CN1173050C - Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid - Google Patents
Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid Download PDFInfo
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- CN1173050C CN1173050C CNB021444056A CN02144405A CN1173050C CN 1173050 C CN1173050 C CN 1173050C CN B021444056 A CNB021444056 A CN B021444056A CN 02144405 A CN02144405 A CN 02144405A CN 1173050 C CN1173050 C CN 1173050C
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- rare earth
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract
The present invention relates to a low-temperature roasting and decomposing process of a rare earth concentrate by using concentrated sucfuric acid. The concentrate and the concentrated sulfuric acid are roasted after being mixed according to the weight ratio of (1:1.1) to (1:1.7), the roasting temperature is 150 to 330 DEG C (the optimum temperature is 180 to 220 DEG C), and the roasted concentrate is leached by water, and filtered so as to obtain water-leach liquor and water-leach slag; in the water-leach liquor the leaching rate of rare earth is 95 to 98%, and the leaching rate of thorium is more than 95%; the water-leach slag contain less than 3% of rare earth and less than 3% of thorium, the total specific radioactivity of the rare earth and the thorium is less than or equal to 7.4*10<4>Bq/Kg, and the rare earth and the thorium contain small quantity of slag; thorium is extracted from the water-leach liquor so as to obtain a thorium product and a rare earth product, and the rare earth product does not contain radioactive ThO2 and REO (the ratio of ThO2/ REO is less than or equal to 1*10<-5>).
Description
One, technical field:
The present invention relates to a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique.
Two, background technology:
At present, the main method of handling rare earth ore concentrate both at home and abroad is a vitriol oil high-temperature roasting method, and this method had obtained using widely in recent years.Though use this method can obtain certain economic benefits, " three wastes " problem that produces in vitriol oil high-temperature calcination process is difficult to solve.(1) waste residue: in vitriol oil high-temperature calcination process, the radioelement thorium mainly concentrates in the waste residue, belong to high slagging, this waste residue is difficult to dissolving and reclaims, many producers can only be stacked in the slag storehouse, cause the serious environmental pollution problem, the expense that is stored in the slag storehouse because of waste residue simultaneously is 0.25 yuan/kilogram, and this increases the burden of rare earth factory more.(2) waste gas: in vitriol oil high-temperature calcination process, produce a large amount of sulfur-bearings, fluorine, strongly-acid waste gas, contain obnoxious flavoures such as hydrogen fluoride, sulfurous gas, sulphur trioxide in this waste gas, atmosphere is caused serious pollution.(3) waste water: in vitriol oil high-temperature calcination process, near the serious salinization in farmland making after the non-rare earth impurity discharging in the waste water, serious environment pollution.Except that above " three wastes " problem was difficult to solve, vitriol oil high-temperature roasting method also existed the problem that energy consumption is big, expense is high.Because above problems are not resolved, and cause some rare earth factories to shut down, stop, merge and change, and become the key issue that influences the Sustainable development of northern China rare earth.
Three, technology contents:
The objective of the invention is to exist waste residue, waste gas, waste water serious environment pollution at rare earth ore concentrate vitriol oil high-temperature roasting method, and insoluble problems such as energy consumption is big, provide a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, utilize this technology can reach (1) and make the thorium content in the waste residue drop to discharging standards, can build the dam discharging; (2) quantity discharged in the waste gas significantly reduces, and is convenient to recycling; (3) the detrimental impurity amount drops to minimumly in the waste water, does not cause environmental pollution.Adopt low-temperature bake technology, energy consumption cost also reduces greatly.For rare earth factory saves overspending.The present invention also aims to: rare earth ore concentrate is behind vitriol oil low-temperature bake, contain radioactive roasted ore after leaching dissolving, adopt extraction process that the radioelement thorium is focused on, both helped radioactive protection, can turn waste into wealth again, thorium be made the important source material product of nuclear industry.Other non-rare earth impurities also adopt corresponding technology to reclaim and produce corresponding product sale.
