Title of Invention

A PROCESS FOR PREPARATION OF ION IMPRINTED POLYMER PARTICLES FOR PRECONCENTRATIVE SEPARATION OF PALLADIUM (II) IONS VIA SOLID PHASE EXTRACTION

Abstract Palladium(II) ion imprinted polymer (IIP) particles are synthesized containing palladium(II) ion memory recognition sites. Palladium(II) IIP materials are prepared by bulk polymerization of palladium-amino, hydroxyl or mercaptoquinoline-4-vinyl pyridine ternary complex dissolved in 2-methoxy ethanol (porogen) with 2-hydroxy ethyl methacrylate (HEMA) and ethylene glycol dimethacrylate (EGDMA) as functional and crosslinking monomers in the presence of 2,2"-azobisisobutyronitrile (AIBN) as thermal initiator. The above material was ground and sieved to obtain polymer particles which are subjected to treatment with mineral acid to obtain leached palladium(II) IIP particles. The resultant particles finds application for the preconcentrative separation of palladium(II) ions from dilute aqueous solutions containing platinum(IV), copper(II), nickel(II) and zinc(II) which are likely to coexist with palladium in its minerals/ores.
Full Text This invention relates to the process for the preparation of ion imprinted polymer particles for pre concentrative separation of palladium(II) ions via solid phase extraction . Palladium ion imprinted polymer particles were prepared by bulk polymerization of palladium-amino, hydroxy or mercaptoquinoline-4-vinyl pyridine ternary complex with 2-hydroxyethyl methacrylate (HEMA) and ethylene glycol dimethacrylate (EGDMA) as functional and crosslinking monomers in the presence of 2,2'-azobisisobutyronitrile (AIBN) as initiator. The synthesis was carried out using 2-methoxyethanol as porogen. The polymer particles thus synthesized enables the preconcentrative separation of palladium from platinum and other transition metals (which coexist with palladium in its minerals/ores) either individually or in mixtures.
BACKGROUND OF THE INVENTION
Ion imprinted polymers
Reference may be made to John et al, W099 15, 707; 1999 relating to the detection and extraction of uranyl ions by polymer imprinting wherein the complexable functionality is of the formula CTCOOH, when T is a hydrogen or any halogen (preferably chlorine), methyl and halogen substituted forms thereof or CCOOH or PhCOOH. Another reference may be made to Gladis and Rao, Indian Patent, 2003 IPA 516 DEL 03 dt. 28.3.03, who have synthesized ion imprinted polymers for solid phase extractive preconcentration/separation of uranyl ions from host of tetravalent, tervalent and bivalent inorganic ions from both aqueous and synthetic seawater solutions. This patent relates to the synthesis of uranyl ion imprinted polymer particles by thermal polymerization of uranium-Quinoline-8-ol or its dihalo derivatives-4-vinyl pyridine ternary complex with monomers such as styrene and divinyl benzene in presence of AIBN as initiator. Yet another reference may be made to Dai et al US patent 6, 251, 280; 2001 who prepared mesoporous sorbent materials by ion imprinting technique for the separation of
reference may be made to Dai et al US patent 6, 251, 280; 2001 who prepared mesoporous sorbent materials by ion imprinting technique for the separation of inorganics using bifunctional ligands such as amines, thiols, carboxylic acids, sulphonic acids and phosphonic acids.
Still another reference may be made to Singh et al, US Patent 6, 248, 842; 2001 who produced selective crosslinked chelating polymers by substituting an acyl chelating agent with a polymerizable functional group. The resulting substituted acyl chelating agent was complexed with the target metal ion, i.e. copper and crosslinked with a suitable monomer. The complexed metal is then removed providing a crosslinked polymeric chelating agent that has been templated for copper ion. However, there are no patents related to the preparation of ion imprinted polymer particles for preconcentrative separation of palladium(II) from platinum(IV) and other transition metals. Catalysts
