containing oxide organic colloids

a cerium-containing oxide and organic colloids technology, applied in the field of colloidal nanoparticle dispersions, can solve the problems of high cost of conventional aqueous processes, inability to stabilize in a non-polar environment, and the agglomeration of particles, etc., and achieves the effect of simple, rapid and low temperature processes

Inactive Publication Date: 2013-08-01
CERION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Benefits of technology

[0011]The present invention has various embodiments that provide simple, rapid, low temperature processes for th...

Problems solved by technology

However, conventional aqueous processes—precipitation in particular—are costly as they involve multiple steps that are often time and energy consuming, as well as equipment intensive.
However, most particle stabilizers used to prevent particle agglomeration in an aqueous environment are ill-suited to the task of stabilization in a non-polar environment.
When placed in a non-polar solvent, such particles tend to immediately agglomerate and, consequently, lose some, if not all, of their desirable particulate properties.
Changing stabilizers can involve a difficult displacement reaction or separate, tedious isolation and re-dispersal methods such as, for example, precipitation and subsequent re-dispersal with a new stabilizer using, for instance, a ball millin...

Method used

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  • Rapid method for production of cerium-containing oxide organic colloids

Examples

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example 1

Extraction of Ce0.6Fe0.4O(2-δ) with Oleic Acid and DEGME

[0052]A 100 ml aliquot of Ce0.6Fe0.4O(2-δ) aqueous nanoparticle dispersion prepared as described above, was added to a 500 ml reaction vessel and heated to a temperature of about 60° C. A 74.0 ml aliquot of Kensol® 50H and 37.6 g of oleic acid were then added, these two materials being at room temperature at the time of addition. The mixture was stirred by manual shaking of the vessel for a period of 1 minute, forming an emulsion. The emulsion mixture was then held at 40° C. to age for 2 hours. Then, 30 ml of DEGME was added to the emulsion and it separated in about 4 hours to yield a stable dark brown non-turbid substantially non-polar colloid phase, above a nearly colorless aqueous phase. The non-polar colloid phase was separated out by pipette.

[0053]To 100 ml of the separated organic colloid phase were added 13.9 ml of DEGME and 7.2 ml of PGME. Long-term stability observations of samples of the above non-polar colloid were c...

example 2

Extraction of Ce0.6Fe0.4O(2-δ) with Oleic Acid and DEGME

[0054]A 100 ml aliquot of Ce0.6Fe0.4O(2-δ) aqueous nanoparticle dispersion prepared as described above, was added to a 500 ml reaction vessel and heated to a temperature of about 60° C. A 75.0 ml aliquot Kensol® 50H and 35.9 g of oleic acid were then added, these two materials being at room temperature at the time of addition. The mixture was stirred by manual shaking of the vessel for a period of 1 minute. The emulsion mixture was then held at 40° C. to age for 2 hours. Then, 30 ml of DEGME was added to the emulsion and it was returned to 40° C., thereafter it completely separated in about 4 hours to yield a stable dark brown non-turbid substantially non-polar colloid phase, above a nearly colorless aqueous phase. The non-polar colloid phase was separated out by pipette. To 100 ml of the separated organic colloid phase were added 12.2 ml of DEGME and 9.1 ml of PGME.

[0055]Long-term stability observations of samples of the above...

example 3

Extraction of Ce0.6Fe0.4O(2-δ) with Oleic Acid and DEGME

[0056]A 500 ml aliquot of Ce0.6Fe0.4O(2-δ) aqueous nanoparticle dispersion prepared as described above, was heated to a temperature of about 60° C. and transferred to a 2 L reaction vessel. The liquid was stirred with a 1 9 / 16″ R100 (Rushton) impeller that was lowered into the reactor vessel. The mixer head was positioned slightly above the bottom of the reactor vessel. The mixer was set to 1690 rpm. A mixture of 370 ml of Kensol® 50H and 188 g of oleic acid, at room temperature, was added to the vessel over a 30 second period. The whole mix was then stirred at 1750 rpm for 2 minutes resulting in the formation of an emulsion. The reaction vessel was then moved to hot plate with magnetic stirrer and stirred using a 2½″ magnetic bar at high speed setting. 50 ml of DEGME was then added over 15 seconds. The vessel was then held without stirring at a temperature of about 45° C. After about 4 hours, the emulsion separated completely ...

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Abstract

Improved methods for producing colloidal dispersions of cerium-containing oxide nanoparticles in substantially non-polar solvents is disclosed. The cerium-containing oxide nanoparticles of an aqueous colloid are transferred to a substantially non-polar liquid comprising one or more amphiphilic materials, one or more low-polarity solvents, and, optionally, one or more glycol ether promoter materials. The transfer is achieved by mixing the aqueous and substantially non-polar materials, forming an emulsion, followed by a phase separation into a remnant polar solution phase and a substantially non-polar organic colloid phase. The organic colloid phase is then collected. The promoter functions to speed the transfer of nanoparticles to the low-polarity phase. The promoter accelerates the phase separation, and also provides improved colloidal stability of the final substantially non-polar colloidal dispersion. The glycol ether promoter reduces the temperature necessary to achieve the phase separation, while providing high extraction yield of nanoparticles into the low-polarity organic phase. In addition, use of particular amphiphilic materials, such as heptanoic acid or octanoic acid, enable efficient extractions at ambient temperatures without the use of a glycol ether promoter.

Description

CROSS-REFERENCE TO RELATED APPLICATIONS[0001]This application is a continuation-in-part of U.S. patent application Ser. No. 13 / 753,992, IMPROVED METHOD FOR PRODUCTION OF STABLE CERIUM OXIDE ORGANIC COLLOIDS, filed Jan. 30, 2013, which claims priority to U.S. Provisional Application No. 61 / 632,778, filed Jan. 30, 2012, the disclosures of which are incorporated herein by reference in its entirety. This application also claims the benefit of priority to Provisional Application Ser. No. 61 / 632,881, METHOD FOR PRODUCTION OF STABLE CERIUM OXIDE ORGANIC COLLOIDS, filed Feb. 1, 2012, the disclosure of which is incorporated herein by reference in its entirety.FIELD OF THE INVENTION[0002]The present invention relates generally to colloidal nanoparticle dispersions and more specifically to improved processes for the manufacture of doped and un-doped cerium oxide colloidal dispersions in solvents having low-polarity.BACKGROUND OF THE INVENTION[0003]Cerium-containing oxide nanoparticles have man...

Claims

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Application Information

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IPC IPC(8): C10L10/00
CPCC10L10/00C10L2200/0245C10L1/1881C10L1/1826C10L1/1852C10L1/10C01G49/0054C01P2002/85C01P2004/04C01P2004/64C10L1/1233C10L10/02C10L2200/0254C10L2290/24C10L1/18C10M125/10C10M129/16C10M129/40
Inventor PROK, GARY ROBERTWILLIAMS, STEPHEN CHARLES
Owner CERION
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