Title of Invention

"A PROCESS FOR SEPARATION OF IRON AND LEAD FROM EFFLUENTS/WASTE WATER/LEACH LIQUORS"

Abstract The present invention produces an improved process for separation of iron and lead from solution (effluents/waste water/leach liquors) at different chloride concentration by two cationic exchange such as commercially available Duolite ES-467 and resin containing hydroxamic acid functional groups.
Full Text The present invention relates to a process for the separation of iron and lead from efluents/wastewater/leach liquors.
Lead is toxic element and causes various types of diseases like anaemia, ensephalopathy, hepatitis, renal disturbances, lung insufficiency, bone lesions, cancer and hypertension. Lead is a common pollutant especially for battery industry. The effluent from battery industry mainly contains lead and iron. The pH of the solution varies from 1.5 to 3. Based on legislation currently enforced in the European union, the maximum permissible Pb (II) concentration for discharge in public water is set at 0.2 mg/L. Due to rapid growth of automobile industry in India, there is an urgent need to develop a process to treat wastewater of battery industry.
Reference may be made to various process developed for the separation of iron and lead from effluents / wastewater / leach liquors. Pagano et al (M. Pagano, D.pertruzzelli, G. Tiravanti and R. Passino, Pb/Fe separation and recovery from automobile battery watewaters by selective ion exchange, Solvent Extr. Ion Exch. 18(2), 387-399 (2000).) studied Pb/Fe separation and recovery from automobile battery wastewaters by selective ion exchange method using two types of commercially available resins; weak anionic resin Duolite A7 as selective sorbent for ferric species and weak cation resin Purolite C106 for removal and recovery of lead species. Petuzzelli et al (D.Petruzzelli, M.Pagano, G.Tiravanti and R. Passino,Lead removal and recovery from battery wastewaters by natural zeolite

clinoptilolite. Solvent Extr.lon Exch.17 (3) 677-694(1999)) studied lead removal and recovery from battery waste waters by natural zeolite, clinoptilolite. They have demonstrated the technical feasibility of the process for removal and recovery of lead present in battery manufacturing wastewaters in absence of aluminium and ferric species. Both the above processes used a very low concentration of Pb/and Fe(
from solutions. The process can be applied where the concentration of the metal ions were high. For low concentration the solvent extraction process is not very fruitful, as the effluent would be contaminated with chelating agent due to inherent solubility. The contamination of chelating agent would increase the bacterial oxygen demand thereby it requires further treatment before disposal.
Use of ion exchange resin containing active functional groups provides a better alternative to treat solutions where the concentrations of metal ions are low. The usual technique for separation of Fe and Pb is the formation of cationic and anionic species, by the addition of chloride and sulphate ions. Once Fe and Pb forms anions species, then by the use of cationic and anionic exchanger would eventually separate both the metal ions.
The process depends on
1. Concentration of anions
2. Efficiency of the exchanger
The main objective of the present invention is to provide a process for the separation of Fe and Pb using two different chelating cation exchangers in presence of chloride ions.
Another object of present invention is to test the newly synthesized chelating ion exchange resin containing hydroxamic acid functional group

regarding its suitability in extracting the anionic Pb complex.
Accordingly the present invention provides A process for separation of Fe and Pb from effluents/waste water/leach liquors which comprises
a) treating the solution of industry effluents /waste water / leach liquors containing iron and lead, in presence of chlorides ions concentration ranging between 50-200 g/L, at pH 2-3 with chelating ion exchange resin, macro porous styrene divinyl benzene (Duolite ES-467), under agitation for a period 5-30 minutes to obtain a rafinate after getting extraction of more than 90% of iron.
b) treating the rafinate obtained from step (a) with hydroxamic acid functional group embedded methyl methacrylate(MMA)-divinyl benzene(DVB) polymer, as chelating ion-exchange resin, to extract more than 95% of lead.
The present invention provides a process for separation of Fe and Pb from solution at different chloride ions concentration. The major steps in the process are:
a. preparation of Fe and Pb solution
b. Concentration variation of chloride ions.
c. Separation of Fe and Pb by two cation exchange such as commercially
available Duolite ES-467 and resin containing hydroxamic acid functional
groups. The hydroxamic acid resin was embedded in methymethacrylate

