CN102277483B - Method for preparing rare earth chloride by using Baiyunebo rare earth concentrate - Google Patents
Method for preparing rare earth chloride by using Baiyunebo rare earth concentrate Download PDFInfo
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Abstract
The invention relates to a new method for preparing rare earth chloride by using Baiyunebo rare earth concentrate and belongs to the field of wet-process metallurgy. The invention comprises the following steps: performing thermal decomposition, wherein a raw material used is Baiyunebo mixed rare earth concentrate with a grade of 60 to 80 percent; leaching in hydrochloric acid, namely leaching ore obtained after thermal decomposition in hydrochloric acid; performing alkaline decomposition, namely decomposing filter residue obtained after leaching in hydrochloric acid with solution of sodium hydroxide; washing, namely washing the ores obtained after alkaline decomposition with water till the pH value is 7 to 9, and recovering fluorine and phosphorus from washing solution; performing primary neutralization, namely mixing hydrochloric acid leachate and water washing residue, and neutralizing till the pH value is 0.5 to 2.5; and performing secondary neutralization, namely neutralizing the filtrate obtained by the primary neutralization till the pH value is 4 to 5, wherein the filtrate of the secondary neutralization is solution of rare earth chloride. The method has the advantages of facilitating recovery of other elements, avoiding waste gas, waste water and waste residue, along with small alkali consumption, stable process and high rare earth recovery rate of more than or equal to 95 percent.
Description
Technical field
The present invention relates to the novel method that a kind of Bayan Obo rare earth ore concentrate prepares rare earth chloride, belong to the hydrometallurgy field.
Background technology
Baiyuneboite is the maximum and even maximum in the world rare-earth mineral of China so far, and this rare-earth mineral mainly is that the form with hamartite and urdite mixings ore deposit exists, and belongs to typical difficult choosing, difficulty smelting mineral.In industrial production, this mineral mainly contain two kinds of smelting technologyes: concentrated sulfuric acid roasting technology and sodium hydroxide decomposition technique.Concentrated sulfuric acid roasting technology is that what to handle baiyuneboite also is the most sophisticated smelting technology the earliest, and this technology biggest advantage is strong to the flexibility of mineral, but also exists a lot of serious defectives; Though in secular application process; These defectives have been done some improved, but because the limitation of technology itself, this technology still exists following distinct issues; As: the three-waste pollution problem is difficult to solve always, and a lot of useful elements run off with the form of refuse in vain; The radioelement thorium exists with the form of thorium pyrophosphate, is difficult to further handle, and can only transfer to environmental administration and deposit specially, and need pay high expense.More and more stronger along with to environmental protection consciousness and dynamics, and the enforcement of new environmental regulation, this technology has the danger of comprehensively abrogating probably.
In recent years, Baotou rare earth enterprise also fully recognized the deficiency of concentrated sulfuric acid roasting technology when rare-earth smelting, had researched and developed the sodium hydroxide decomposition technique for this reason; But this technology alkali consumption is big, production cost is high, and this technology is because the baiyuneboite rare earth grade that adopts is not high in addition, and foreign matter content is big; Make this technology be difficult to stable smooth operation always, in addition, in the rare-earth smelting process because the influence of detrimental impurity calcium; Cause rare earth yield low, cause serious economy loss.
Summary of the invention
The object of the present invention is to provide a kind of novel method for preparing rare earth chloride from the Bayan Obo rare earth ore concentrate; This technology can solve the three-waste pollution problem in the rare-earth smelting process effectively; Rare earth yield is high, and can realize the comprehensive reutilization of other useful element.
The object of the invention is realized by following process step.
(1) thermolysis: be that 60～68% Bayan Obo rare earth ore concentrate carries out thermolysis at first with grade, 400～600 ℃ of temperature, the time is 0.5～2 hour;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 6～12mol/L, the consumption of hydrochloric acid: REO quality in the Bayan Obo rare earth ore concentrate: concentrated hydrochloric acid quality=1: 1.2～2.4 baiyuneboite after the thermolysis; Extraction temperature is 60～95 ℃, and 0.5～2 hour time is in the leaching process; Add the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.05～0.3, after hydrochloric acid leaches; Filter, get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that hydrochloric acid leached mud liquid is carried out alkali and decompose; Sodium hydroxide concentration is 56～75% solution; Consumption is: REO quality in the Bayan Obo rare earth ore concentrate: sodium hydroxide quality=1: 0.8～1.5; Temperature was controlled at 150～230 ℃, 0.5～1.5 hour time when alkali decomposed;
(4) washing: alkali is decomposed mineral wash, washing temperature is 18～95 ℃, and washing to pH is to filter in 7～9 o'clock, water lotion and washing slag;
(5) in 1: will wash slag and join in the hydrochloric acid leachate, temperature is 18～95 ℃, mix and stir, to pH be 0.5～2.5 o'clock, filter, in slag 1 and neutralizer 1;
(6) in 2: in neutralizer 1, add alkaline matter, stir, temperature is controlled at 18～95 ℃; Filter pH to 4～5 of adjustment neutralizer 1, in slag 2 and neutralizer 2; Neutralizer 2 is final re chloride, in can be used as the raw material of carrying thorium with slag 2, or solid envelope is preserved.
