Process for preparing chelating ion exchanger resins and the use

Details Process for preparing chelating ion exchanger resins and the use Process for preparing chelating ion exchanger resins and the use

1992-07-28

1994-03-01

Silverman, Stanley S.

Liquid purification or separation

Processes

Ion exchange or selective sorption

210681, 210660, 521 31, C02F 142

Patent

active

052904539

DESCRIPTION:

BRIEF SUMMARY
In recent years, the extraction of metals from aqueous solutions has gained increasing importance. Thus, the statutorily permissible maximum limits, especially for objectional metals in effluents, make it absolutely necessary to separate off these metals.
Moreover, the removal of interfering metals has a positive effect on numerous industrial processes such as, for example, electrolytic processes.
For the recovery of metals, extraction processes have recently increasingly displaced other methods, because they combine the advantages of high selectivity and good economics and permit metal recovery from highly dilute solutions.
Thus, solvent extraction with liquid extractants (liquid/liquid extraction) is an established method and is employed for the recovery of numerous metals.
The liquid extractants used are, inter alia, water-in-soluble 7-alkyl-8-hydroxyquinoline derivatives such as, e.g., KELEX.RTM. 100 (registered trademark of Schering AG) for the selective extraction of, for example, germanium and gallium (cf. EP-A-46,437; U.S. Pat. No. 4,724,129).
In liquid/liquid extraction, a certain loss of extractants and also additionally of used organic solvents as a result of the process is unavoidable, which is a disadvantage for both ecological and economic reasons.
There has therefore been no lack of attempts in the past to minimize these losses.
In U.S. Pat. No. 4,631,177, a process is described according to which the liquid extractants are physically adsorbed on solid carrier materials such as adsorber resins/ A certain progress was achieved by this measure. In long-term operation, however, it was found that this physical fixing of the extractants on the resins was not firm enough and consequently washing-out losses arose, which led to a deterioration in the extraction properties (loading capacity).
It was therefore proposed to fix the extractants on the carrier materials by stable chemical bonds.
Thus, it is proposed by J. R. Parrish, Chem. Ind., London 1956, 137, to bind 8-hydroxyquinoline chemically to styrene resin via azo groups. These resins proved to be relatively slow in absorbing metals and their loading capacity is also low. They were therefore able to gain as little acceptance in practice as products in which 8-hydroxyquinoline or derivatives thereof were bound via azo groups to other carrier materials (P. Burba, K. H. Lieser, Angewandte Makromolekulare Chemie, 50 (1976) 151-161; Z. Slovak, S. Slovakova, M. Smrz, Analytica Chimica Acta, 75 (1975), 127-138). A. Warshawsky et al. (U.S. Pat. No. 4,317,887) propose, inter alia, to bind 8-hydroxyquinoline via 5--CH.sub.2 --NH--CH.sub.2 -- groups or via 5--CH.sub.2 --NH--(CH.sub.2 --CH.sub.2 --NH).sub.n --CH.sub.2 -- groups to the particular carrier resins. These syntheses start from 5-chloromethylated 8-hydroxyquinolines, which are highly sensitive to hydrolysis. Because of the necessary use in their synthesis of hydrochloric acid or chlorinating agents which release hydrochloric acid, expensive corrosion-resistance special apparatus is necessary.
Moreover, highly toxic bis-(dichloromethyl) ether can be formed as a by-product in the preparation of the 5-chloromethyl-8-hydroxyquinolines.
In USSR Patent Specification 407,922, a process for the preparation of complex-forming ion exchangers containing 8-hydroxyquinoline groups is described which is characterized in that polymers containing primary and/or secondary amino groups and having a three-dimensional structure are reacted with 8-hydroxyquinoline and formaldehyde.
Reaction products of amines and epichlorohydrin and in addition also products of the amination of chloromethylated styrene/divinylbenzene copolymers are proposed as the polymers containing primary and/or secondary amino groups.
Although the reaction products of the amine/epichlorohydrin reaction products with formaldehyde and 8-hydroxyquinoline show an improved sorption capacity, they do not yet meet the requirements in practice with regard to the mechanical, physical and chemical stresses during the extraction process. Moreover, the macro

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Z. Slovak et al., Analytica Chemica Acta., 75, 127-138 (1975).

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