The potential for induced chirality at transtiion metal catalysts within molecular imprinted polymer binding sites has been elegantly explored by Gagne et al [Organometallics, 17 (1998) 3138-3140; J. Am. Chem. Soc. 122 (2000) 6217-6225] in some very detailed and vigorous investigations employng metals as diverse as rhodium, titanium and platinum. Lemaire et al [Tetrahedron Lett. 135 (1995) 8779-8782; J. Mol. Cat. A. Chem. 135 (1998) 89-98] have demonstrated the increase of enantioselectivity of hydride transfer reaction by using molecular imprinted polymer based rhodium complexes as catalysts. To overcome the site heterogenity problem, Gagne and coworkers [Organometallics, 21 (2002) 7-9] adopted a poisoning stragegy using diamine derivatives of binaphthol to block the most easily accessible sites in a MIP containing chiral phosphine platinum complexes. Further, the immobilized catalysts produced via molecular imprinting methodology can be made more selective through chemical modification with suitable "poisons", a result which may trigger post-imprinting derivatisation of imprinted polymer binding sites [Krisch et al. Polymer, 41 (2000) 5583-5590];
Polboron and Severin [J. Chem. Soc. Chem. Commun. (1999) 2481-2482; Chem. Eur. J. 6 (2000) 4604-4611] have synthesized immobilized ruthenium catalysts based on molecular imprinting for the reduction of benzophenone.
Cammidge et al [Chem. Commun. 2001, 2588-2589] have synthesized heterogenous palladium catalyst assemblies by molecular imprinting using methacrylic acid, EGDMA or styrene-divinyl benzene monomers in presence of bis PdCl2-(4-ethenyl phenyl) diphenyl phosphine)-l,2-dihydroxy benzene complex. These authors have demonstrated the clear superiority of catalysts prepared by molecular imprinting over traditional polymeric ligands. Solid phase extraction
Rao et al [Trends in Anal. Chem. 2004] have reviewed the preparation of tailored materials for preconcentration/separation of metals by ion imprinted polymers for solid phase extraction [IIP-SPE). IIP materials with nanopores were prepared by formation of ternary complex of palladium imprint ion with dimethyl glyoxime and 4-vinyl pyridine and thermally polymerizing with styrene and divinyl benzene in presence of 2,2'-azobis isobutyronitrile using cyclohexanol as porogen [Sobhi et al. Anal. Chim. Acta, 488 (2003) 173-182]. 2-Hydroxy ethyl methacrylate (HEMA) polymers
Joshi et al [Chem. Engg. Sci. 53 (1998) 2271-2284] have prepared MIP's for the removal of traces of phenol from anisole using different functional monomers including 2-hydroxy ethyl methacrylate. From equilibrium sorption studies on various MIP's, it was observed that HEMA based MIP showed slightly higher sorption capacity than methacrylic acid based system. In continuation of the above work on removal of trace impurities from bulk chemicals, same authors [Chem. Engg. Sic. 55 (2000) 1509-1522] report on the separation of phenol, bisphenol-A and 2,4-dihydroxybenzophenone isomers (2,4-DHB) using HEMA by employing surface as well as bulk imprinted polymerization approaches. Sreenivasan has utilized y-irradiation to synthesize molecular imprinted poly-HEMA containing memory sites while developing sensor components for
testosterone [Polymer Gels and Networks, 5 (1997) 17-22] and salicylic acid [Talanta, 44 (1997) 1137-40]. Inspite of several advantages of imprinted polymers based on HEMA, as functional monomer there are no reports so far for the preconcentrative separation of noble metals including palladium. Patent documents
W099 15,707 Johnetal
Detection and extraction of an ion in a solution, particularly uranium ion
IPA 516 Del 03 dated 28.3.03 Gladisetal
Synthesis of solid phase extractant materials by polymer imprinting suitable for uptake of uranyl ions and a process thereof.
US 6,251,280 Daietal
