Liquid purification or separation – Processes – Ion exchange or selective sorption
Reexamination Certificate
2002-10-15
2004-12-07
Hopkins, Robert A. (Department: 1724)
Liquid purification or separation
Processes
Ion exchange or selective sorption
C210S688000, C502S085000
Reexamination Certificate
active
06827859
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to a method for removing heavy metals or radionuclides from an aqueous solution using an ion exchange material. In one aspect, the invention relates to use of solid ion exchange materials, liquid ion exchange materials, and mixtures thereof useful in said method. The present invention further relates to solid and liquid ion-exchange materials useful for removing heavy metals or radionuclides from an aqueous solution and a process for producing the ion exchange materials thereof.
BACKGROUND OF THE INVENTION
A significant amount of industrial waste water is contaminated with heavy metals such as lead, zinc, copper, antimony, chromium and nickel and radioisotope ions such as radioisotopes of uranium, cobalt, thorium, strontium and cesium. These metals become contaminants in aqueous systems as the result of activities including chemical manufacture, smelting, electroplating, wood treating, industrial and medical use of radioisotopes, etc. When such metals are used, metal discharges in aqueous streams severely damage the environment by posing risk to wild life and human health, and have become a worldwide environmental concern. The successful treatment of low level radioactive effluent also presents a major challenge to the nuclear industry. Therefore, improved methods for removing heavy metals or radioactive isotope ions rapidly and efficiently from contaminated industrial aqueous solutions are highly desired.
Existing metal removal methods include standard, conventional techniques such as evaporation, precipitation, electrolytic techniques, membrane separation, fixed and movable bed ion exchange, and activated carbon purification. However, these methods are not economical or efficient enough in most cases. Zeolites and organically modified smectite clays have also been used in these applications, but there remains a continual need to develop improved materials that are more effective for removal of heavy metals and radioisotopes.
Previous studies have identified natural zeolites, e.g. naturally occurring clinoptilolite, for use in removing heavy metals and radioisotope ions from aqueous solutions. While natural zeolites have been used, they are not sufficiently cost-effective and efficient in removing heavy metals and radioisotope ions.
It has been suggested to use modified zeolites to improve the metal removal efficiency of the natural Zeolites. U.S. Pat. No. 5, 268,107 (the '107 patent) describes a modified clinoptilolite as an ion exchange material for the removal of radioisotope cations such as the cations of cesium (
137
Cs) and strontium (
90
Sr) from an aqueous environment containing radioisotope cations. The modified clinoptilolite of the '107 patent is produced by treating a natural clinoptilolite with sodium hydroxide at a concentration of 0.1 to 5 M or with hydrochloric acid at a concentration of from 0.1 to 5 M for a treatment time longer than one hour at a temperature of 30° C. to 80° C. The modified clinoptilolite is preferably calcined at a suitable calcining temperature of from 400° C. to 500° C. for a calcining time of at least 3 hours. While the modified clinoptilolite of the '107 patent is improved over unmodified clinoptilolite, it is still desired to have further improvement in the heavy metal or radioisotope ion removal efficiency to have a more commercially attractive product. Applicants have now discovered an improved modified clinoptilolite based ion exchange materials with improved heavy metal and radioisotope ion removal efficiency.
SUMMARY OF THE INVENTION
According to the invention, a process for preparing an ion exchange material useful for removing heavy metals or radionuclides from an aqueous solution is provided comprising contacting clinoptilolite with an alkaline solution at a temperature of about 85° C. to about 300° C. and for a sufficient time to form a treated slurry comprising an ion exchange material having a solid fraction and a liquid fraction. The solid ion exchange material is further processed by separating the solid fraction from the treated slurry and washing the solid fraction. The liquid ion exchange material is further processed by recovering the liquid fraction from the treated slurry. A mixture of the solid ion exchange material and the liquid ion exchange material that can be used to remove heavy metals or radionuclides from an aqueous solution can be the treated slurry directly produced, or alternatively, can be prepared by mixing the solid ion exchange material with the liquid ion exchange material.
Further according to the invention, novel solid and liquid ion exchange materials prepared by the process of the invention are provided.
Still further according to the invention, a method for removal of heavy metals or radionuclides from a contaminated aqueous solution is provided comprising contacting the contaminated aqueous solution with an ion exchange material selected from a solid ion exchange material, a liquid ion exchange material, or mixtures thereof, wherein the ion exchange material is prepared according to the process of the invention.
BRIEF DESCRIPTION OF THE DRAWINGS
Not Applicable
REFERENCES:
patent: 4247524 (1981-01-01), Leonard
patent: 5268107 (1993-12-01), Hutchings et al.
patent: 5690833 (1997-11-01), Crawford et al.
patent: 5919287 (1999-07-01), Moreau
patent: 6218329 (2001-04-01), Singh et al.
patent: 6261986 (2001-07-01), Bowman et al.
patent: 6413492 (2002-07-01), Kuznicki et al.
Green Fred H.
Lockwood James M.
Hopkins Robert A.
Lathrop & Gage L.C.
Synlite Chemical Company LLC
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