Chemistry of inorganic compounds – Treating mixture to obtain metal containing compound – Group viib metal
Reexamination Certificate
1999-03-29
2001-07-31
Bos, Steven (Department: 1754)
Chemistry of inorganic compounds
Treating mixture to obtain metal containing compound
Group viib metal
C423S054000, C423S063000, C423S087000, C423S089000, C423S099000, C423S112000, C423S139000, C423S157000, C210S634000
Reexamination Certificate
active
06267936
ABSTRACT:
FIELD OF THE INVENTION
The present invention relates to the use of hydrocarbon-soluble aminomethylenephosphonic acid derivatives comprising the structural element of the formula I
where R
1
and R
2
are hydrogen, C
1
-C
30
-alkyl which can additionally bear up to 15 hydroxyl groups and/or be interrupted by up to 14 non-adjacent oxygen atoms, C
2
-C
30
-alkenyl, C
7
-C
18
-aralkyl or C
6
-C
14
-aryl which can be substituted by up to three C
1
-C
12
-alkyl groups, C
1
-C
12
-alkoxy groups, halogen atoms, cyano groups, hydroxyl groups or C
1
-C
4
-alkoxycarbonyl groups, for the solvent extraction of one or more metal ions from the group consisting of lithium, sodium, potassium, rubidium, cesium, francium, beryllium, magnesium, calcium, strontium, barium, radium, scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, promethium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, actinium, thorium, protactinium, neptunium, plutonium, americium, curium, berkelium, californium, einsteinium, fermium, mendelevium, nobelium, lawrencium, titanium, zirconium, hafnium, vanadium, niobium, tantalum, chromium, molybdenum, tungsten, manganese, technetium, rhenium, ruthenium, osmium, cobalt, rhodium, iridium, nickel, platinum, copper, silver, gold, zinc, cadmium, mercury, aluminum, gallium, thallium, germanium, tin, lead, arsenic and polonium from aqueous solutions.
The invention also relates to the use of these hydrocarbon-soluble aminomethylenephosphonic acid derivatives for selectively separating one or more of the above metal ions from one another by solvent extraction.
DESCRIPTION OF THE BACKGROUND
The removal of undesired accompanying metals from aqueous solutions and the separation of metals is particularly important in hydrometallurgical nonferrous metal production, eg. in the winning of copper, zinc, noble metals or other special metals. Solutions of desired metals are frequently obtained from ores by digestion or leaching with aqueous, usually acid systems. The interfering or accompanying metals have to be removed from these solutions and separated from one another. In addition, the work-up of metal-containing wastes or residues (eg. flue dusts or precipitation sludges from wastewater treatment) and the recycling of used metal products (eg. catalysts) nowadays play an ever more important role in the provision of aqueous solutions of desired metals. Regardless of the origin of the metal salt solutions, it is always necessary to remove interfering elements from these solutions of desired metals and to separate the metals into individual fractions so that pure metals can be isolated. Apart from improving the quality of the desired metals, recovery of metals and reducing contamination of landfill areas is sought in the waste and residue processing sector for economic and ecological reasons.
The solvent extraction of iron ions is known in the literature. Thus, DE-A 38 01 430 (1) describes the use of a mixture comprising a primary amine and an alkylphosphonic monoester such as mono-2-ethylhexyl 2-ethylhexylphosphonate for the removal of iron(III) ions from acid zinc salt solutions by solvent extraction.
Furthermore, JP-A 1985/077936 (2) discloses that aminomethylenephosphonic acid derivatives are suitable for the solvent extraction of uranium, antimony or bismuth and of indium.
U.S. Pat. No. 4,741,831 (3) relates to a process for separating metals such as iron, cobalt, copper, vanadium, cadmium, nickel, zinc, lead or aluminum from aqueous solutions using water-soluble polymeric complexing agents, for example polyethyleneiminephosphonates. The metal complex is subsequently separated off by dialysis or ultrafiltration by means of membranes.
WO-A 96/00309 (4) describes the solvent extraction of iron ions from aqueous solutions, particularly from solutions of zinc or copper, by means of the present hydrocarbon-soluble aminomethylenephosphonic acid derivatives.
In the reference Proc. Symp. Solvent Extr. (1995) 59-60 (5), Y. Baba, Y. Kawano and J. Shibata describe the separation of palladium from chloride solutions by means of di (2-ethylhexyl) aminomethylenephosphonic acid.
However, the above processes of the prior art still have disadvantages. They are mostly not efficient enough and are too uneconomical. In particular, the selectivity of the separation of the interfering metals from the desired metals and the loading capacity of the complexing agents used are still in need of improvement.
