CN102399999A - Comprehensive recovery process for rare earth and strontium intergrowth multi-metal ore - Google Patents
Comprehensive recovery process for rare earth and strontium intergrowth multi-metal ore Download PDFInfo
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Abstract
The present invention relates to a comprehensive recovery process for a rare earth and strontium intergrowth multi-metal ore. The mineral mainly comprises rare earth fluoro-carbonate and at least one selected from a sulfate of the strontium, a carbonate of the strontium or a strontium oxide. According to the present invention, at least one method selected from gravity separation, magnetic separation and flotation separation is adopted to carry out concurrent screening for the rare earth and the strontium in the rare earth and strontium intergrowth multi-metal ore to obtain the bulk concentrate containing the rare earth and the strontium; then the bulk concentrate is subjected to oxidizing roasting for 1-8 hours at a temperature of 350-700 DEG C in air atmosphere or oxygen atmosphere; the resulting calcine is subjected to leaching for 1.0-5.0 hours by a sulfuric acid solution with the hydrogen ion concentration of 0.5-12.0 mol/L, wherein the leaching temperature is 20-100 DEG C, the leaching liquid-solid ratio (by weight) is 1-5:1. The comprehensive recovery process of the present invention has the following advantages that: the rare earth is almost entirely leached in the solution; the strontium sulfate (SrSO4) is remained in the residue; the strontium concentrate with the grade of about 70% is obtained, and can be sold directly or deep processed; with the comprehensive recovery process of the present invention, the multi-metal ore containing the rare earth and the strontium can be effectively separated.
Description
Technical field
The present invention relates to altogether association polymetallic ore comprehensive recycling process of a kind of rare earth and strontium, particularly relate to a kind of hamartite with contain strontium mineral, fluorite, barium etc. altogether the total score of associated minerals from recycling.Be raw material with containing the strontium polymetallic ore specifically with rare earth; Adopt oxidizing roasting, sulfuric acid to leach and obtain the rare earth sulfuric acid salts solution; Rare earth sulfate solution carries out extracting and separating or double salt precipitation-alkali method for transformation; Reach rare earth, thorium, fluorine and all reclaim with the form of product, the leached mud staple is the strontium mineral product that exists with the Strontium Sulphate form.
Background technology
Rare earth is the advantage mineral of China, also is a kind of strategic materials.China's rare earth reserves account for the world more than 80%.Adopt, develop through surveying in decades, China has formed three big Rare Earth Production base, i.e. packet header, the Inner Mongol, Ganzhou, the Liangshan Mountain, Sichuan.On the side hilltop, continent township, Dechang County, the Liangshan Mountain, found large stretch of rare-earth mineral primary outcrop.Continent township rare earth mineral deposit belongs to the hamartite rare earth mineral deposit.The technological property of ore and the contrast of mineral deposit, Mianning yak level ground have own characteristic:. the hamartite natural particle size is little, and generally below 0.2mm ,-200 orders account for 30～40%; Hamartite with contain strontium mineral, calcite etc. each other intergrowth, to wrap up phenomenon each other common; Gangue mineral contains strontium mineral and other rich strontium mineral is obviously higher, and dust shape ore significantly increases; Its dust is formed very complicated; Rare earth ore concentrate contains ThO
2Be 0.10～0.16wt%.
The Dechang rare-earth mineral is to contain in the polymetallic ore of strontium, barium, and the occurrence status of rare earth also has very big difference with the Mianning rare-earth mineral.If adopt the identical technique of preparing (method) of maoniuping rare-earth mineral of single hamartite, will produce two big serious consequences: the one, sorting index will be seriously on the low side, and concentrate grade is low, and rare earth yield is low, and valuable rare earth resources will be fully utilized; The 2nd, contain strontium mineral and abandon it as mine tailing, with contaminate environment, tie up the farmland, influence the eubiosis.
In existing manufacturing technique, people consider usually hamartite with contain the strontium mineral mineral intergrowth and be used as single hamartite and carry out ore dressing and separate, the rare earth ore concentrate grade is low, is merely about 50% the concentrate taste low 10～20% of producing than single hamartite; The recovery of rare earth is low, is merely about 60%, than the recovery low 20～30% of single hamartite.In addition, the recovery that contains strontium mineral is on the low side, less than 55%.In recent years, hamartite and contain strontium mineral altogether aspect the comprehensive utilization of associated minerals gradually cause concern.
The separating technology of mineral such as collective concentrate middle-weight rare earths and strontium, still unmanned at present research.