Imprint coating synthesis of selective functionalized ordered mesoporous sorbents for separation and sensors.
US 6,248,842 Singh etal
Synthetic polymer materials including preorganized chelation sites for the
selective and reversible binding of metals.
Other References
B.P. Santora, A.O. Larsen, M.R. Gagne, Organometallics, 17 (1998) 3138-3140.
Toward the molecular imprinting of titanium Lewis acids - demonstration of
Diels-Alder Catalysis.
N.M. Brunkan, M.R. Gagne, J. Am.Chem. Soc. 122 (2000) 6217-6225.
Effect of chiral cavities associated with molecularly imprinted platinum centers on
the selectivity of ligand-exchange reactions at platinum.
P. Gamez, B. Dunjic, C. Pinel, M. Lemaire, Tetrahedron Lett. 36 (1995) 8779-
8782.
Molecular imprinting effect in the synthesis of immobilized rhodium complex
catalyst (IRC cat.).
F. Locatelli, P. Gamez, M. Lemaire, J. Mol. Catal. A. Chem. 135 (1998) 89-98.
Molecular imprinting of polymerized catalytic complexes in asymmetric catalysis.
J.H. Koh, A.O. Larsen, P.S. White, M.R. Gagne, Organometallics, 21 (2002) 7-9.
The disparate roles of chiral ligands and molecular imprinted cavities in
assaymetric catalysis and chiral poisoning.
N. Kirsch, C. Alexander, M. Lubke, M.J. Whitcombe, E.N. Vulfson, Polymer, 41
(2000) 5583-5590.
Enhancement of selectivity of imprinted polymers via post-imprinting
modification of recognition sites.
K. Polbom, K. Severin, J. Chem. Soc. Chem. Commun. (1999) 2481-2482.
Molecular imprinting with an organometallic transition state Analogue.
K. Polbom, K. Severin, Chem. Eur. J., 6 (2000) 4604-4611.
Biomimetic catalysis with immobilized organometallic ruthenium complexes -
substrate - regioselective transfer hydrogenation of ketones.
A.N. Cammidge, N.J. Baines, R.K. Bellingham, Chem. Commun. (2001) 2588-
2589.
Synthesis of heterogenous palladium catalyst assemblies by molecular imprinting.
T. Prasada Rao, Sobhi Daniel, J. Mary Gladis, Trends in Anal. Chem. 23(2004)28-
35.
Tailored materials for preconcentration or separation of metals by ion imprinted
polymers for solid phase extraction (IIP-SPE).
Sobhi Daniel, J. Mary Gladis, T. Prasada Rao, Anal. Chim. Acta, 488 (2003) 173-
182.
Synthesis of imprinted polymer material with palladium ion nanopores and its
analytical application.
V.P. Joshi, S.K. Karode, M.G. Kulakami, R.A. Mashelkar, Chem. Engg. Sci. 53
(1998)2271-2284.
Novel separation strategies based on molecularly imprinted adsorbents.
V.P. Joshi, M.G. Kulkami, R.A. Mashelkar, Chem. Engg. Sci. 55 (2000) 1509-
1522.
Enhancing adsorptive separations by molecular imprinted polymers: Role of
imprinting techniques and system parameters.
K. Sreenivasan, Polymer Gels and Networks, 5 (1997) 17-22.
A note on the selectivity of y-irradiation polymerised molecularly imprinted
poly(HEMA).
K. Sreenivasan, Talanta, 44 (1997) 1137-1140.
On the feasibility of using molecularly imprinted poly (HEMA) as a sensor
component.
The main objectives of the present investigation are:
• To prepare palladium(II) IIP materials using palladium(II)-8-aminoquinoline-4-vinyl pyridine ternary complex
• to prepare palladium(II) materials using palladium(II)-8-hydroxyquinoline-4-vinyl pyridine ternary complex
• To prepare palladium(II) IIP materials using palladium(II)-8-mercaptoquinoline-4-vinyl pyridine ternary complex
Yet another object of the present investigation is
• to preconcentratively separate palladium(II) from platinum(IV) and transition
metal ions through solid phase extraction
Accordingly, the present invention provides a process for preparation of ion
imprinted polymer particles for pre concentrative separation of palladium(ii) ions
via solid phase extraction comprising:
a) Preparing binary complex of palladium(II) ion with organic chelate selected
from the group comprising of 8-aminoquinoline, 8-hydroxyquinoline or 8-
mercaptoquinoline and the molar proportion of imprint ion with binary complex
Pd-8-aminoquinoline /8-hydroxy quinoline /8-mercapto quinoline complex
precipitate being in the ratio of about 1:2 .
b) Dissolving above isolated binary complexes in a suitable porogen selected
from 2-methoxy ethanol to form a prepolymerizing mixture/prepolymer solution ;
c) Combining the mixtures from (b) with functional monomers (4- vinyl pyridine,
2-hydroxylethylmethacrylate) and crosslinking monomer
(ethyleneglycoldimethacrylate) in a ratio of about 1:2:8:32 in presence of initiator 2,2' -azobisisobutyronitrile and polymerization being carried by heating the mixture in oil bath at about 80°C for about 15 minutes with constant stirring to obtain the ion imprinted polymers.
d) Grinding of polymer materials obtained in (c) using a mortar and pestle followed by sieving with 45-µm test sieve to collect palladium(II) ion imprinted polymer particles of the size ranging 45-212)xm.
e) Selective leaching of imprint ion (i.e. palladium) from polymer particles obtained in (d) using about 50%v/v hydrochloric acid for about 18 hours followed by drying in an oven about 60° C.
In an embodiment of the present invention the binary complex of palladium(II)
with 8-aminoquinoline is isolated.
In another embodiment of the present invention the binary complex of
palladium(II) with 8-hydroxyquinoline is isolated.
In yet another embodiment of the present invention the binary complex of
palladium(II) with 8-mercaptoquinoline is isolated.
In still another embodiment of the present invention the functional monomers are
4-vinyl pyridine and 2-hydroxy ethyl methacrylate.
In still another embodiment of the present invention the crosslinking monomer is
ethylene glycol dimethacrylate.
In still another embodiment of the present invention the 2,2'-azobisisobutyronitrile
is used as initiator.
In still another embodiment of the present invention the palladium(II) ion
imprinted polymer materials were ground and sieved after drying to obtain
particles.
In still another embodiment of the present invention palladium(II) ion embedded
in the polymer is leached out using mineral acid to obtain palladium(II) ion
imprinted polymer particles.
In still another embodiment of the present invention , polymer particles obtained is
used for enrichment of palladium(II) ion from dilute aqueous solutions containing
copper , zinc and nickel.
In still another embodiment of the present invention , ion imprinted polymer
particle obtained is used for enhanced selectivity coefficients for palladium(II)
over platinum(IV) compared to control or blank polymer particles
Detailed description of the invention
The present invention offers methods for synthesizing palladium(II) selective ion imprinted polymer particles having accessible and homogenous imprinted sites for solid phase extraction from dilute aqueous solutions.
As used herein, the term "ion imprinting polymer (IIP) refers to a material that has been polymerized around an imprint ion in such a way that when imprint ion is removed from the material, cavities or "Imprinted sites" remain in the material that are complementary in shape and size of the imprint ion. On the addition of IIP particles to dilute solution containing imprint ion, the imprint sites selectively binds imprint ion. Such binding allows the use of tailored IIP particles for enrichment/separation of imprint ions from other such ions which are similar to it. The salient features of the invention include the following, i) making the polymer materials
ii) pretreatment of the polymer materials to leach the imprint ion iii) Preconcentrative separation of Palladium(II) from platinum(IV) and other transition metal ions
There are three main steps in the synthesis of tailored palladium(II) IIP particles: (I) formation of binary complex of imprint ion (palladium) with AQ or Q or MQ, (ii) formation of ternary complex in presence of 4-vinyl pyridine and (iii) polymerization of ternary mixed ligand complex with HEMA and EGDMA. The
formation of ternary complex was carried out by mixing binary Pd(II)-AQ or Pd(II)-Q or Pd(II)-MQ precipitates with 4-vinyl pyridine in 2-methoxyethanol (Porogen). Evidence for formation of binary and ternary complexes with palladium were monitored by recording UV-visible absorption spectra. Figs.l,2&3 show the absorption spectra of AQ or Q or MQ, VP, Pd(II)-AQ orPd(II)-Q or MQ, Pd(II)-VP and Pd(II)-AQ-VP or Pd(II)-Q-VP or Pd(II)-MQ-VP. These spectra clearly shows the formation of binary and ternary complexes (See Fig.4) in 2-methoxyethanol solution.
The ternary complexes viz. Pd(II)-AQ-VP or Pd(II)-Q-VP or Pd(II)-MQ-VP were imprinted on addition of HEMA (functional monomer) and EGDMA (crosslinking monomer) in presence of AIBN. The resulting IIP materials were dried in an oven at 60° to obtain palladium IIP materials. Fig.5 shows the schematic representation of polymer imprinting process. These materials were ground and sieved to obtain palladium(II) IIP particles. i) Pretreatment of the IIP particles to leach the imprint ion
The imprint ion, i.e. palladium(II) ion was removed from the IIP particles by stirring with 100 ml of 50% (v/v) HCl for 18 h. The resulting IIP particles were dried in an oven at 60°C to obtain palladium(II) IIP-SPE particles which can be used for selective enrichment of palladium ions from dilute aqueous solutions. Fig.6 shows the percent enrichment of palladium(II) ions by using AQ, Q or MQ based HP's. The retention capacities of AQ, Q or MQ based HP's are shown in Fig.7. ii) Preconcentrative separation of palladium(II) from platinum(IV) and other
transition metal ions
The preconcentrative separation of palladium(II) from platinum(IV), copper(II), zinc(II) and nickel(II) when present individually and in admixtures was studied by using AQ, Q and MQ based palladium(II) IIP particles. The results show quantitative separation from copper(II), palladium(II), nickel(II) and zinc(II) (which are likely to coexist with palladium in its mineral or ore deposits). Further,
selectivity coefficients (Spd(II)/pt(iv)) were found to be 550, 4.25 and 8.19 for AQ, Q
and MQ based palladium IIP particles.
In the drawings accompanying this speciflcation,
Fig.l represents the UV-visible absorption spectra of 8-aminoquinoline (AQ), 4-
vinylpyridine (VP), Pd(II)-AQ, Pd(II)-VP and Pd(II)-AQ-VP.
Fig.2 represents the UV-visible absorption spectra of 8-hydroxyquinoline (Q), 4-
vinylpyridine (VP), Pd(II)-Q, Pd(II)-VP and Pd(II)-Q-VP.
Fig.3 represents the UV-visible absorption spectra of 8-mercaptoquinoline (MQ),
4-vinylpyridine (VP), Pd(II)-MQ, Pd(II)-VP and Pd(II)-MQ-VP.
Fig.4 Schematic representation of formation of ternary mixed ligand complexes
via. Pd(II)-AQ-VP, Pd(II)-Q-VP and Pd(II)-MQ-VP.
Fig.5. Schematic representation of polymer imprinting process.
Fig.6 represents the percent enrichment of Pd(II) by using AQ,Q or MQ based
HP's.
Fig.7 represents the retention capacities of Pd(II) by using AQ, Q or MQ based
HP's.
Example 1
Synthesis of palladium(II) selective extraction agent prepared by polymer
imprinting with 8-aminoquinoline and 4-vinylpyridine.
The polymer preparation was carried out in 2 steps: (i) the binary complex of palladium with 8-aminoquinoline was prepared by precipitating palladium(II) ions with 8-aminoquinoline from pH 2.5 solutions after the addition of monochloroacetic acid buffer. The resulting precipitate was filtered, washed with water and dried in an oven at 60'C, (ii) for polymerization, 0.01, 0.10 and 0.30 g of Pd(II)-AQ precipitate was dissolved in 10 ml of 2-methoxyethanol and mixed with 40 ^il vinyl pyridine (VP), 0.02, 0.20 and 0.6 ml of 2-hydroxy ethyl methacrylate (HEMA) and 0.13, 1.30, 3.90 ml of ethylene glycoldimethacrylate (EGDMA) and 50 mg of 2,2'-azobisisobutyronitrile (AIBN). The above polymerization mixture was cooled to 0°C; purged with N2 for 15 min, sealed and
