The Selective Flotation of Xenotime from Heavy Minerals

M S OZEREN 1 and H HUTCHINSON 2

ABSTRACT
Froth flotation is applied to mineral sand concentrates in order to produce commercially viable xenotime concentrates. Experiments indicate that a xenotime product containing 38% Y203 at 47% recovery or 34% Y203 at 83% recovery can be obtained from a 27% Y203 feed. The process involves a primary stage of reverse flotation at which oxide and silicate gangue is floated, and secondary stage of direct flotation at which xenotime is floated. Of the various collectors screened an amphoteric compound was found to be effective at both stages. This was made possible by the addition of sodium silicate at the second stage, which acted as depressant for the remainder of the gangue. Similar studies on a low grade feed material were somewhat unsatisfactory as the grade achieved fell short of what was targeted.

paper which was an extension of these earlier studies, was carried out at the Department of Mineral Technology, University of Otago in 1984 in the form of a final year student project. Despite the limited time available a large number of flotation variables and stage combinations were tested. The details can be found in the project report [1]. A more detailed description of Cable Sands' mining and processing operations is also available in the literature [2].

EXPERIMENTAL
Flotation testwork was conducted on both the low and high grade xenotime concentrates, representing, respectively, the headfeed and the product of the xenotime treatment carried out in the modified monazite circuit. Work on the low grade material was aimed at obtaining a product with a minimum of 27.5% Y203, thus replacing the existing xenotime process. Work on the high grade material was aimed at producing a premium product with 35% plus Y203.

INTRODUCTION
Cable Sands Pty Ltd conducts a beach sand mining operation at Ambergate, Western Australia. The orebody consists of a seam of essentially silica sand containing on average about 20% of valuable heavy minerals. In a processing plant at Ambergate the ore passes through various stages of wet gravity concentrating spirals where silica and other gangue minerals are removed resulting in the production of a heavy mineral bulk concentrate, rich in ilmenite, leucoxene, zircon, monazite and xenotime. The heavy mineral concentrate is road-hauled to a mineral separation plant in Bunbury, where it is stored and dried. The dried concentrate is passed over Reading crossbelt separators where the ilmenite, being relatively strongly magnetic, is recovered as standard ilmenite product. The nonmagnetics from this stage undergo further wet spiral separation to remove residual silica. The cleaner concentrate is then subjected to an attrition scrubbing process with high shear mechanical agitators. After this stage the concentrate is drained, dried, heated, and processed through high tension, electrostatic, magnetic and pneumatic separators to produce various grades of ilmenite, leucoxene, zircon, and a rare earth concentrate. The latter contains monazite, xenotime, the residual ilmenite and zircon as well as the gangue minerals; garnet, tourmaline and other silicates. This material is upgraded in a subsection of the plant to produce a monazite product, using gravity, electrostatic and magnetic equipment. This process also results in a xenotime-rich material containing up to 4% Y203. This material is stockpiled and is batched through the monazite circuit with different settings to produce a xenotime product with a grade of 30% Y203. Such a grade is commercially acceptable but Cable Sands is interested in the possibility of producing a premium grade (35% Y203) xenotime product. Currently applied separation techniques proved to be ineffective in attaining such a high quality product. The possibility that froth flotation can provide a solution to this problem was subsequently conceived and laboratory testwork was initiated at the Bunbury plant. The work described in this
1 Lecturer, Dept. of Mining Eng., University of Auckland, New Zealand. 2 Metallurgist, Cable Sands Pty Ltd, P.O. Box 133, Bunbury, 6230, Western Australia.

Composition of Samples
The chemical and mineralogical composlUons of the two samples, as supplied by Cable Sands, are given in Table 1. As is seen both samples contain substantial amounts of unwanted silicates and ilmenite, which persist in these products due to the similar specific gravity and/or overlapping magnetic and electrical properties, reflecting the limited success achieved by physical methods.
TABLE 1. Composition ofthe samples used

Oxide/Mineral [%]

Low Grade Sample 3.9 6.4 5.21 18.1 18.0 27.0 3.1 4.6 43.9

High Grade Sample 28.9 47.1 0.56 1.9 7.26 10.9 0.22 0.3 39.8

Y203 Xenotime (YP04) Ce02 Monazite (CeP04) Ti02 Ilmenite (FeTi03) Zr02 Zircon (ZrSi04) Garnet, tourmaline and other silicates

Flotation Parameters
Tests were conducted in the model D-12 Denver laboratory flotation machine. The unchanged parameters include pulp
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density ( 10% solids by mass), agitator speed (llOOrpm), aeration (fully open valve). The parameters examined included conditioning time, pH, type of collector and flotation time. In addition effects of recleaning, attrition scrubbing, and grinding were also observed.