Chinese patent 20071017771.3 discloses the comprehensive utilization process of a kind of hamartite and celestite paragenic; This process using hydroximic acid or hydroxyl oximate be that collective concentrate is produced in the synchronous flotation of trapping agent, adopted oxidizing roasting-salt acid leaching process to obtain mixed chlorinated rare earth solution and lazurite again.This method is in oxidizing roasting-hydrochloric acid leaching process; The part rare earth will reclaim with the chloride soln form, can directly be connected rare earth extraction and separate, but some rare earth get in the leached mud with fluorine cpd or oxyfluoride form and lazurite jointly; And when if strontium exists with Strontium carbonate powder or strontium oxide form in the ore; Strontium will form strontium chloride and get in the leach liquor, cause strontium to be dispersed in leach liquor and the slag, and difficult and Rare Earth Separation reclaims.
Summary of the invention
The purpose of this invention is to provide a kind of rare earth and strontium association polymetallic ore comprehensive recycling process altogether; This technical process is simple, effectively rare-earth separating and strontium mineral, the leaching yield of rare earth >=95%; Contain the strontium mineral amount in the leached mud and be able to enrichment, its grade can reach more than 70% through this method.
For reaching the foregoing invention purpose, the present invention adopts following technical scheme:
The present invention is according to hamartite thing and the greatest differences that contains the solubility property of strontium mineral thermal decomposition product in sulfuric acid medium; Carrying out oxidizing roasting-sulfuric acid leaches; REE is able to efficient leaching; Get in the sulphuric leachate jointly with fluorine, Th, and strontium mineral gets in the leached mud with the Strontium Sulphate state of low solubility, thereby realize rare earth and contain the effective of strontium mineral and separate.
Technology is reclaimed in the comprehensive utilization of polymetallic ores such as this rare earth and strontium, barium, calcium, and the concrete steps of its Separation and Recovery are:
1) adopts at least a method in gravity treatment, magnetic separation and the flotation that rare earth and strontium in rare earth and the common association polymetallic ore of strontium are selected altogether, obtain containing the collective concentrate of rare earth and strontium;
The collective concentrate that 2) will contain rare earth and strontium carries out oxidizing roasting;
3) calcining after the roasting leaches with sulphuric acid soln, filters, and obtains containing the sulphuric leachate of quadrivalent cerium, fluorine and trivalent rare earth and the leached mud of sulfur acid strontium.
Rare earth oxide content in the collective concentrate that the process ore dressing obtains is 10%-50wt%, and strontium oxide content is 20-50wt%.
The sulphuric leachate that contains quadrivalent cerium, fluorine and trivalent rare earth uses the synergic reagent based on P507 or P204 to carry out extracting and separating, obtains single or mixed rare earth compound, thorium product, fluorine product.See patent: " method of a kind of hamartite oxidizing roasting-sulfuric acid leaching-extraction back organic phase defluorination (patent No.: 200410070199.1 ", the present invention does not explain this part.
Wherein ratio is in the strontium in rare earth in the step 1) and strontium, barium, the common associated minerals of calcium and other the non-rare-earth mineral: the strontium composition/greater than 70wt%, the strontium composition calculates according to Strontium Sulphate (strontium composition+non-rare-earth mineral composition).Oxidizing roasting temperature in the step 1) is 350～700 ℃, and roasting 1～8 hour obtains calcining.
Step 2) sulfuric acid leaches operation in, and using the Sorensen value of sulphuric acid soln is 0.5～12.0mol/L, liquid-solid ratio 1～5: 1, and extraction temperature is 20-100 ℃, the leaching mode can be step leaching, multistep leaches or adverse current leaches.The rare earth leaching velocity increases and increases along with the stirring velocity that leaches usually, but is not unlimited increase, generally is controlled at 100-600rpm.The leaching yield of rare earth prolongs and increases along with extraction time, reaches stationary value subsequently, generally is controlled at 0.5-5.0h.Content of rare earth wherein is in rare earth oxide REO.
The leaching yield of concentrate middle-weight rare earths >=95% among the present invention contains grade >=70% of strontium mineral in the leached mud.
Leach liquor is the rare earth sulfate solution that contains high price cerium, fluorine, thorium and iron; This treatment process that contains the rare earth sulfate solution of quadrivalent cerium, trivalent rare earth, fluorine, thorium has multiple; Can adopt the double salt precipitation of early development---the alkali method for transformation is handled; But the emission problem that has fluoride waste, thoriated slag, the rare earth yield is on the low side simultaneously.
