CN103627915A - Method of roasting, converting and decomposing fluorine-containing rear earth by calcium compound - Google Patents
Method of roasting, converting and decomposing fluorine-containing rear earth by calcium compound Download PDFInfo
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- CN103627915A CN103627915A CN201310592359.8A CN201310592359A CN103627915A CN 103627915 A CN103627915 A CN 103627915A CN 201310592359 A CN201310592359 A CN 201310592359A CN 103627915 A CN103627915 A CN 103627915A
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Abstract
The invention discloses a method of roasting, converting and decomposing fluorine-containing rear earth by a calcium compound. The method comprises the following steps of: levigating the fluorine-containing rear earth, adding the calcium compound powder for mixing, filling into a crucible after uniformly mixing; then, roasting, so that rare earth fluoride in minerals is converted into a rear earth compound which is easily dissolved in hydrochloric acid; stirring uniformly the roasted minerals in water, adding hydrochloric acid for leaching to obtain rare earth chloride liquor, wherein leaching recovery rate of the rear earth is 95%. The method disclosed by the invention does not need alkali-converting and washing, so that process flow is shortened; fluorine in the minerals is reacted to generate calcium fluoride, so that atmosphere and water are not polluted, and calcium fluoride can be reutilized. The method disclosed by the invention saves energy resources and lowers consumption, so that rear earth ore conversation rate is over 97%, and rear earth leaching recovery rate also reaches over 95%. The method disclosed by the invention has the advantages that economic benefits are increased, energy resources and mineral resources can be saved for emprises.
Description
Technical field
The present invention relates to rare earth metallurgy technical field, particularly a kind of calcium cpd roasting transforms and decomposes the method that fluorine-containing rare earth reclaims rare earth chloride.
Background technology
Hamartite is important in the world rare earth resources, and these mineral mainly originate from Sichuan Province China and U.S. awns court of a feudal ruler Paasche.China's hamartite aboundresources, be applied to industrial hamartite decomposition and Extraction of rare earth technique and reached the remaining kind of l0, as oxidizing roasting, hydrochloric acid leaching, alkali conversion, washing, hydrochloric acid leaching, sulfuric acid baking, water logging, carbon ammonium precipitation, dissolving with hydrochloric acid, it can be divided into acid system and alkaline process on the whole; Wherein acid system mainly adopts hydrochloric acid or sulfuric acid Bastnaesite, the technique of sulfuric acid strengthening roasting Bastnaesite is disclosed in the < < rare earth > > first volume that sulfuric acid process is published as: metallurgical industry press, this technological process produces HF gas, and sulfuric acid mist, not only contaminate environment but also larger to the corrodibility of equipment.The technique of salt acid system will turn defluorination by sodium hydroxide alkali after hamartite oxidizing roasting, and alkali turns ore deposit, and through washing, to carry out hydrochloric acid excellent molten, after excellent molten slag washing, entirely after molten, precipitation, calcination, obtains the cerium oxide product that purity is greater than 95% again through hydrochloric acid.This technique is turned first fluorine is removed by alkali, but consume sodium hydroxide, produces waste water containing fluorine simultaneously.
Summary of the invention
In view of above-mentioned weak point, the object of the present invention is to provide a kind of technical process simply, not need alkali to transform and washing, a kind of calcium cpd roasting that does not produce hydrogen fluoride gas and fluoride waste transforms decomposes the method that fluorine-containing rare earth reclaims rare earth chloride.
In order to achieve the above object, the present invention has adopted following technical scheme: the present invention is that calcium cpd roasting transforms the method for decomposing fluorine-containing rare earth recovery rare earth chloride, the method is that fluorine-containing rare-earth mineral is levigate, add calcium cpd powder to mix, after mixing, pack crucible into, then roasting makes the fluorine-containing rare earth in mineral be converted into the rare earth compound that is soluble in hydrochloric acid, roasted ore is uniformly mixed in the water the inside of heating and adds hydrochloric acid leaching, obtain re chloride, the leaching rate of recovery of rare earth reaches more than 95%.
Be specially: a kind of calcium cpd roasting transforms the method for decomposing fluorine-containing rare earth, carries out according to the following steps:
(1) fluorine-containing rare-earth mineral is levigate to 200 orders, be then mixed to get compound with calcium cpd powder, its blending ratio is fluorine-containing rare-earth mineral by mass: in calcium cpd, calcium simple substance is 100:5-20; The object that this step adds calcium cpd is: allow calcium and the fluorine generation Calcium Fluoride (Fluorspan) that reacts, do not produce hydrogen fluoride gas, without washing, therefore do not produce fluoride waste; The Calcium Fluoride (Fluorspan) generating is insoluble to hydrochloric acid, and fluorine can be recycled.
(2) compound mixing is put into crucible;
(3) then put into retort furnace at 800 ℃ of-1000 ℃ of roasting temperature 2-5 hour, obtain roasted ore;
(4) by mass, allow roasted ore: water mixes post-heating to 40 ℃-60 ℃ with the ratio of 5-8:1, and under agitation adds hydrochloric acid leaching, every liter of 30-40 gram of Controlled acidity, reaction 1-2 hour, slag liquid is separated, obtains rare earth chloride.
Described calcium cpd is selected from one or more in calcium carbonate, calcium hydroxide, calcium oxide.
?beneficial effect of the present invention is: the present invention does not need alkali to transform and washing, has shortened technical process, and in ore deposit, fluorine reaction generates Calcium Fluoride (Fluorspan), and all pollution-free to atmosphere and water body, Calcium Fluoride (Fluorspan) can also recycle.Save energy of the present invention reduces consumption, and rare-earth mineral transformation efficiency is reached more than 97%, and the rare earth leaching rate of recovery also reaches more than 95%; Above advantage, can be enterprise increases economic benefit, saves the energy and Mineral resources.