TABLE 2. Mass balance for best results from tests on low grade sample Products Mass (%) Grade (%Y20 3) 0.61 6.78 1.05 3.56 Recovery (%Y203) 3.53 86.41 10.06 100.00

Flotation Procedure
After a number of preliminary tests it was observed that the most promising procedure was to conduct initially a reverse flotation stage resulting in a gangue-rich froth product, and a sink concentrate consisting mainly of xenotime and monazite. The concentrate thus achieved would then be subjected to a direct flotation stage aiming at further upgrading the xenotime by floating it away from the remainder of the minerals. Stage I froth Stage IT froth Stage IT sink Feed 20.57 45.34 34.09 100.00

Reverse Flotation
A large number of collectors, supplied by Hoescht via Cable Sands, were screened at pH values ranging form 3 to 10, with a frother such as MIRC or pine oil added as required. Collectors of anionic type produced poor results. Promising results were observed with amphoteric collectors acting highly selectively towards gamet and ilmenite in acidic conditions. The most effective amphoteric collector observed was F74286 (no more information is available about this reagent at this stage). In acid conditions, where it should have a cationic ionicity, thjs reagent showed little or no tendency to collect monazite or xenotime, but the gangue recovery in the float product was also less than satisfactory.

High Grade Sample The tests on this sample were highly successful. The best results, which are given in Table 3, were achieved under the following conditions: Stage I (reverse flotation): Feed: Collector: pH: Frother: Conditioning time: Flotation time: Stage IT (direct flotation) Collector: Sodium silicate: pH: Conditioning time:

attritioned in HCl, top size 212m as in original F74286, O.4cc for 137g solids 3 withH2S04 MIRC (2 drops) 10 minutes 2 minutes

Direct Flotation
It was possible to selectively float xenotime from associated minerals using F74286 as collector and sodium silicate as depressant for the remaining silicates and ilmenite. A high quantitity of sodium silicate e.g., 3 to 7kg/tonne, was found to be necessary to create the required depression. This resulted in a pulp pH of about 10, at which the collector should show anionic action. Despite the high quantitites used sodium silicate proved to be highly selective in its depressing action on silicates.

F74286 (additionaI2cc) 5kg/tonne 10.6 10 minutes

Stage ill (re-floating of stage IT froth): No further reagents added Conditioning time: 3.5 minutes As is seen in Table 3, a xenotime final product with a grade of 37.83% Y 203 is achieved at a recovery of 46.8%Y203. Also note that the feed to stage II is a xenotime product with a grade of 34.06% Y203 at 83.9% Y203 recovery. Hence a recleaning stage, although it improves the grade significantly, is somewhat unattractive due to a substantial drop in recovery.

RESULTS Low Grade Sample

The best results on this sample which are given in Table 1, were achieved under the following conditions: Stage I (reverse flotation): Feed: Collector: pH: Conditi oning time: Stage IT (direct flotation) Collector: Sodium silicate: pH: Conditioning time:

attritioned in HCl, top size 212m as in original F74286, 0.2cc for 125g solids 4.1 with HCl 5 minutes

TABLE 3. Mass balance for best results from tests on high grade sample Products Mass (%) Grade (%Y203) 14.43 37.83 30.19 27.16 Recovery (%Y20 3) 16.92 46.80 36.29 100.00

F74286 (additional1.2cc) 5.2kg/tonne 9.8 5 minutes.

Stage I froth Stage ill froth Stage IT sink. Stage ill sink Feed

31.85 33.60 90 32.65 100.00

As is seen in Table 2, the maximum' grade achieved on this sample was 6.78% Y203, which is well below the desired 27.5% Y203.

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CONCLUSIONS
It seems possible that froth flotation can play an important role in the benefication of beachsands containing metal oxides and rare-earth phosphates such as monazite and xenotime, particularly as a-final cleaning technique. According to experimental results it is possible to effectively float xenotime or possibly monazite from oxides and silicates in the presence of sodium silicate acting as a depressant. An amphoteric compound was found to be a highly selective collector for silicates and iImenite in acidic conditions. In alkaline conditions the same compound acts in an opposite manner so as to collect phosphates rather than the oxides and silicates.

ACKNOWLEDGEMENT
The authors wish to thank the Cable Sands Pty Ltd of Australia for initiating this project and supplying the samples and collectors used. Thanks are also due to Associate Professor Buckenham for permission to use facilities at the University of Otago.

REFERENCES
Brodie, H.A., 1984, Upgrading of xenotime concentrates by flotation. Final year project report, Department of Mineral Technology, University of Otago. Newman, P.w., Scanlon, T.J., 1980, Dry mineral sand separation plant of Cable Sands Pty. Ltd, Bunbury, W.A., The Aus IMM monograph 10, pp. 763-68.

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