SUMMARY OF THE INVENTION
It is an object of the present invention to find an improved system for the solvent extraction of metal ions from aqueous solutions which no longer has the disadvantages of the prior art.
We have found that this object is achieved by the use as defined in the introduction of the hydrocarbon-soluble aminomethylenephosphonic acid derivatives having the structural element I.
Preferably, use is made of hydrocarbon-soluble aminomethylenephosphonic acid derivatives comprising the structural element of the formula Ia
For the purpose described, particular preference is given to hydrocarbon-soluble aminomethylenephosphonic acid derivatives of the general formula II
where
R
3
to R
6
are each hydrogen, C
1
-C
30
-alkyl which can additionally bear up to 15 hydroxyl groups and/or be interrupted by up to 14 non-adjacent oxygen atoms, C
2
-C
30
-alkenyl, C
7
-C
18
-aralkyl, C
6
-C
14
-aryl which can be substituted by up to three C
1
-C
12
-alkyl groups, C
1
-C
12
-alkoxy groups, halogen atoms, cyano groups, hydroxyl groups or C
1
-C
4
-alkoxycarbonyl groups, or are each a group of the formula —CR
1
R
2
—PO
3
H
2
, —CH
2
—COOH or —CH
2
—CH(OH)—R
1
, where at least one of the radicals R
3
to R
6
is the group —CR
1
R
2
—PO
3
H
2
and at least a further one of these radicals is C
6
-C
30
-alkyl, C
6
-C
30
-alkenyl, C
7
-C
18
-aralkyl, unsubstituted or substituted C
6
-C
14
-aryl or the group —CH
2
—CH(OH)—R
9
, where R
9
is C
6
-C
30
-alkyl, C
6
-C
30
-alkenyl, C
7
-C
18
-aralkyl or unsubstituted or substituted C
6
-C
14
-aryl, and where R
1
and R
2
are as defined above,
A is a C
1
-C
12
-alkylene group which can additionally bear as substituents up to three C
1
-C
30
-alkyl groups, C
2
-C
30
-alkenyl groups, C
7
-C
18
-aralkyl groups or C
6
-C
14
-aryl groups which can in turn be substituted by up to three C
1
-C
12
-alkyl groups, C
1
-C
12
-alkoxy groups, halogen atoms, cyano groups, hydroxyl groups or C
1
-C
4
-alkoxycarbonyl groups, where, if a plurality of groups A are present, these can be identical or different, and
p is a number from 0 to 30,000.
The compounds II can be in the form of monomers (p=0), oligomers or polymers.
Suitable straight-chain or branched alkyl radicals as R
1
to R
9
and as substituents on aryl groups, which are mentioned as C
1
-C
30
-, C
6
-C
30
- or C
1
-C
12
-alkyl radicals, are, for example, methyl, ethyl, n-propyl, iso-propyl-, n-butyl, iso-butyl, sec-butyl, tert-butyl, n-amyl, iso-amyl, sec-amyl, tert-amyl, neopentyl, n-hexyl, n-heptyl, n-octyl, 2-ethylhexyl, n-nonyl, iso-nonyl, n-decyl, n-undecyl, n-dodecyl, n-tridecyl, iso-tridecyl, n-tetradecyl, n-pentadecyl, n-hexadecyl, n-heptadecyl, n-octadecyl and n-eicosyl.
Suitable alkyl radicals additionally bearing up to 15, in particular up to 10, especially up to 5, hydroxyl groups and/or interrupted by up to 14, in particular by up to 9, especially by up to 4, non-adjacent oxygen atoms are, for example, corresponding polyoxyalkylene chains, in particular polyoxyethylene chains, whose terminal hydroxyl groups can be etherified by alkyl radicals, for example groups of the formula —CH
2
CH
2
—OH, —CH
2
CH
2
—O—CH
3
, —CH
2
CH
2
—O—CH
2
CH
2
—OH, —CH
2
CH
2
—O—CH
2
CH
2
—O—CH
3
, —CH
2
CH
2
CH
2
—OH, —CH
2
CH
2
CH
2
—O—CH
2
CH
3
, —CH
2
CH
2
—O—CH
2
CH
2
—O—CH
2
CH
2
—OH or —CH
2
CH
2
—O—CH
2
CH
2
—O—CH
2
CH
2
—O—CH
2
CH
2
—OH.
Among these, preferred radicals as R
1
and R
2
and as substituents on aryl groups are in general lower alkyl radicals, in particular C
1
-C
12
-alkyl radicals, but especially C
1
-C
4
-alkyl radicals, in particular ethyl an
Delmas Francisco
Ehle Michael
Nogueira Carlos
Oppenlander Knut
BASF - Aktiengesellschaft
Bos Steven
Oblon & Spivak, McClelland, Maier & Neustadt P.C.
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