Embodiment
Calcium cpd roasting transforms a method of decomposing fluorine-containing rare earth, and the method is carried out according to the following steps:
(1) fluorine-containing rare-earth mineral is levigate to 200 orders, be then mixed to get compound with calcium carbonate (also can with calcium hydroxide, calcium oxide) powder, its blending ratio is fluorine-containing rare-earth mineral by mass: in calcium carbonate, calcium simple substance is 100:5-20;
(2) compound mixing is put into crucible;
(3) then put into retort furnace at 800 ℃ of-1000 ℃ of roasting temperature 2-5 hour, obtain roasted ore;
(4) by mass, allow roasted ore: water mixes post-heating to 40 ℃-60 ℃ with the ratio of 5-8:1, and under agitation adds hydrochloric acid leaching, every liter of 30-40 gram of Controlled acidity, reaction 1-2 hour, slag liquid is separated, obtains rare earth chloride.
Claims (3)
1. calcium cpd roasting transforms a method of decomposing fluorine-containing rare earth, it is characterized in that carrying out according to the following steps:
(1) fluorine-containing rare earth is levigate to 200 orders, be then mixed to get compound with calcium cpd powder, its blending ratio is fluorine-containing rare earth by mass: in calcium cpd, calcium simple substance is 100:5-20;
(2) compound mixing is put into crucible;
(3) then put into retort furnace at 800 ℃ of-1000 ℃ of roasting temperature 2-5 hour, obtain roasting rare earth;
(4) by mass, allow roasting rare earth: water mixes post-heating to 40 ℃-50 ℃ with the ratio of 5-8:1, and under agitation adds hydrochloric acid leaching, every liter of 30-40 gram of Controlled acidity, reaction 1-2 hour, slag liquid is separated, obtains rare earth chloride.
2. calcium cpd roasting according to claim 1 transforms the method for decomposing fluorine-containing rare earth, it is characterized in that: described calcium cpd is selected from one or more in calcium carbonate, calcium hydroxide, calcium oxide.
3. calcium cpd roasting according to claim 1 transforms the method for decomposing fluorine-containing rare earth, it is characterized in that: described fluorine-containing rare earth is selected from fluorine carbon cerium mischmetal ore deposit or the fluorine carbon cerium mischmetal ore deposit fluorine carbon cerium mischmetal ore deposit after oxidizing roasting adds hydrochloric acid leaching.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201310592359.8A CN103627915A (en) | 2013-11-22 | 2013-11-22 | Method of roasting, converting and decomposing fluorine-containing rear earth by calcium compound |
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| CN201310592359.8A CN103627915A (en) | 2013-11-22 | 2013-11-22 | Method of roasting, converting and decomposing fluorine-containing rear earth by calcium compound |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014154182A1 (en) * | 2013-03-29 | 2014-10-02 | 四川省彭山宇力化工有限公司 | Method for converting and decomposing bastnaesite rare earth ore by calcinating same with calcium compound and masking agent |
| CN104694736A (en) * | 2015-03-23 | 2015-06-10 | 东北大学 | Calcium roasting floatation separation method for bastnaesite |
| CN104843761A (en) * | 2015-03-31 | 2015-08-19 | 福建省长汀金龙稀土有限公司 | Method for recovering rare earth from rare earth fluoride fused salt electrolysis waste with effects of environmental protection and low cost |
| CN105177324A (en) * | 2015-10-21 | 2015-12-23 | 江西理工大学 | Method for recovering rare earths from vacuum-calcium-thermic-reduction rare-earth slag |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
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| EP0238185A1 (en) * | 1986-03-18 | 1987-09-23 | General Motors Corporation | Metallothermic reduction of rare earth chlorides |
| CN102796888A (en) * | 2012-09-09 | 2012-11-28 | 贵州黔鸿瑞磷稀土分裂开发有限公司 | Process for extracting rare earth from phosphate concentrate |
| CN103184332A (en) * | 2013-03-29 | 2013-07-03 | 四川省彭山宇力化工有限公司 | Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound |
-
2013
- 2013-11-22 CN CN201310592359.8A patent/CN103627915A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0238185A1 (en) * | 1986-03-18 | 1987-09-23 | General Motors Corporation | Metallothermic reduction of rare earth chlorides |
| CN102796888A (en) * | 2012-09-09 | 2012-11-28 | 贵州黔鸿瑞磷稀土分裂开发有限公司 | Process for extracting rare earth from phosphate concentrate |
| CN103184332A (en) * | 2013-03-29 | 2013-07-03 | 四川省彭山宇力化工有限公司 | Method for roasting, converting and resolving fluorocarbon cerium rare earth mine by adding covering agent to calcium compound |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014154182A1 (en) * | 2013-03-29 | 2014-10-02 | 四川省彭山宇力化工有限公司 | Method for converting and decomposing bastnaesite rare earth ore by calcinating same with calcium compound and masking agent |
| CN104694736A (en) * | 2015-03-23 | 2015-06-10 | 东北大学 | Calcium roasting floatation separation method for bastnaesite |
| CN104843761A (en) * | 2015-03-31 | 2015-08-19 | 福建省长汀金龙稀土有限公司 | Method for recovering rare earth from rare earth fluoride fused salt electrolysis waste with effects of environmental protection and low cost |
| CN105177324A (en) * | 2015-10-21 | 2015-12-23 | 江西理工大学 | Method for recovering rare earths from vacuum-calcium-thermic-reduction rare-earth slag |
| CN105177324B (en) * | 2015-10-21 | 2017-05-10 | 江西理工大学 | Method for recovering rare earths from vacuum-calcium-thermic-reduction rare-earth slag |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
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Application publication date: 20140312 |