Leach liquor is that the rare earth sulfate solution that contains high price cerium, fluorine, thorium and iron also can adopt the Sichuan hamartite process for cleanly preparing of Beijing Non-Ferrous Metal Research General Academy's exploitation to adopt the method for extracting and separating to handle, and this technology comprises following core patent:
■ 95103694.7, a kind of from fluorine-containing rare earth sulfate solution the technology of extracting and separating cerium
■ 200410070199.1, the method for a kind of hamartite oxidizing roasting-sulfuric acid leaching-extraction back organic phase defluorination
The process method of ■ extraction separation of quadravalence cerium, thorium and few cerium trivalent rare earth from rare earth sulfate solution, 200710098733.3
The process method of ■ extraction separation of quadravalence cerium, thorium, fluorine and few cerium trivalent rare earth from rare earth sulfate solution, 200710098732.9
In addition, this rare earth sulfate solution that contains quadrivalent cerium, trivalent rare earth, fluorine, thorium also can adopt the Changchun modest extraction and separation technology of being developed of the Li De of applied chemistry institute to handle.
Adopt the advantage of extraction separating method to be to this rare earth sulfate solution that contains quadrivalent cerium, trivalent rare earth, fluorine, thorium: can improve the cerium product gas purity preferably; And obtain trivalent rare earth solution; Guarantee the recovery of fluorine, thorium, thereby realize the purpose of cleaner production and comprehensive utilization of resources.
This technological advantage:
(1) this technical process is simple, effectively rare-earth separating and strontium mineral, and the leaching yield of rare earth >=95% contains the strontium mineral amount and is able to enrichment in the leached mud, and its grade can reach more than 70% through this method.
(2) adopt medium and low temperature oxidizing roasting, no poisonous fume produces, and atmosphere pollution to not corrosion of roasting apparatus, does not adopt common kiln, like rotary kiln, just can reach good roasting effect, and equipment is simple, less investment, is convenient to operation.
(3) adopt sulfuric acid to leach to the oxidizing roasting ore deposit, production cost is lower, and can rare earth, thorium, fluorine all be changed in the solution, is easy to and has now or be connected each other at the process for cleanly preparing of developing, and the resource overall utilization rate is high.
(4) adopt sulfuric acid to leach, rare earth gets into the liquid phase infusion solution, and strontium gets into the solid phase leached mud, and earth solution is with to contain the strontium slag promptly separable through simple filtration.
Description of drawings
Fig. 1: process flow sheet of the present invention
Will be through the collective concentrate of ore dressing, through oxidizing roasting, the calcining after the roasting leaches with sulphuric acid soln, filters, and obtains re dip solution and celestite concentrate, adds extraction agent in the rare earth liquid, through extraction and back extraction, obtains rare-earth products.
Embodiment
Embodiment 1:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 434.5g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:10.0wt%; SrO:35.6wt%), obtain calcining 92.1g, use the 150ml Sorensen value to leach 3h at 50 ℃ as the 2.0mol/L sulphuric acid soln at 550 ℃ of following roasting 2.0h; Can get slag 70.0g, slag is the grade (SrSO of celestite ore
4%) 84.6%.The recovery 94.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 96.2%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 2:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 438.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:20.2wt%; SrO:20.0wt%), obtain calcining 86.1g, use the 300ml Sorensen value to leach 3h at 50 ℃ as the 2.0mol/L sulphuric acid soln at 550 ℃ of following roasting 2.0h; Can get slag 39.4g, slag is the grade (SrSO of celestite ore
4%) 85.5%.The recovery 95.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 95.1%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 3:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 435.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:16.7wt%; SrO:25.4wt%), obtain calcining 88.2g, use the 440.0ml Sorensen value to leach 2h at 45 ℃ as the 1.0mol/L sulphuric acid soln at 680 ℃ of following roasting 1.0h; Can get slag 50.0g, slag is the grade (SrSO of celestite ore
4%) 85.5%.The recovery 95.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 98.0%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 4:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 430.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:15.0wt%; SrO:28.0wt%), obtain calcining 89.1g, use the 440.0ml Sorensen value to leach 4h at 80 ℃ as the 1.0mol/L sulphuric acid soln at 375 ℃ of following roasting 8.0h; Can get slag 55.0g, slag is the grade (SrSO of celestite ore
4%) 81.0%.The recovery 90.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 50.0%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 5:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 437.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:15.3wt%; SrO:27.5wt%), obtain calcining 88.9g, use the 100.0ml Sorensen value to leach 2h at 30 ℃ as the 12.0mol/L sulphuric acid soln at 500 ℃ of following roasting 2.0h; Can get slag 54.0g, slag is the grade (SrSO of celestite ore
