Composition And Method For Use Of 1-Alkyl-5-Oxopyrrolidine-3-Carboxylic Acids As Collectors For Phosphate And Lithium Flotation

Abstract

The invention relates to a flotation agent for lithium or phosphate ore, comprising at least one fatty acid and at least one 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof of the formula (1)

##STR00001##

wherein R is a C.sub.7 to C.sub.21 alkyl or alkenyl group, wherein the amount of fatty acid is from 70 to 99 wt.-%, and wherein the amount of the 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid of the formula (I) is from 1 to 30 wt.-%.

Claims

1. A flotation agent for a phosphate or a lithium ore, comprising at least one fatty acid and at least one 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof of the formula (I) ##STR00003## wherein R is a C.sub.7 to C.sub.21 alkyl or alkenyl group, wherein the amount of fatty acid is from 70 to 99 wt.-%, and wherein the amount of the 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid of the formula (I) is from 1 to 30 wt.-%.

2. The flotation agent as claimed in claim 1, wherein the fatty acid has from 8 to 26 carbon atoms.

3. The flotation agent as claimed in claim 1, wherein R is a C.sub.11 to C.sub.19 alkyl or alkenyl residue.

4. The flotation agent as claimed in claim 1, wherein R is a C.sub.13 to C.sub.18 alkyl or alkenyl residue.

5. The flotation agent as claimed in claim 1, wherein R is a C.sub.12 to C.sub.17 alkenyl residue having at least one double bond.

6. The flotation agent as claimed in claim 1, wherein the ore is a phosphate ore and R is a C.sub.18 alkenyl group.

7. The flotation agent as claimed in claim 1, wherein the ore is a lithium ore and R is a C.sub.12 alkyl group.

8. (canceled)

9. A process for flotating a phosphate ore, the process comprising the step of adding from 100 to 1000 g/t of a flotation reagent comprising at least one fatty acid and at least one 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof of the formula (I) ##STR00004## wherein R is a C.sub.7 to C.sub.21 alkyl or alkenyl group, wherein the amount of fatty acid is from 70 to 99 wt.-%, and wherein the amount of the 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid of the formula (I) is from 1 to 30 wt.-%, to an aqueous suspension of the phosphate ore, and aerating the so obtained mixture.

10. The process for flotating a phosphate ore as claimed in claim 9, wherein the fatty acid has from 8 to 26 carbon atoms.

11. The process for flotating a phosphate ore as claimed in claim 9, wherein R is a C.sub.11 to C.sub.19 alkyl or alkenyl residue.

12. The process for flotating a phosphate ore as claimed in claim 9, wherein R is a C.sub.13 to C.sub.18 alkyl or alkenyl residue.

13. The process for flotating a phosphate ore as claimed in claim 9, wherein R is a C.sub.12 to C.sub.17 alkenyl residue having at least one double bond.

14. The process for flotating a phosphate ore as claimed in claim 9, wherein R is a C.sub.18 alkenyl group.

15. A process for flotating a lithium ore, the process comprising the step of adding from 100 to 1000 g/t of a flotation reagent comprising at least one fatty acid and at least one 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof of the formula (I) ##STR00005## wherein R is a C.sub.7 to C.sub.21 alkyl or alkenyl group, wherein the amount of fatty acid is from 70 to 99 wt.-%, and wherein the amount of the 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid of the formula (I) is from 1 to 30 wt.-%, to an aqueous suspension of the phosphate ore, and aerating the so obtained mixture.

16. The process for flotating a lithium ore as claimed in claim 15, wherein the fatty acid has from 8 to 26 carbon atoms.

17. The process for flotating a lithium ore as claimed in claim 15, wherein R is a C.sub.11 to C.sub.19 alkyl or alkenyl residue.

18. The process for flotating a lithium ore as claimed in claim 15, wherein R is a C.sub.13 to C.sub.18 alkyl or alkenyl residue.

19. The process for flotating a phosphate ore as claimed in claim 15, wherein R is a C.sub.12 to C.sub.17 alkenyl residue having at least one double bond.