Described Bayan Obo rare earth ore concentrate is the hamartite of REO grade between 60～68% and the mixed rare earth concentrate of solitary stone ore.
Described chlorine suppressor factor is thiocarbamide, H
2O
2, a kind of in the sodium sulphite, barium sulphide.
Described alkaline matter is the solution of the oxyhydroxide of ammoniacal liquor or alkali-metal oxyhydroxide or earth alkali metal.
Described water lotion is the mixing solutions of Sodium Fluoride, sodium phosphate, sodium hydroxide, can be used for reclaiming Sodium Fluoride, sodium phosphate, and the raw material when unnecessary sodium hydroxide can be used as the alkali decomposition adds.
Can return with slag 1 in described and join next time in the alkali decomposition step.
The present invention is at first from the baiyuneboite raw material; Researched and developed a kind of new baiyuneboite ore-dressing technique, we have obtained the Bayan Obo rare earth ore concentrate of higher-grade, high-recovery to use this technology, and the present invention is raw material with the baiyuneboite rare earth ore concentrate of this higher-grade, high-recovery just; Invented a kind of novel process of new production rare earth chloride; This technology three-waste free pollution, rare earth yield is high, process stabilizing; And can realize the recycling of other useful element, for the improvement of the smelting technology of baiyuneboite provides new direction.
Advantage of the present invention is:
1, the present invention is not have poisonous, severe corrosive gas generation with respect to the advantage of concentrated sulfuric acid roasting technology; Can not produce a large amount of ammonia nitrogen waste waters; The major impurity element can effectively be recycled, and becomes Industrial products, the cost when reducing rare-earth smelting; The quantity of slag of radioelement thorium is little, is easy to preserve and recycles once more.
2, the present invention is that alkali consumption is few with respect to the advantage of sodium hydroxide decomposition technique; Rare earth yield is high; In addition, raw material of the present invention is the Bayan Obo rare earth ore concentrate of higher-grade, high-recovery, owing to adopted the principle of fine fodder; Production efficiency is high, the unit's of greatly reducing rare earth chloride production cost of products.
4, the present invention not only is suitable for to be master's baiyuneboite, also to be suitable for other mishmetal mineral that other is the master with the hamartite with hamartite and solitary stone ore.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Through specific embodiment technical scheme of the present invention is described in detail below, but content of the present invention not only is confined to following embodiment.
Embodiment 1
(1) thermolysis: get the 1.5kg grade and be 60.2% baiyuneboite and carry out thermolysis, 420 ℃ of pyrolysated temperature, the time is 1.5 hours;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 7mol/L, the consumption of hydrochloric acid: REO quality in the baiyuneboite: concentrated hydrochloric acid quality=1: 2.2 baiyuneboite after the thermolysis; Extraction temperature is 75 ℃; 1.5 hours time, add thiocarbamide in the leaching process as the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.06; Thermolysis mineral to after the hydrochloric acid leaching filter, and get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; When alkali decomposes sodium hydroxide being mixed with mass concentration is 75% solution; The consumption of sodium hydroxide is: REO quality in the baiyuneboite: sodium hydroxide quality=1: 0.8; The alkali decomposition temperature is 220 ℃, 0.5 hour time;
(4) washing: adopt the general industry water that alkali is decomposed mineral and washes, the temperature of water lotion is 75 ℃, and washing to the pH of water lotion is to filter in 7.5 o'clock;
(5) in 1: the washing slag that will obtain in the time of will wash joins in the hydrochloric acid leachate, and temperature is 55 ℃, mix and stir, be 2 o'clock until PH, filtration;
(6) in 2: in neutralizer 1, add mass concentration slowly and be 14% ammonia soln, stir, temperature is controlled at 55 ℃; Be adjusted to PH to 4.5 after-filtration of neutralizer 1, neutralizer 2 with in slag 2, neutralizer 2 is final re chloride; Through measuring this re chloride volume is 4100ml; The content of REO is 209.89g/L, and the total recovery of rare earth is 95.3%, and the content of thorium is less than 0.01%.