Rare earth ore concentrate vitriol oil low-temperature decomposition technology of the present invention, it is characterized in that rare earth ore concentrate and the vitriol oil by weight 1: 1.1-1: 1.7 mixed evenly forms sulfuric acid and mixes the ore deposit, and put into the retort furnace roasting, its maturing temperature is 150-330 ℃, its maturing temperature is 180-220 ℃, forms roasted ore after roasting; Roasted ore is gone out, filters through water logging, obtain the infusion and the water logging slag of roasted ore, adopt extraction process to extract the thorium in the infusion, get rare-earth products after the separation.
Effect of the present invention is: rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, solved former high-temperature roasting technology indeterminable " three wastes " problem, and have following significant effect:
(1) the waste residue amount is reduced to half of former technology, its thorium content＜3%; Radioactivity always than put≤7.4 * 10
4Bq/Kg reaches the low slagging emission standard of country, can build the dam discharging, has saved waste residue is deposited in a large sum of expense in the slag storehouse.
(2) in the low-temperature bake process, decomposition reaction does not take place in sulfuric acid, and the tolerance of generation seldom is convenient to recycle with spraying process.
(3) in the low-temperature bake process, the roasted ore infusion, rare earth leaching yield 95-98%, thorium leaching yield＞95%, the thorium in the infusion can be used the extraction process extraction separation, produces the thorium product and recycles.Do not contain radioactivity (ThO in the rare-earth products that obtains simultaneously
2/ REO≤1 * 10
-5), there is not problem of environment pollution caused.
Four, embodiment:
Key problem in technology of the present invention is the preparation of roasted ore, and the weight ratio of promptly controlling the rare earth ore concentrate and the vitriol oil is 1: 1.1-1: within 1.7 the scope, and the control maturing temperature is between 150-330 ℃; All continue to use maturation process of the prior art from roasted ore to the extracting and separating that makes rare-earth products and thorium, so among the present invention this part technology is not described in detail.In fact, the roasted ore that makes by technology of the present invention goes out, filters through water logging, and the leaching yield of gained infusion middle-weight rare earths (in REO) is 95-98%, and thorium is (with ThO
2Meter) leaching yield is＞95%, and the water logging quantity of slag is half of the former high-temperature roasting quantity of slag that technology produces, water logging slag middle-weight rare earths＜3%, ThO
2＜3%, its radioactivity always than put≤7.4 * 10
4Bq/Kg has reached national low slagging emission standard.
Provide embodiments of the invention below:
Embodiment 1:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at 150 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore, filter then, obtain the infusion and the water logging slag of roasted ore.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 2:
(1) with a certain amount of rare earth ore concentrate (REO 〉=40%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at about 200 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 3:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at 330 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 4:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, slowly adds to carry out roasting in the rotary kiln, and maturing temperature is controlled at 240-280 ℃.After after a while, effusive from the kiln tail both had been roasted ore.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Claims (2)
1, a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, it is characterized in that rare earth ore concentrate and the vitriol oil by weight 1: 1.1-1: 1.7 mixed evenly forms sulfuric acid and mixes the ore deposit, and put into the retort furnace roasting, its maturing temperature is 150-330 ℃, forms roasted ore after roasting; Roasted ore is gone out, filters through water logging, obtain the infusion and the water logging slag of roasted ore, adopt extraction process to extract the thorium in the infusion, get rare-earth products after the separation.
2, roasting decomposition technique according to claim 1 is characterized in that maturing temperature is 180-220 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021444056A CN1173050C (en) | 2002-09-25 | 2002-09-25 | Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid |
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| CNB021444056A CN1173050C (en) | 2002-09-25 | 2002-09-25 | Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid |
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| CN1405337A CN1405337A (en) | 2003-03-26 |
| CN1173050C true CN1173050C (en) | 2004-10-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
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2002
- 2002-09-25 CN CNB021444056A patent/CN1173050C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
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| CN1405337A (en) | 2003-03-26 |
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