4%) 87.3%.The recovery 97.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 98.1%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 6:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 436.5g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:15.5wt%; SrO:27.2wt%), obtain calcining 88.8g, use the 100.0ml Sorensen value to leach 3h at 40 ℃ as the 8.0mol/L sulphuric acid soln at 500 ℃ of following roasting 2.0h; Can get slag 53.5g, slag is the grade (SrSO of celestite ore
4%) 85.5%.The recovery 95.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 97.2%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 8:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 434.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:15.2wt%; SrO:27.7wt%), obtain calcining 89.0g, use the 100.0ml Sorensen value to leach 5h at 60 ℃ as the 3.0mol/L sulphuric acid soln at 500 ℃ of following roasting 5.0h; Can get slag 54.5g, slag is the grade (SrSO of celestite ore
4%) 85.5%.The recovery 95.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 97.0%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Embodiment 9:
Take by weighing the raw ore of 2000.0g, but through flotation, gravity treatment output rare earth and strontium mixing ore deposit 436.0g.Take by weighing 100.0g rare earth and strontium mixing ore deposit (REO:15.3wt%; SrO:27.6wt%), obtain calcining 89.1g, use the 100.0ml Sorensen value to leach 2h at 50 ℃ as the 2.0mol/L sulphuric acid soln at 500 ℃ of following roasting 4.0h; Can get slag 54.2g, slag is the grade (SrSO of celestite ore
4%) 87.3%.The recovery 97.0% of strontium.Leach liquor is the mixing rare earth sulfate solution, rare earth leaching yield 97.0%, and the mixing rare earth sulfate solution carries out extracting and separating and can obtain single rare-earth products.
Claims (10)
1. rare earth and strontium association polymetallic ore comprehensive recycling process altogether, said polymetallic ore fine size, the mutual embedding cloth of the mineral of rare earth and strontium is difficult to sort together, it is characterized in that it comprises following step:
1) adopts at least a method in gravity treatment, magnetic separation and the flotation that rare earth and strontium in rare earth and the common association polymetallic ore of strontium are selected altogether, obtain containing the collective concentrate of rare earth and strontium;
The collective concentrate that 2) will contain rare earth and strontium carries out oxidizing roasting;
3) calcining after the roasting leaches with sulphuric acid soln, filters, and obtains containing the sulphuric leachate of quadrivalent cerium, fluorine and trivalent rare earth and the leached mud of sulfur acid strontium.
2. a kind of rare earth according to claim 1 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that the rare earth in the said polymetallic ore mainly exists with the fluoro carbonate form.
3. a kind of rare earth according to claim 1 and 2 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that, the strontium mineral in the said polymetallic ore is at least a in strontianite, lazurite or the oxide compound.
4. a kind of rare earth according to claim 1 and 2 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that, the rare earth oxide content in the collective concentrate that the process ore dressing obtains is 10%-50wt%, and strontium oxide content is 20-50wt%.
5. according to claim 1 or 2 or 4 described a kind of rare earths and strontium association polymetallic ore comprehensive recycling process altogether, it is characterized in that step 2) in oxidizing roasting atmosphere be air or oxygen, temperature is 350～700 ℃, roasting time 1～8 hour.
6. according to claim 1 or 5 described a kind of rare earths and the common association polymetallic ore comprehensive recycling process of strontium, it is characterized in that sulfuric acid leaches operation in the step 3), the Sorensen value of sulphuric acid soln is 0.5～12.0mol/L, and leaching liquid-solid ratio is 1～5: 1.
7. according to claim 1 or 6 described a kind of rare earths and the common association polymetallic ore comprehensive recycling process of strontium, it is characterized in that sulfuric acid leaches operation in the step 3), extraction temperature is 20～100 ℃.
8. a kind of rare earth according to claim 1 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that, sulfuric acid described in the step 3) leaches and comprises that step leaching, multistep leach or adverse current leaches mode.
9. a kind of rare earth according to claim 1 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that sulphuric leachate directly carries out extracting and separating, obtains various rare earth compounds, thorium and fluorine product.
10. a kind of rare earth according to claim 1 and strontium be association polymetallic ore comprehensive recycling process altogether, it is characterized in that, the leached mud of the sulfur acid strontium that obtains in the step 3) dries or heat drying through nature, obtains strontium concentrate product, the recovery of strontium >=90%.
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