Embodiment 2
(1) thermolysis: get the 1.5kg grade and be 65.36% baiyuneboite and carry out thermolysis, 490 ℃ of pyrolysated temperature, the time is 1.0 hours;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach the baiyuneboite after the thermolysis, and concentration of hydrochloric acid 10mol/L, the consumption of hydrochloric acid: REO quality in the baiyuneboite: concentrated hydrochloric acid quality=1: 1.7, extraction temperature are 75 ℃, 1.5 hours time, add H in the leaching process
2O
2As the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.3, the thermolysis mineral after the hydrochloric acid leaching are filtered, get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; When alkali decomposes sodium hydroxide being mixed with mass concentration is 70% solution; The consumption of sodium hydroxide is: REO quality in the baiyuneboite: sodium hydroxide quality=1: 1.0; The alkali decomposition temperature is 200 ℃, 0.8 hour time;
(4) washing: adopt the general industry water that alkali is decomposed mineral and washes, the temperature of water lotion is 35 ℃, and washing to the pH of water lotion is to filter in 7.9 o'clock;
(5) in 1: the washing slag that will obtain in the time of will wash joins in the hydrochloric acid leachate, and temperature is 25 ℃, mix and stir, be 2.5 o'clock until PH, filtration;
(6) in 2: in neutralizer 1, add mass concentration slowly and be 5% sodium hydroxide solution, stir, temperature is controlled at 60 ℃; Be adjusted to PH to 4.2 after-filtration of neutralizer 1, neutralizer 2 with in slag 2, neutralizer 2 is final re chloride; Through measuring this re chloride volume is 4200ml; The content of REO is 224.79g/L, and the total recovery of rare earth is 96.3%, and the content of thorium is less than 0.01%.
Embodiment 3
(1) thermolysis: get the 1.5kg grade and be 67.65% baiyuneboite and carry out thermolysis, pyrolysated temperature 5500, the time is 0.5 hour;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 6mol/L, the consumption of hydrochloric acid: REO quality in the baiyuneboite: concentrated hydrochloric acid quality=1: 1.6 baiyuneboite after the thermolysis; Extraction temperature is 95 ℃; 1.0 hours time, add sodium sulphite in the leaching process as the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.07; Thermolysis mineral to after the hydrochloric acid leaching filter, and get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; When alkali decomposes sodium hydroxide being mixed with mass concentration is 70% solution; The consumption of sodium hydroxide is: REO quality in the baiyuneboite: sodium hydroxide quality=1: 1.5; The alkali decomposition temperature is 200 ℃, 1.0 hours time;
(4) washing: adopt the general industry water that alkali is decomposed mineral and washes, the temperature of water lotion is 95 ℃, and washing to the pH of water lotion is to filter in 7.2 o'clock;
(5) in 1: the washing slag that will obtain in the time of will wash joins in the hydrochloric acid leachate, and temperature is 85 ℃, mix and stir, be 1.6 o'clock until PH, filtration;
(6) in 2: in neutralizer 1, add mass concentration slowly and be 10% potassium hydroxide solution, stir, temperature is controlled at 75 ℃; Be adjusted to PH to 4.0 after-filtration of neutralizer 1, neutralizer 2 with in slag 2, neutralizer 2 is final re chloride; Through measuring this re chloride volume is 4400ml; The content of REO is 224.17g/L, and the total recovery of rare earth is 97.2%, and the content of thorium is less than 0.01%.
Embodiment 4
(1) thermolysis: get the 1.5kg grade and be 64.88% baiyuneboite and carry out thermolysis, 590 ℃ of pyrolysated temperature, the time is 0.5 hour;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 12mol/L, the consumption of hydrochloric acid: REO quality in the baiyuneboite: concentrated hydrochloric acid quality=1: 2.3 baiyuneboite after the thermolysis; Extraction temperature is 45 ℃; 1.4 hours time, add barium sulphide in the leaching process as the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.16; Thermolysis mineral to after the hydrochloric acid leaching filter, and get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; When alkali decomposes sodium hydroxide being mixed with mass concentration is 57% solution; The consumption of sodium hydroxide is: REO quality in the baiyuneboite: sodium hydroxide quality=1: 1.4; The alkali decomposition temperature is 230 ℃, 1.2 hours time;
(4) washing: adopt the general industry water that alkali is decomposed mineral and washes, the temperature of water lotion is 70 ℃, and washing to the pH of water lotion is to filter in 8.5 o'clock;
(5) in 1: the washing slag that will obtain in the time of will wash joins in the hydrochloric acid leachate, and temperature is 20 ℃, mix and stir, be 2 o'clock until PH, filtration;
(6) in 2: in neutralizer 1, add mass concentration slowly and be 20% ammonia soln, stir, temperature is controlled at 65 ℃; Be adjusted to PH to 4.4 after-filtration of neutralizer 1, neutralizer 2 with in slag 2, neutralizer 2 is final re chloride; Through measuring this re chloride volume is 4100ml; The content of REO is 225.73g/L, and the total recovery of rare earth is 95.1%, and the content of thorium is less than 0.01%.
Embodiment 5
(1) thermolysis: get the 1.5kg grade and be 63.54% baiyuneboite and carry out thermolysis, 500 ℃ of pyrolysated temperature, the time is 1.0 hours;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 12mol/L, the consumption of hydrochloric acid: REO quality in the baiyuneboite: concentrated hydrochloric acid quality=1: 2.0 baiyuneboite after the thermolysis; Extraction temperature is 78 ℃; 1.4 hours time, add thiocarbamide in the leaching process as the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.065; Thermolysis mineral to after the hydrochloric acid leaching filter, and get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; When alkali decomposes sodium hydroxide being mixed with mass concentration is 70% solution; The consumption of sodium hydroxide is: REO quality in the baiyuneboite: sodium hydroxide quality=1: 0.9; The alkali decomposition temperature is 200 ℃, 1.5 hours time;
(4) washing: adopt the general industry water that alkali is decomposed mineral and washes, the temperature of water lotion is 75 ℃, and washing to the pH of water lotion is to filter in 7.9 o'clock;
(5) in 1: the washing slag that will obtain in the time of will wash joins in the hydrochloric acid leachate, and temperature is 85 ℃, mix and stir, be 2.2 o'clock until PH, filtration;
(6) in 2: in neutralizer 1, add mass concentration slowly and be 40% sodium hydroxide solution, stir, temperature is controlled at 18 ℃; Be adjusted to PH to 4.0 after-filtration of neutralizer 1, neutralizer 2 with in slag 2, neutralizer 2 is final re chloride; Through measuring this re chloride volume is 4500ml; The content of REO is 202.48g/L, and the total recovery of rare earth is 95.6%, and the content of thorium is less than 0.01%.
Claims (6)
1. the Bayan Obo rare earth ore concentrate prepares the method for rare earth chloride, it is characterized in that, method steps is following:
(1) thermolysis: be that 60～68% Bayan Obo rare earth ore concentrate carries out thermolysis at first with grade, 400～600 ℃ of temperature, the time is 0.5～2 hour;
(2) hydrochloric acid leaches: adopt hydrochloric acid to leach concentration of hydrochloric acid 6～12mol/L, the consumption of hydrochloric acid: REO quality in the Bayan Obo rare earth ore concentrate: concentrated hydrochloric acid quality=1: 1.2～2.4 the Bayan Obo rare earth ore concentrate after the thermolysis; Extraction temperature is 60～95 ℃, and 0.5～2 hour time is in the leaching process; Add the chlorine suppressor factor, add-on: REO quality in the Bayan Obo rare earth ore concentrate: chlorine suppressor factor=1: 0.05～0.3, after hydrochloric acid leaches; Filter, get hydrochloric acid leachate and hydrochloric acid leached mud;
(3) alkali decomposes: adopt sodium hydroxide that the hydrochloric acid leached mud is carried out alkali and decompose; Sodium hydroxide concentration is 56～75% solution; Consumption is: REO quality in the Bayan Obo rare earth ore concentrate: sodium hydroxide quality=1: 0.8～1.5; Temperature was controlled at 150～230 ℃, 0.5～1.5 hour time when alkali decomposed;
(4) washing: alkali is decomposed mineral wash, washing temperature is 18～95 ℃, and washing to pH is to filter in 7～9 o'clock, water lotion and washing slag;
(5) in 1: will wash slag and join in the hydrochloric acid leachate in the step (2), temperature is 18～95 ℃, mix and stir, to pH be 0.5～2.5 o'clock, filter, in slag 1 and neutralizer 1;
(6) in 2: in neutralizer 1, add alkaline matter, stir, temperature is controlled at 18～95 ℃; Filter pH to 4～5 of adjustment neutralizer 1, in slag 2 and neutralizer 2; Neutralizer 2 is final re chloride, in slag 2 as the raw material of carrying thorium, or solid envelope is preserved.
2. Bayan Obo rare earth ore concentrate according to claim 1 prepares the method for rare earth chloride, it is characterized in that: described Bayan Obo rare earth ore concentrate is the hamartite of REO grade between 60～68% and the mixed rare earth concentrate of solitary stone ore.
3. Bayan Obo rare earth ore concentrate according to claim 1 prepares the method for rare earth chloride, it is characterized in that: described chlorine suppressor factor is thiocarbamide, H
2O
2, a kind of in the sodium sulphite, barium sulphide.
4. Bayan Obo rare earth ore concentrate according to claim 1 prepares the method for rare earth chloride, it is characterized in that: described alkaline matter is the hydroxide solution of ammoniacal liquor or alkali-metal oxyhydroxide or earth alkali metal.
5. Bayan Obo rare earth ore concentrate according to claim 1 prepares the method for rare earth chloride; It is characterized in that: described water lotion is the mixing solutions of Sodium Fluoride, sodium phosphate, sodium hydroxide; Be used to reclaim Sodium Fluoride, sodium phosphate, the raw material when unnecessary sodium hydroxide decomposes as alkali adds.
6. Bayan Obo rare earth ore concentrate according to claim 1 prepares the method for rare earth chloride, it is characterized in that: return with slag 1 in described and join next time in the alkali decomposition step.
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| CN103103349B (en) * | 2013-02-05 | 2014-08-13 | 内蒙古科技大学 | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature |
| CN104593622B (en) * | 2014-12-29 | 2017-01-18 | 乐山盛和稀土股份有限公司 | Technology for obtaining cerium enrichment with a partition larger than 99% by optimal extraction of fluoride carbonate rare earths by hydrochloric acid |
| CN104818390B (en) * | 2015-05-14 | 2016-09-28 | 孙东江 | Rare earth metal metallurgy slag environment-friendly treating process |
| CN105200247B (en) * | 2015-09-30 | 2018-06-08 | 中铝广西国盛稀土开发有限公司 | A kind of method for improving low-grade ore solubility and feed liquid removal of impurities |
| CN105543509A (en) * | 2016-01-04 | 2016-05-04 | 李梅 | Method for preparing rare earth chloride from mixed rare earth concentrate or bastnaesite concentrate |
| CN110512098A (en) * | 2019-08-29 | 2019-11-29 | 包头钢铁（集团）有限责任公司 | A kind of method that bastnaesite wet process prepares rare earth chloride |
| CN110983038A (en) * | 2020-01-03 | 2020-04-10 | 四川省冕宁县方兴稀土有限公司 | Method for inhibiting chlorine generation of acid-leaching rare earth ore and acid leaching method of fluorine-carbon-cerium roasted ore |
| CN111187926A (en) * | 2020-01-07 | 2020-05-22 | 包钢集团矿山研究院（有限责任公司） | Method for hydrometallurgical smelting of baiyuneboite concentrate |
| CN111270092B (en) * | 2020-02-07 | 2022-08-05 | 包头稀土研究院 | Method for decomposing mixed rare earth ore |
| CN114182113A (en) * | 2021-12-14 | 2022-03-15 | 上海理工大学 | Method for efficiently removing fluorine from fluorine-containing mixed rare earth chloride solution |
| CN114480835B (en) * | 2022-01-28 | 2023-12-12 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN115369243B (en) * | 2022-09-15 | 2024-04-16 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for acid leaching of rare earth roasting ore |
| CN115637340B (en) * | 2022-11-03 | 2023-09-12 | 东北大学 | Mixed rare earth concentrate suspension state ore phase conversion-clean leaching system and use method thereof |
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| CN101400607B (en) * | 2006-03-13 | 2012-03-21 | 昭和电工株式会社 | Method of recovering rare earth element from composition containing rare earth fluoride |
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| CN1240759A (en) * | 1998-07-08 | 2000-01-12 | 李玉平 | Process for preparing mixed chlorinated rare earth from bastnaesite |
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