20. The process for flotating a phosphate ore as claimed in claim 9, wherein R is a C.sub.12 alkyl group.

Description

EXAMPLES

[0021] Collecting Agent Formulation Preparation for All Examples

[0022] A crude soy oil fatty acid was heated to around 60° C. until all solids are molten and are subsequently homogenized. A 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof was heated to around 60° C. until all solids are molten and are subsequently homogenized. 85 g of the molten homogenized crude soy oil fatty acid was transferred to a heated beaker and (under stirring at around 100 rpm) 15 g of the molten homogenized 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof was added slowly, and the mixture was homogenized for 30 minutes under heating at 60° C.

[0023] Materials Used:

TABLE-US-00001 TABLE 1 Description of the Fatty Acid and Co-collectors Ratio Reagent 1: Reagent 1 Reagent 2 Reagent 2 Fatty Acid Crude soy oil fatty — 1:0 acid (Almad S/A) (comparative) Co-collector 1 Itaconic acid Octylamine 1:1 Co-collector 2 Itaconic acid Laurylamine 1:1 Co-collector 3 Itaconic acid Oleylamine 1:1 Co-collector 4 Itaconic acid Cocoylamine 1:1 Co-collector 5 Itaconic acid Stearylamine 1:1 Co-collector 6 Itaconic acid Dodecyl 1:1 dipropylene triamine Co-collector 7 Itaconic acid Dodecyl 2:1 dipropylene triamine Co-collector 8 Itaconic acid Tallowamine 1:1

Example 1

[0024] Applications-Related Investigations for Phosphate Flotation

[0025] Froth flotation experiments were conducted using a Denver laboratory flotation cell. 1.00 kg of ground ore was conditioned by stirring at 1100 rpm with 0.66 liter of water (solids content of the pulp 60 wt-%). A depressant (maize corn caustic starch) and the above described collector was added and conditioning continued for 5 minutes thereafter. The solids content of the pulp was adjusted to 30% by adding water. The pH was adjusted to 9.0 and the mixture was stirred for 1 minute.

[0026] The stirring was adjusted to 1400 rpm, the air intake was opened, and the ore was floated for 3 minutes, obtaining the rougher concentrate (froth) and rougher tailing (remaining ore in the cell). The rougher concentrate was returned to the flotation cell and was floated again, without adding collector, for 2 minutes at 1000 rpm, obtaining the cleaner concentrate (phosphate concentrate) and cleaner tailing. The cleaner concentrate and cleaner tailing, besides the rougher tailing (final tailing dried at 105±5° C.), were weighed and analysed to determine their phosphate grade by the XRF method (x-ray fluorescence).

[0027] The efficiency of Collecting Agent Formulations based on 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof (Collecting Agent Formulations P2 to P17) were compared to the pure Fatty Acid (Collecting Agent Formulation P1). The concentration of fatty acid can be reduced, relative to the comparison product, from 100% to 85% thereby improving the recovery and keeping the P.sub.2O.sub.5 in acceptable grade. P.sub.2O.sub.5 in acceptable grade means a target of ≥35.8 weight-% P.sub.2O.sub.5. In addition, total replacement of fatty acid by Collecting Agent Formulation P12 (oleyl 1-alkyl-5-oxopyrrolidine-3-carboxylic acid) improved the phosphate recovery along with keeping the P.sub.2O.sub.5 in acceptable grade (Target ≥35.8 wt.-% P.sub.2O.sub.5).

TABLE-US-00002 TABLE 2 Composition and flotation results for phosphate ore Formulation (wt.-%) Collecting Com- Com- Grade Recovery Agent ponent ponent Dosage P.sub.2O.sub.5 P.sub.2O.sub.5 Formulation 1 % 2 % (g/t) (wt.-%) (wt.-%) P1  Fatty 100 — — 250 39.60 48.08 Acid P2  Fatty 85 Co- 15 250 38.91 51.78 Acid collector 1 P3  Fatty 85 Co- 15 250 39.00 53.55 Acid collector 2 P4  Fatty 85 Co- 15 250 39.61 65.40 Acid collector 3 P5  Fatty 85 Co- 15 250 39.97 50.11 Acid collector 4 P6  Fatty 85 Co- 15 250 38.95 55.68 Acid collector 5 P7  Fatty 85 Co- 15 250 38.86 1.39 Acid collector 6 P8  Fatty 85 Co- 15 250 39.99 14.57 Acid collector 7 P9  Fatty 85 Co- 15 250 39.90 37.41 Acid collector 8 P10 Fatty 0 Co- 100 250 17.47 2.64 Acid collector 1 P11 Fatty 0 Co- 100 250 17.47 2.64 Acid collector 2 P12 Fatty 0 Co- 100 250 39.06 81.28 Acid collector 3 P13 Fatty 0 Co- 100 250 30.37 3.11 Acid collector 4 P14 Fatty 0 Co- 100 250 n.a. n.a. Acid collector 5 P15 Fatty 0 Co- 100 250 10.25 0.58 Acid collector 6 P16 Fatty 0 Co- 100 250 14.73 0.61 Acid collector 7 P17 Fatty 0 Co- 100 250 15.37 0.95 Acid collector 8 *n.a. means that there was no flotation observed

Example 2

[0028] Materials used are those listed in Table 1 above.

[0029] Applications-related investigations for lithium flotation Froth flotation experiments were conducted using a Denver laboratory flotation cell. 0.8 kg of ground ore was conditioned by stirring at 1500 rpm with 0.8 liter of water (solids content of the pulp 50 wt-%). Collector was added and conditioning continued for 7 minutes thereafter. The pH was adjusted to 10.0 and the mixture was stirred for 1 minute.

[0030] The stirring was adjusted to 1300 rpm, the air intake was opened, and the ore was floated for 7 minutes, obtaining the rougher concentrate (froth) and rougher tailings. The rougher concentrate and rougher tailing are dried at 105±5° C., were weighed and analysed to determine their lithium grade by ICP-OES method.

[0031] The efficiency of Collecting Agent Formulations based on 1-alkyl-5-oxopyrrolidine-3-carboxylic acid or 1-alkenyl-5-oxopyrrolidine-3-carboxylic acid or a mixture thereof (Collecting Agent Formulation L2 to L17) were compared to the pure Fatty Acid (Collecting Agent Formulation L1). The concentration of fatty acid can be reduced, relative to the comparison product, from 100% to 85% thereby improving the recovery and keeping the Li.sub.2O in acceptable grade. Li.sub.2O in acceptable grade means a target of ≥4.0 weight-% Li.sub.2O, considering the rougher concentrate.

TABLE-US-00003 TABLE 3 Composition and flotation results for lithium ore Formulation (wt.-%) Collector Com- Com- Grade Recovery Agent ponent ponent Dosage Li.sub.2O Li.sub.2O Formulation 1 % 2 % (g/t) (wt.-%) (wt.-%) L1  Fatty 100 — — 600 4.89 51.6 Acid L2  Fatty 85 Co- 15 600 3.85 48.5 Acid collector 1 L3  Fatty 85 Co- 15 600 4.76 77.4 Acid collector 2 L4  Fatty 85 Co- 15 600 5.03 58.0 Acid collector 3 L5  Fatty 85 Co- 15 600 4.86 65.5 Acid collector 4 L6  Fatty 85 Co- 15 600 5.11 40.6 Acid collector 5 L7  Fatty 85 Co- 15 600 2.50 25.4 Acid collector 6 L8  Fatty 85 Co- 15 600 4.33 34.3 Acid collector 7 L9  Fatty 85 Co- 15 600 3.66 17.1 Acid collector 8 L10 Fatty 0 Co- 100 600 1.10 8.50 Acid collector 1 L11 Fatty 0 Co- 100 600 1.43 30.9 Acid collector 2 L12 Fatty 0 Co- 100 600 3.05 12.6 Acid collector 3 L13 Fatty 0 Co- 100 600 1.55 10.8 Acid collector 4 L14 Fatty 0 Co- 100 600 n.a. n.a. Acid collector 5 L15 Fatty 0 Co- 100 600 1.24 47.5 Acid collector 6 L16 Fatty 0 Co- 100 600 1.35 26.0 Acid collector 7 L17 Fatty 0 Co- 100 600 1.55 5.48 Acid collector 8 *n.a. means that there was no flotation observed