(MMA) - Divinyl benzene (DVB) polymer. This resin can withstand high
alkali concentration.
In an embodiment of the present invention the chloride ion concentration varied from 50-200 g/L.
In another embodiment of the present invention the pH of the solution ranges between 2-3.
The process of this invention is illustrated by examples, which should not be construed to limit the scope of this invention.
Example 1 The solution contained 100 mg/L each of Fe and Pb prepared using their respective chloride salts. Total chloride ion concentration was maintained at 100 g/L adding requisite amount of NaCI. 200 mL of above solution was mixed with 20 g of the Duolite ES-467 resin in a 500 beaker. The solution was agitated by a Remi stirrer at a agitation speed of 500rpm for a period of 15 minutes. It was observed that the extraction efficiently of Fe was more than 90% and the co-extraction of Pb was less than 10%. The raffinate was separated and mixed with 30 g of hydroxamic acid functional group chelating ion-exchange resin in a 500ml beaker. The solution was agitated by a Remi stirrer at a agitation speed of 500rpm for a period of 15 minutes. The Pb

extraction efficiently by this resin was more than 95% . The effluent contained only 4.5% of lead and below detectable level of iron.
Example 2 The solution contained 100 mg/L each of Fe and Pb prepared using their respective chloride salts. Total chloride ion concentration was maintained at 150 g/L by adding requisite amount of NaCI. 200 mL of above solution was mixed with 20 g of the ES-467 resin in a 500ml beaker. The solution was agitated by a Remi stirrer at a agitation speed of 500 rpm for a period of 15 minutes. It was observed that Duolite ES-467 could extract more than 95% of Fe and the co-extraction of Pb was less than 7%. The raffinate was separated
and mixed with 30 g of hydroxamic acid functional group chelating ion-exchange resin in a 500ml beaker. The solution was agitated by a Remi stirrer at a agitation speed of 500rpm for a period of 15 minutes. The Pb extraction efficiency by this resin was more than 90%. The effluent contained only 9.3 % of lead and below detectable level of iron.
The main advantages of the process of the present invention are:
1) Fe and Pb can be effectively separated from the solution.
2) The Fe and Pb sorption kinetics are fast.
3) The process can be carried out at ambient temperature and pressure.
4) Using two different cationic exchangers carried out Fe and Pb separations.




We claim:
1. A process for separation of Fe and Pb from effluents/waste water/leach
liquors which comprises
a) treating the solution of industry effluents /waste water / leach liquors containing iron and lead, in presence of chlorides ions concentration ranging between 50-200 g/L, at pH 2-3 with chelating ion exchange resin, macro porous styrene divinyl benzene (Duolite ES-467), under agitation for a period 5-30 minutes to obtain a rafinate after getting extraction of more than 90% of iron.
b) treating the rafinate obtained from step (a) with hydroxamic acid functional group embedded methyl methacrylate(MMA)-divinyl benzene(DVB) polymer, as chelating ion-exchange resin, to extract more than 95% of lead.
2. A process for separation of Fe and Pb from effluents/waste water/leach
liquors substantially as herein described with the reference to the examples
accompanying this specification.

Documents:

249-DEL-2003-Abstract-(17-09-2008).pdf

249-del-2003-abstract.pdf

249-DEL-2003-Claims-(17-09-2008).pdf

249-del-2003-claims.pdf

249-del-2003-complete specification(granted).pdf

249-DEL-2003-Correspondence-Others-(17-09-2008).pdf

249-del-2003-correspondence-others.pdf

249-del-2003-correspondence-po.pdf

249-DEL-2003-Description (Complete)-(17-09-2008).pdf

249-del-2003-description (complete).pdf

249-DEL-2003-Form-1-(17-09-2008).pdf

249-del-2003-form-1.pdf

249-del-2003-form-18.pdf

249-DEL-2003-Form-2-(17-09-2008).pdf

249-del-2003-form-2.pdf

249-DEL-2003-Form-3-(17-09-2008).pdf

249-del-2003-form-3.pdf


Patent Number 228661
Indian Patent Application Number 249/DEL/2003
PG Journal Number 08/2009
Publication Date 20-Feb-2009
Grant Date 05-Feb-2009
Date of Filing 07-Mar-2003
Name of Patentee COUNCIL OF SCIENTIFIC AND INDUSTRIAL RESEARCH
Applicant Address RAFI MARG, NEW DELHI-110 001,INDIA
Inventors:
# Inventor's Name Inventor's Address
1 PRITISH KUMAR DASH REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013,ORISSA,INDIA
2 DAYANANDA SARANGI REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013,ORISSA,INDIA
3 GAUTAM ROY CHAUDHURY REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013,ORISSA,INDIA
4 KARANAM SRINIVASA RAO REGIONAL RESEARCH LABORATORY, BHUBANESWAR-751013,ORISSA,INDIA
PCT International Classification Number C22B 13/06
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA