CN101476033B - Novel method for leaching, impurity removing and precipitating ion type rare earth ore - Google Patents
Novel method for leaching, impurity removing and precipitating ion type rare earth ore Download PDFInfo
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- CN101476033B CN101476033B CN2008101759127A CN200810175912A CN101476033B CN 101476033 B CN101476033 B CN 101476033B CN 2008101759127 A CN2008101759127 A CN 2008101759127A CN 200810175912 A CN200810175912 A CN 200810175912A CN 101476033 B CN101476033 B CN 101476033B
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Abstract
The invention relates to a novel method of ion type rare-earth ore leaching, impurity removing and depositing, and the method consists of steps of leaching of ion type rare-earth ore, impurity removing for the rare earth leaching liquid, depositing of the rare earth solution after the impurity removal, rare earth burning and the like.The method is characterized in that a mixed leaching agent consisting of calcium chloride of 1-10% and ammonium chloride of 0.5-2% is added to the ion type rare earth ore leaching pond or in-situ place; using calcium oxide and water with a weight ratio of 1: (2-20) to the rare earth leaching liquid to obtain lime cream the PH of which is then adjusted to 5.0-5.4 and then a impurity removal process is performed; after the impurity removal process, the rare earth is deposited by using a deposition agent which is calcium oxide or a mixer of calcium oxide and seed crystal (the quantity ratio of the rare earth, the calcium oxide and the seed crystal is 1: (2-3) : (1/3-3)l in the rare earth solution, and in a sedimentation tank with seed crystal or added with seed crystal, the PH of the solution is adjusted to 8.0-9.0 by using lime cream to deposit the rareearth.The invention has characteristics of high rate of deposition of rare earth, environment protection by the reutilization of waste water, and further reducing of production cost.
Description
Technical field
The present invention relates to a kind of novel method of leaching, impurity removing and precipitating ion type rare earth ore, belong to technical field of wet metallurgy.
Technical background
From China ion adsorption type rare earth ore be found, after the invention of name and maceration method extraction process, the deposit impregnating technology of ion adsorption type rare earth ore successively adopts sodium-chlor and ammonium sulfate as soaking the ore deposit agent, and depositing technology successively adopts oxalic acid, bicarbonate of ammonia ammoniacal liquor, yellow soda ash etc. as precipitation agent precipitating rare earth from rare earth feed liquid.Present production technique one is not have impurity removal process, and product impurity is higher; The 2nd, deposit impregnating technology and depositing technology use ammonium sulfate, oxalic acid and bicarbonate of ammonia, ammonium, nitrogen content discharging exceed standard, the wastewater treatment difficulty is big, general manufacturer does not carry out the waste water reclamation utilization, environment is polluted, indivedual producers reclaim the waste water of sectional interest, but cost recovery is very high.
Summary of the invention
In order to overcome the deficiency that existing ion adsorption type re soaks impurity-removing precipitating aspect, ore deposit, the invention provides a kind of novel method of leaching, impurity removing and precipitating ion type rare earth ore.When guaranteeing high purity product, simplify flow chart, reduce waste water ammonium, nitrogen content, the protection environment can reduce production costs again significantly, improves business economic benefit and social benefit.
The technical solution adopted for the present invention to solve the technical problems is: a kind of novel method of leaching, impurity removing and precipitating ion type rare earth ore, and it is made up of the operations such as ore deposit, removal of impurities, precipitation and rare earth calcination of soaking of ion type rareearth ore, it is characterized in that:
A kind of novel method of leaching, impurity removing and precipitating ion type rare earth ore, it is made up of the operations such as ore deposit, removal of impurities, precipitation and rare earth calcination of soaking of ion type rareearth ore, it is characterized in that:
(1) soaks the ore deposit: soak in the rare-earth mineral pond or the original place is soaked in the ore deposit to add and formed mixing by calcium chloride and ammonium chloride and soak the ore deposit agent and soak the ore deposit, soak when leaching mother liquor rare earth concentration is lower than 0.3g/L in the ore deposit in the original place, all feed back and soak the ore deposit, leach the mother liquor rare earth concentration and enter impurity removal process after greater than 0.3g/L;
(2) removal of impurities: re dip solution is adjusted pH (5.0～5.4) with milk of lime carry out removal of impurities and remove metallic impurity such as aluminium, iron, the clear liquid of placing after the clarification enters depositing technology;
(3) precipitation: in settling tank, put into the crystal seed for preparing in advance, squeeze into rare earth infusion solution after the removal of impurities, calcium oxide or milk of lime joined as precipitation agent carry out precipitin reaction in the settling tank, adding speed 0.5～2 hour, stirred 1～3 hour, to precipitate good slip again squeezes into the transition jar and carries out filter dehydration, the output filter cake.Filter cake adds water sizes mixing and carries out washing and filtering dehydration more for several times, and the solid phase prod after the dehydration is rare earth hydrate, the wash water recycling.
According to the novel method of above-mentioned described a kind of leaching, impurity removing and precipitating ion type rare earth ore, deposit impregnating technology is characterised in that: be made up of to mix calcium chloride and ammonium chloride and soak the ore deposit agent, its consumption is (1～10%) calcium chloride, (0.5～2%) ammonium chloride.
According to the novel method of above-mentioned described a kind of leaching, impurity removing and precipitating ion type rare earth ore, impurity removal process is characterised in that: milk of lime is calcium oxide: water=1:(2～20 by add weight ratio in water) unslaked lime under 20 ℃～60 ℃, size mixing and make.
