Monazite and apatite paragenetic ore enrichment method

Abstract

The present invention discloses a monazite and apatite paragenetic ore enrichment method. High-grade and high-recovery-rate monazite concentrate can be obtained by adopting the method through steps of ore grinding, floatation, magnetic separation and low-acid advanced leaching treatment and re-floatation. In this process, the applicable range of ore pulp temperature is wide, the process flow is short, the ore dressing conditions are mild, the energy consumption is small, the used diluted acid can be cyclically regenerated and used, the pollution is small, the environmental stress is small and the recovery rate of low-grade monazite and apatite paragenetic ores can be obviously improved.

Claims

1. A monazite and apatite paragenetic ore enrichment method, comprising the following steps: performing acid leaching of mixed concentrate containing rare earth and apatite with inorganic acid and then performing liquid-solid separation to obtain acid leaching residues and leaching solution, wherein the acid leaching residues are monazite and apatite paragenetic ores; and a liquid-solid ratio of the inorganic acid to the mixed concentrate is 2.0-5.0, an acid excess coefficient is 0.2-3.0, and 0.1-0.3% of flocculating agent by mass percentage based on a mass sum of the mixed concentrate and the inorganic acid is added during the acid leaching, and liquid temperature of a leaching system during the acid leaching is 20-120 C.

2. The monazite and apatite paragenetic ore enrichment method according to claim 1, characterized in that the mixed concentrate is a solid matter obtained by performing ore grinding to raw ores, then performing pulp mixing and performing primary flotation and/or magnetic separation, the content of REO in the raw ores of the monazite and apatite paragenetic ores is 0.3-10% by mass.

3. The monazite and apatite paragenetic ore enrichment method according to claim 1, characterized in that the inorganic acid is one of HCl, HBr, HI, HNO.sub.3 and H.sub.3PO.sub.4.

4. The monazite and apatite paragenetic ore enrichment method according to claim 1, characterized in that the inorganic acid is HCl and/or H.sub.3PO.sub.4, and a volume ratio of HCl to H.sub.3PO.sub.4 is 2:1 when the inorganic acid is mixture of HCl and H.sub.3PO.sub.4.

5. The monazite and apatite paragenetic ore enrichment method according to claim 1, characterized in that the flocculating agent is polyacrylamide and/or gelatin.

6. The monazite and apatite paragenetic ore enrichment method according to claim 1, characterized in that the flocculating agent is polyacrylamide and gelatin, and a mass ratio of the polyacrylamide to the gelatin is 2:1.

7. The monazite and apatite paragenetic ore enrichment method according to claim 2, characterized in that a mass ratio of water to solid substances in ore pulp is (2-3):5 during the primary flotation.

8. The monazite and apatite paragenetic ore enrichment method according to claim 2, characterized in that magnetic field intensity during the magnetic separation is 8000-12000 Oe.

9. The monazite and apatite paragenetic ore enrichment method according to claim 7, characterized in that the ore pulp is obtained during the primary flotation by a method which comprises the following steps: grinding the raw ores into ones wherein the weight of particles with a particle size of <0.074 mm is not lower than 60% of total weight of the raw ores, and adding water for pulp mixing.

10. The monazite and apatite paragenetic ore enrichment method according to claim 7, characterized in that the primary flotation comprises primary roughing and primary cleaning.

11. The monazite and apatite paragenetic ore enrichment method according to claim 10, characterized in that the primary roughing is flotation by adding flotation agent I into the ore pulp, the flotation agent I comprises an inhibitor and a collector, and the collector is at least one of sodium aliphatate and oxidized paraffin wax soap.

12. The monazite and apatite paragenetic ore enrichment method according to claim 11, characterized in that a dose of the collector in the flotation agent I is 200-500 g/t raw ore.

13. The monazite and apatite paragenetic ore enrichment method according to claim 11, characterized in that the inhibitor in the flotation agent I is water-soluble silicate or water-soluble fluosilicate.

14. The monazite and apatite paragenetic ore enrichment method according to claim 10, characterized in that the primary cleaning is blank cleaning without adding any agent.

15. The monazite and apatite paragenetic ore enrichment method according to claim 11, characterized in that a dose of the inhibitor in the flotation agent I is 500-2000 g/t raw ore.

16. The monazite and apatite paragenetic ore enrichment method according to claim 10, characterized in that the primary flotation further comprises scavenging, a collector used for the scavenging is at least one of sodium aliphatate and oxidized paraffin wax soap, and a dose of the collector is 100-250 g/t.Math.raw ore; and an inhibitor is water-soluble silicate or water-soluble fluosilicate, and a dose of the inhibitor is 250-1000 g/t.Math.raw ore.

17. The monazite and apatite paragenetic ore enrichment method according to claim 11, characterized in that the collector in the flotation agent I is at least one of sodium oleate, saturated sodium aliphatate, sodium dodecyl sulfate and oxidized paraffin wax soap.

18. The monazite and apatite paragenetic ore enrichment method according to claim 11, characterized in that the collector in the flotation agent I is sodium oleate.

19. The monazite and apatite paragenetic ore enrichment method according to claim 16, characterized in that the collector used during scavenging is at least one of sodium oleate, saturated sodium aliphatate, sodium dodecyl sulfate and oxidized paraffin wax soap.

20. The monazite and apatite paragenetic ore enrichment method according to claim 16, characterized in that the collector used during scavenging is sodium oleate.

21. The monazite and apatite paragenetic ore enrichment method according to claim 20, characterized in that, after the acid leaching, the acid leaching residues are taken and added with water for pulp mixing and flotation agent II is added for secondary flotation to obtain monazite concentrate.

22. The monazite and apatite paragenetic ore enrichment method according claim 21, characterized in that the flotation agent II comprises an inhibitor and a collector, and the collector is at least one of sodium aliphatate and oxidized paraffin wax soap.

23. The monazite and apatite paragenetic ore enrichment method according to claim 22, characterized in that the secondary flotation comprises secondary roughing and secondary cleaning; and during the secondary flotation, a mass ratio of water to solid substances in the ore pulp is (3-6):10.

24. The monazite and apatite paragenetic ore enrichment method according to claim 23, characterized in that the flotation agent II is added during the secondary roughing, the flotation agent II comprises an inhibitor and a collector, and the collector is at least one of sodium aliphatate and oxidized paraffin wax soap.

25. The monazite and apatite paragenetic ore enrichment method according to claim 24, characterized in that a dose of the collector in the flotation agent II is 200-500 g/t.Math.raw ore; and the collector in the flotation agent II is at least one of sodium oleate, saturated sodium aliphatate, sodium dodecyl sulfate and oxidized paraffin wax soap.

26. The monazite and apatite paragenetic ore enrichment method according to claim 24, characterized in that the inhibitor in the flotation agent II is water-soluble silicate or water-soluble fluosilicate.

27. The monazite and apatite paragenetic ore enrichment method according to claim 24, characterized in that the inhibitor in the flotation agent II is water glass, sodium silicate and/or sodium fluosilicate, and a dose thereof is 500-2000 g/t.Math.raw ore.

28. The monazite and apatite paragenetic ore enrichment method according to claim 23, characterized in that the secondary flotation further comprises at least one time of scavenging, a collector used for the scavenging is at least one of sodium aliphatate and oxidized paraffin wax soap, and a dose of the collector is 100-250 g/t.Math.raw ore; and an inhibitor used for the scavenging is water-soluble silicate or water-soluble fluosilicate, and a dose of the inhibitor is 250-1000 g/t.Math.raw ore.

29. The monazite and apatite paragenetic ore enrichment method according to claim 23, characterized in that the secondary cleaning is blank cleaning without adding any agent and the blank cleaning is conducted 2-5 times.

30. The monazite and apatite paragenetic ore enrichment method according to claim 21, characterized in that magnetic separation is performed to the obtained monazite concentrate after the secondary flotation and magnetic field intensity during the magnetic separation is 8000-12000 Oe.

31. The monazite and apatite paragenetic ore enrichment method according to claim 30, characterized in that the liquid temperature of a leaching system during the acid leaching is 40-100 C. and time of acid leaching treatment is 50-300 min.

32. The monazite and apatite paragenetic ore enrichment method according to claim 31, characterized in that the acid excess coefficient during the acid leaching is 0.2-2.0.

Description

DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 is a process flowchart of a method provided by the invention, wherein the part in a dotted line frame is the treatment step of enrichment of monazite and apatite paragenetic ores performed by using inorganic acid and flocculating agent in the present invention and the step shown by the part in round brackets is an unnecessary step.

DESCRIPTION OF THE EMBODIMENTS

(2) The above-mentioned contents of the present invention will be further described below in detail through embodiments. However, it shall not be understood as that the range of the above-mentioned subject of the present invention is only limited to the following embodiments. Enrichment of monazite and apatite paragenetic ores which is realized based on the above-mentioned contents of the present invention belongs to the range of the present invention.

Embodiment 1

(3) For certain monazite and apatite paragenetic ores originated from United States, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 0.45% and 5.0%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 75% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 2:5, a water glass mixture was added and used as an inhibitor, sodium oleate was added and used as a collector, and a flotation process including one time of roughing, one time of scavenging and four times of cleaning at normal temperature was performed, wherein a dose of the water glass during roughing is 1500 g/t.Math.raw ore, a dose of sodium oleate is 300 g/t.Math.raw ore, the dose of the agent was halved during one time of scavenging, the four times of cleaning are blank cleaning, floated mixed concentrate can be obtained thereby, the content of REO therein is 2.5%, the operation recovery rate of REO is 85%, the content of P.sub.2O.sub.5 is 31.2% and the operation recovery rate of P.sub.2O.sub.5 is 92.5%. The mixed concentrate was subjected to high-intensity magnetic separation at magnetic field intensity of 10000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 6.5%, the operation recovery rate of REO is 92%, the content of P.sub.2O.sub.5 is 25% and the operation recovery rate of P.sub.2O.sub.5 is 30%. Nonmagnetic products are high-purity phosphate concentrate products. Hydrochloric acid was used and mixed with the magnetic products, an acid excess coefficient was controlled to be 3.0, a liquid-solid ratio L/S was controlled to be 2.0, temperature was controlled to be 90 C., 0.1% of polyacrylamide and gelatin mixture by mass percentage was added and used as flocculating agent, a mass ratio of polyacrylamide to gelatin is 2:1, the leaching time is 150 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 25%, the operation recovery rate thereof is 90%, water was added until a mass ratio of water to solid substances in ore pulp is 3:10, a water glass mixture was added and used as an inhibitor, sodium oleate was added and used as a collector, and a flotation process including one time of roughing, one time of scavenging and three times of cleaning was performed, wherein the dose of the water glass during roughing is 1500 g/t.Math.raw ore, the dose of sodium oleate is 500 g/t.Math.raw ore, the dose of the water glass and sodium oleate during scavenging is half of the dose during roughing, the three times of cleaning are blank cleaning, monazite concentrate with the grade of REO which is 55% can be obtained through flotation retreatment, then strong-intensity magnetic flotation was performed to the floated concentrate at magnetic field intensity of 8000 Oe, magnetic products, i.e., monazite concentrate with the grade of REO which is 60.25% can be obtained thereby, and the operation recovery rate thereof is 93%.

Embodiment 2

(4) For certain monazite and apatite paragenetic ores originated from Australia, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 3.5% and 12%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 80% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 9:20, a water glass mixture was added and used as an inhibitor, oxidized paraffin wax soap was added and used as a collector, and the flotation process including one time of roughing, one time of scavenging and three times of cleaning at normal temperature was performed, wherein the dose of the water glass during roughing is 2000 g/t.Math.raw ore, the dose of oxidized paraffin wax soap is 400 g/t.Math.raw ore, the dose of the agent was halved during one time of scavenging, the three times of cleaning are blank cleaning, floated mixed concentrate can be obtained thereby, the content of REO therein is 8%, the operation recovery rate of REO is 95%, the content of P.sub.2O.sub.5 is 32% and the operation recovery rate of P.sub.2O.sub.5 is 94%. The mixed concentrate was subjected to high-intensity magnetic separation at magnetic field intensity of 10000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 12%, the operation recovery rate of REO is 92%, the content of P.sub.2O.sub.5 is 24% and the operation recovery rate of P.sub.2O.sub.5 is 32%. Nonmagnetic products are high-purity phosphate concentrate products. Mixture of hydrochloric acid and phosphoric acid with a volume ratio of 2:1 was used and mixed with the magnetic products, an acid excess coefficient was controlled to be 0.8, a liquid-solid ratio L/S was controlled to be 2.5, the temperature was controlled to be 75 C., 0.2% of polyacrylamide and gelatin mixture was added and used as flocculating agent, a mass ratio of polyacrylamide to gelatin is 2:1, the leaching time is 100 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 32%, the operation recovery rate thereof is 92%, water was added until a mass ratio of water to solid substances in ore pulp was 3:10, a water glass mixture was added and used as an inhibitor, oxidized paraffin wax soap was added and used as a collector, and the flotation process including one time of roughing, one time of scavenging and three times of cleaning was performed, wherein the dose of the water glass during roughing is 2000 g/t.Math.raw ore, the dose of the collector is 200 g/t.Math.raw ore, the dose of the inhibitor and the collector during scavenging is half of the dose during roughing, the three times of cleaning are blank cleaning, and monazite concentrate with the grade of REO which is 62% can be obtained through flotation retreatment.

Embodiment 3

(5) For certain monazite and apatite paragenetic ores originated from Russia, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 2.5% and 10%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 90% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 3:5, a water glass mixture was added according to a dose of 1000 g/t.Math.raw ore and used as an inhibitor, oxidized paraffin wax soap and sodium oleate were mixed according to a mass ratio of 1:1 to obtain mixed agent which is used as a collector, and the flotation process including one time of roughing, one time of scavenging and three times of cleaning at normal temperature was performed, wherein the dose of the water glass during roughing is 1000 g/t.Math.raw ore, the dose of the collector is 200 g/t.Math.raw ore, the dose of the agent was halved during one time of scavenging, the three times of cleaning are blank cleaning, floated mixed concentrate can be obtained thereby, the content of REO therein is 6%, the operation recovery rate of REO is 88%, the content of P.sub.2O.sub.5 is 31.5% and the operation recovery rate of P.sub.2O.sub.5 is 92%. The mixed concentrate was subjected to strong-intensity magnetic separation at magnetic field intensity of 9000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 13%, the operation recovery rate of REO is 88%, the content of P.sub.2O.sub.5 is 27% and the operation recovery rate of P.sub.2O.sub.5 is 24%. Nonmagnetic products are high-purity phosphate concentrate products. Phosphoric acid was used and mixed with the magnetic products, the acid excess coefficient was controlled to be 2.0, the liquid-solid ratio L/S was controlled to be 5.0, the temperature was controlled to be 70 C., 0.2% of polyacrylamide and gelatin mixture was added and used as flocculating agent, the mass ratio of polyacrylamide to gelatin is 2:1, the leaching time is 250 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 28%, the operation recovery rate thereof is 95%, water was added until a mass ratio of water to solid substances in ore pulp is 3:10, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and sodium oleate with a mass ratio of 1:1 was added and used as a collector, and the flotation process including one time of roughing, one time of scavenging and three times of cleaning was performed, wherein the dose of the water glass during roughing is 500 g/t.Math.raw ore, the dose of the collector is 250 g/t.Math.raw ore, the dose of the inhibitor and the collector during scavenging is half of the dose during roughing, the three times of cleaning are blank cleaning, and monazite concentrate with the grade of REO which is 60% can be obtained through flotation retreatment.

Embodiment 4

(6) For certain monazite and apatite paragenetic ores originated from South Africa, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 7.25% and 10%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 80% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 1:2, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and sodium oleate with a mass ratio of 1:1 was used as a collector, and the flotation process including one time of roughing, one time of scavenging and two times of cleaning at normal temperature was performed, wherein the dose of the water glass during roughing is 1500 g/t.Math.raw ore, the dose of the collector is 500 g/t.Math.raw ore, the dose of the agent is halved during one time of scavenging, the two times of cleaning are blank cleaning, floated mixed concentrate can be obtained thereby, the content of REO therein is 16%, the operation recovery rate of REO is 96%, the content of P.sub.2O.sub.5 is 30% and the operation recovery rate of P.sub.2O.sub.5 is 93%. The mixed concentrate was subjected to high-intensity magnetic separation at magnetic field intensity of 8000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 17%, the operation recovery rate of REO is 93%, the content of P.sub.2O.sub.5 is 26% and the operation recovery rate of P.sub.2O.sub.5 is 90%. Nonmagnetic products are high-purity phosphate concentrate products. Diluted acid was used and mixed with the magnetic products, the acid excess coefficient was controlled to be 0.5, the liquid-solid ratio L/S was controlled to be 2.2, the temperature was controlled to be 120 C., 0.3% of polyacrylamide and gelatin mixture was added and used as a flocculating agent, the mass ratio of polyacrylamide to gelatin is 2:1, the leaching time is 50 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 38%, the operation recovery rate thereof is 95%, water was added until the mass ratio of water to solid substances in ore pulp is 4:10, a water glass mixture was added and used as an inhibitor, mixture of oxidized paraffin wax soap and sodium oleate with a mass ratio of 1:1 was added and used as a collector, and the flotation process including one time of roughing, one time of scavenging and two times of cleaning was performed, wherein the dose of the water glass during roughing is 1000 g/t.Math.raw ore, the dose of the collector is 200 g/t.Math.raw ore, the dose of the inhibitor and the collector during scavenging is half of the dose during roughing, the two times of cleaning are blank cleaning, monazite concentrate with the grade of REO which is 65% can be obtained through flotation retreatment, and the operation recovery rate thereof is 92%.

Embodiment 5

(7) For certain monazite and apatite paragenetic ores originated from Greece, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 1.08% and 17%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 65% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 11:20, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and oleic acid with a mass ratio of 1:1 was used as collector, and the flotation process including one time of roughing, one time of scavenging and three times of cleaning at normal temperature was performed, wherein the dose of the water glass during roughing is 500 g/t.Math.raw ore, the dose of the collector is 500 g/t.Math.raw ore, the dose of the agent was halved during one time of scavenging, the three times of cleaning are blank cleaning, the floated mixed concentrate can be obtained thereby, the content of REO therein is 10%, the operation recovery rate of REO is 95%, the content of P.sub.2O.sub.5 is 32% and the operation recovery rate of P.sub.2O.sub.5 is 93%. The mixed concentrate was subjected to high-intensity magnetic separation at magnetic field intensity of 12000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 16%, the operation recovery rate of REO is 98%, the content of P.sub.2O.sub.5 is 23% and the operation recovery rate of P.sub.2O.sub.5 is 30%. Nonmagnetic products are high-purity phosphate concentrate products. Diluted acid was used and mixed with the magnetic products, the acid excess coefficient was controlled to be 2.0, the liquid-solid ratio L/S was controlled to be 2.2, the temperature was controlled to be 20 C., 0.1% of polyacrylamide by mass percentage was added and used as a flocculating agent, the leaching time is 300 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 38%, the operation recovery rate thereof is 95%, water was added until a mass ratio of water to solid substances in ore pulp is 4:10, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and oleic acid with a mass ratio of 1:1 was added and used as collector, and the flotation process including one time of roughing, one time of scavenging and five times of cleaning was performed, wherein the dose of the water glass during roughing is 2000 g/t.Math.raw ore, the dose of the collector is 200 g/t.Math.raw ore, the dose of the inhibitor and the collector during scavenging is half of the dose during roughing, the three times of cleaning are blank cleaning, monazite concentrate with the grade of REO which is 55% can be obtained through flotation retreatment, and the operation recovery rate thereof is 95%; and then high-intensity magnetic separation was performed to the floated concentrate at magnetic field intensity of 12000 Oe, magnetic products, i.e., monazite concentrate with the grade of REO which is 59% can be obtained thereby, and the operation recovery rate thereof is 93%.

Embodiment 6

(8) For certain monazite and apatite paragenetic ores in Europe, with content of REO and P.sub.2O.sub.5 in raw ores being respectively 0.56% and 17%, 500 g of raw ores were weighed and crushed and ground to 200-mesh ore particles accounting for 75% of the total particles, water was added until a mass ratio of water to solid substances in ore pulp is 10:20, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and oleic acid with a mass ratio of 1:1 was used as a collector, and the flotation process including one time of roughing and three times of cleaning at normal temperature was performed, wherein the dose of the water glass during roughing is 500 g/t.Math.raw ore, the dose of the collector is 600 g/t.Math.raw ore, the three times of cleaning are blank cleaning, floated mixed concentrate can be obtained thereby, the content of REO therein is 8%, the operation recovery rate of REO is 93%, the content of P.sub.2O.sub.5 is 27% and the operation recovery rate of P.sub.2O.sub.5 is 95%. The mixed concentrate was subjected to high-intensity magnetic separation at magnetic field intensity of 11000 Oe, magnetic products, i.e., monazite and apatite mixed concentrate can be obtained thereby, the content of REO therein is 15%, the operation recovery rate of REO is 98%, the content of P.sub.2O.sub.5 is 20% and the operation recovery rate of P.sub.2O.sub.5 is 28%. Nonmagnetic products are high-purity phosphate concentrate products. Diluted acid was used and mixed with the magnetic products, the acid excess coefficient was controlled to be 2.0, the liquid-solid ratio L/S was controlled to be 2.0, the temperature was controlled to be 50 C., 0.2% of polyacrylamide by mass percentage was added and used as a flocculating agent, the leaching time is 200 min, finally the leaching residues were obtained, the grade of REO in the leaching residues is 35%, the operation recovery rate thereof is 92%, water was added until a mass ratio of water to solid substances in ore pulp is 6:10, a water glass mixture was added and used as an inhibitor, a mixture of oxidized paraffin wax soap and oleic acid with a mass ratio of 1:1 was added and used as a collector, and the flotation process including one time of roughing and two times of cleaning was performed, wherein the dose of the water glass during roughing is 1000 g/t.Math.raw ore, the dose of the collector is 250 g/t.Math.raw ore, the dose of the inhibitor and the collector during scavenging is half of the dose during roughing, the two times of cleaning are blank cleaning, monazite concentrate with the grade of REO which is 56% can be obtained through flotation retreatment, and the operation recovery rate thereof is 92%; and then high-intensity magnetic separation was performed to the floated concentrate at magnetic field intensity of 11000 Oe, magnetic products, i.e., monazite concentrate with the grade of REO which is 61% can be obtained thereby, and the operation recovery rate thereof is 94%.