heated in an oil bath at around ~80°C with constant stirring for 15 min. The solid formed was washed with water and dried in an oven at 60°C. This resulted in 0.511, 2.58 and 6.05 g of polymer materials respectively. The palladium(II) embedded in the polymer was leached with 100 ml of 50% (v/v) HCl for 18 h. This resulted in 0.447, 1.81 and 4.55 g of ion imprinted polymer particles after drying in an oven at 60°C. Example 2
Synthesis of palladium(II) selective extraction agent prepared by polymer imprinting with 8-liydroxyquinoline(Q)
The polymer preparation was carried out in 2 steps: (I) The binary complex of Pd(II)-Q was prepared by precipitating palladium ions with 8-hydroxyquinoline from pH 2.5 solutions after the addition of monochloroacetic acid buffer. The resulting precipitate was filtered, washed with water and dried in an oven at 60°C, (ii) For polymerization, 0.10 g of Pd(II)-Q precipitate was dissolved in 10 ml of 2-methoxyethanol and mixed with 40 µl of VP, 0.20 ml of HEMA and 1.30 ml of EGDMA and 50 mg of AIBN. The above polymerization mixture was cooled to 0°C, purged with N2 for 15 min, sealed and heated in an oil bath at around ~80°C with constant stirring for 15 min. The solid formed was washed with water and dried in an oven at 600C. This resulted in 1.78 g of polymer material. The palladium(II) embedded in the polymer was leached with 100 ml of 50% (v/v) HCl for 18 h. This resulted in 0.85 g of palladium ion imprinted polymer particles after drying in an oven at 60°C. Example 3
Synthesis of palladium selective extraction agent by polymer imprinting with 8-mercaptoquinoline (MQ)
The polymer preparation was carried out in 2 steps: (I) The binary complex of Pd(II)-MQ was prepared by precipitating palladium ions with 8-mercaptoquinoline from pH 2.5 solutions after the addition of monochloroacetic acid buffer. The resulting precipitate was filtered, washed with water and dried in an oven at 60°C,
(ii) For polymerization, 0.10 g of Pd(II)-MQ precipitate was dissolved in 10 ml of 2-methoxyethanol and mixed with 40 µl of VP, 0.20 ml of HEMA and 1.30 ml of EGDMA and 50 mg of AIBN. The above polymerization mixture was cooled to 0°C, purged with N2 for 15 min, sealed and heated in an oil bath at around ~80°C with constant stirring for 15 min. The solid formed was washed with water and dried in an oven at 60°C. This resulted in 1.90 g of polymer material. The palladium(II) embedded in the polymer was leached with 100 ml of 50% (v/v) HCl for 18 h. This resulted in 1.76 g of palladium ion imprinted polymer particles after drying in an oven at 60°C.
Thus, palladium(II) ion imprinted polymer particles were synthesized containing palladium(II) ion memory recognition sites. The above synthesis was carried out in 2 steps (i) isolating the binary complexes of palladium with amino, hydroxy or mercaptoquinoline and (ii) polymerization of resultant binary complexes with 4-vinyl pyridine and 2-hydroxy ethyl methacrylate (HEMA) and ethylene glycol dimethacrylate (EGDMA) as functional and crosslinking monomers respectively in the presence of 2,2'-azobisisobutyronitrile as initiator. The leaching of above polymer materials was carried out by stirring with 50% (v/v) HCl for 18 h. The resultant palladium(II) IIP particles offer quantitative separation of palladium(II) from copper(II), nickel(II) and zinc(II) and improved selectivity coefficients for palladium(II) over platinum(IV). Advantages :
The palladium(II) IIP particles prepared in the present invention utilizes simple and readily available chelating ligands like 8-amino, 8-hydroxy or 8-mercapto quinolines. These IIP particles after leaching has the unique capability of picking palladium (II) from very dilute solutions thereby palladium (II) can be recovered from low grade minerals, ores etc. Furthermore, these palladium (II) IIP particles has the additional capability of separating palladium (II) from platinum (IV) and transition elements which are likely to coexist with palladium in nature thus enabling preconcentrative separation.






We claim:
1. A process for preparation of ion imprinted polymer particles for pre
concentrative separation of palladium(II) ions via solid phase extraction
comprising:
a. Preparing binary complex of palladium(II) ion with organic chelate
selected from the group comprising of 8-aminoquinoline, 8-
hydroxyquinoline or 8-mercaptoquinoline and the molar proportion of
imprint ion with binary complex Pd-8-aminoquinoline /8-hydroxy
quinoline /8-mercapto quinoline complex precipitate being in the ratio
of about 1:2 .
b. dissolving above isolated binary complexes in a suitable porogen
selected from 2-methoxy ethanol to form a prepolymerizing
mixture/prepolymer solution.
c. combining the mixtures from (b) with functional monomers (4-
vinylpyridine, 2-hydroxyethylmethacrylate) and crosslinking monomer
(ethyleneglycoldimethacrylain a ratio of about 1:2:8:32 in presence of
initiator 2,2' -azobisisobutyronitrile and polymerization being carried
by heating the mixture in oil bath at about 80°C for about 15
minutes with constant stirring to obtain the ion imprinted polymers.
d. grinding of polymer materials obtained in (c) using a mortar and
pestle followed by sieving with 45-µm test sieve to collect
palladium(II) ion imprinted polymer particles of the size ranging 45-
212µm.
e. selective leaching of imprint ion (i.e. palladium) from polymer particles
obtained in (d) using about 50%v/v hydrochloric acid for about 18
hours followed by drying in an oven about 60°C.
2. A process as claimed in claim 1, wherein the binary complex of
palladium(II) with 8-aminoquinoline is isolated.
3. A process as claimed in claim 1, wherein the binary complex of palladium(II) with 8-hydroxyquinoline is isolated.
4. A process as claimed in claim 1, wherein the binary complex of palladium(II) with 8-mercaptoquinoline is isolated.
5. A process as claimed in claim 1, wherein the functional monomers are 4-vinyl pyridine and 2-hydroxy ethyl methacrylate.
6. A process as claimed in claim 1, wherein the crosslinking monomer is ethylene glycol dimethacrylate.
7. A process as claimed in claim 1, wherein the 2,2'-azobisisobutyronitrile is used as initiator.
8. A process as claimed in claim 1, wherein the palladium(II) ion imprinted polymer materials were ground and sieved after drying to obtain particles.
9. A process as claimed in claim 1, wherein palladium(II) ion embedded in the polymer is leached out using mineral acid to obtain palladium(II) ion imprinted polymer particles.
10. A process as claimed in claim 9 wherein, polymer particles obtained is used for enrichment of palladium(II) ion from dilute aqueous solutions containing copper, zinc and nickel.
11. A process as claimed in claim 9 wherein, ion imprinted polymer particle obtained is used for enhanced selectivity coefficients for palladium(II) over platinum(IV) compared to control or blank polymer particles.
12. A process for preparation of ion imprinted polymer particles for pre concentrative separation of palladium(II) ions via solid phase extraction substantially as herein described with reference to the examples and drawings accompanying this specification.




Documents:

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1886-del-2004-1886-del-2004-Correspondence Others-(09-01-2013).pdf

1886-del-2004-abstract.pdf

1886-del-2004-claims.pdf

1886-del-2004-correspondence-others.pdf

1886-del-2004-description (complete).pdf

1886-del-2004-drawings.pdf

1886-del-2004-form-1.pdf

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1886-del-2004-form-2.pdf

1886-del-2004-form-3.pdf

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Patent Number 259147
Indian Patent Application Number 1886/DEL/2004
PG Journal Number 10/2014
Publication Date 07-Mar-2014
Grant Date 27-Feb-2014
Date of Filing 30-Sep-2004
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 SOBHI DANIEL REGIONAL RESEARCH LABORATORY (CSIR), TRIVENDRUM-695 019,
2 TALASILA PRASADA RAO REGIONAL RESEARCH LABORATORY (CSIR), TRIVENDRUM-695 019,
PCT International Classification Number C08F 2/00
PCT International Application Number N/A
PCT International Filing date
PCT Conventions:
# PCT Application Number Date of Convention Priority Country
1 NA