Novel method according to above-mentioned described a kind of leaching, impurity removing and precipitating ion type rare earth ore, depositing technology is characterised in that: utilize calcium oxide or milk of lime auxiliary down as the precipitation agent precipitating rare earth at crystal seed, when utilizing calcium oxide to make precipitation agent, its usage ratio is: rare earth content: calcium oxide=1:(2～3), the amount of seed ratio is: rare earth content: crystal seed=1:(1/3～3), it is auxiliary that precipitation needs to add crystal seed for the first time, and the back then need not to add because of retaining crystal seed in the settling tank again.
The production technique that is used for rear earth solution precipitator according to above-mentioned described a kind of calcium oxide, it is characterized in that: crystal seed is the crystal formation rare-earth hydroxide of corresponding generation when utilizing calcium oxide to make the precipitation agent precipitating rare earth, also can adopt corresponding crystal formation rare earth oxalate to use as initial seed.
The invention has the beneficial effects as follows:
Mix and to soak the ore deposit agent and can reach ammonium sulfate and soak the ore deposit effect, waste water is recycled, mix and soak that calcium chloride can be recycled in the agent of ore deposit, need not add after adding once again, as long as replenish ammonium chloride, ammonium chloride is more cheap than ammonium sulfate, and consumption also still less; Rare-earth precipitation rate Gao Keda 99%, throw out is the crystal formation rare earth hydrate, be convenient to filtration washing, products obtained therefrom purity height (〉=92%), and can without calcination directly acid carry out Rare Earth Separation after molten, can further reduce production costs and the waste water reclamation cost, not only economy but also material benefit, reduced ammonium in the waste water, nitrogen content simultaneously, solved the cleaner production problem of rare earth, the present invention can be applied to the production of all kinds of ion type rareearth ores.
Embodiment
Embodiment one
Quannan County, Jiangxi Province rare earth small mines, average 6 meters of rare earth layer thickness, rare earth average grade 0.47 ‰, these ore body rare earth reserves are 15 tons, ionic type rare earth ore in-situ lixiviation processing is adopted in the mine, finish the ore body surface and beat operations such as fluid injection well, wiring and ore body bottom brill liquid-collecting hole.According to ore body rare earth reserves, be made into the mixing of 3% calcium chloride and 1% ammonium chloride and soak 4500 cubes of ore deposit agent, adopt the 35kw liquid charge pump to inject 300 cubes every day, mixing is soaked the ore deposit agent and was annotated in 15 days, beginning leach liquor mother liquor rare earth concentration is lower than 0.3g/L, all return and soak the ore deposit again, leaching mother liquid concentration receives liquid pump with 22.5kw after greater than 0.3g/L and is extracted in the removal of impurities pond, inject milk of lime (water add weight ratio be the unslaked lime of calcium oxide: water=1:10 size mixing make) transfer pH5.4 to remove metallic impurity such as ferro-aluminum, place clarification back clear liquid and flow into settling tank, the milk of lime precipitating rare earth reinjects, fully stir with the 7.5kw air compressor machine, leave standstill back supernatant liquor pH8.5, put into and pond for recovering, regulate pH to 5.5 with hydrochloric acid, return the injection mine as recycle-water and soak the ore deposit.Mother liquor rare earth concentration peak value is 1～2g/L, treats that rare earth collects near reserves, changes to annotate clear water and receive liquid, leaches mother liquor through milk of lime removal of impurities and precipitation, and supernatant liquid is put into and pond for recovering, and throw out is then used the clear water washed twice, squeezing back dress bag.
25.4 tons of output rare-earth hydroxides burn till 15.6 tons of rare earth oxides, RE in the rare earth oxide product
2O
3%:92.6%, Al
2O
3%:1.5%, CaO%:2.1%.
Embodiment two
Quannan County, Jiangxi Province rare earth small mines, average 6 meters of rare earth layer thickness, rare earth average grade 0.5 ‰, these ore body rare earth reserves are 18 tons, ionic type rare earth ore in-situ lixiviation processing is adopted in the mine, finish the ore body surface and beat operations such as fluid injection well, wiring and ore body bottom brill liquid-collecting hole.With in leaving among the embodiment one and pond for recovering in clear liquid add 1% ammonium chloride, regulate pH to 5.5 back as soaking the ore deposit agent with hydrochloric acid, also need prepare 3% calcium chloride and 1% ammonium chloride according to clear liquid amount in these ore body reserves and the pond for recovering mixes and soaks 2000 cubes of ore deposit agent, adopt the 35kw liquid charge pump to inject 350 cubes every day, mixing is soaked the ore deposit agent and was annotated in 15 days, leach liquor mother liquor rare earth concentration is lower than returning of 0.3g/L and soaks the ore deposit again, concentration is extracted in the removal of impurities pond with 22.5kw receipts liquid pump greater than 0.3g/L's, inject milk of lime (water add weight ratio be the unslaked lime of calcium oxide: water=1:10 size mixing make) transfer pH5.4, place clarification back clear liquid and flow into settling tank, be placed with the embodiment one output crystal formation rare-earth hydroxide that accounts for pond 1/4 amount in the settling tank, injecting milk of lime fully stirs with the 7.5kw air compressor machine, transfer pH9.0, clear liquid is put into and pond for recovering, regulate pH to 5.5 with hydrochloric acid, return the injection mine as recycle-water and soak the ore deposit.Mother liquor rare earth concentration peak value is 1～2g/L, treats that rare earth collects near reserves, changes to annotate clear water and receive liquid, leaches mother liquor through the milk of lime impurity-removing precipitating, and supernatant liquid is put into and pond for recovering, throw out clear water washed twice, and squeezing back dress wraps.
32.7 tons of output rare-earth hydroxides,, burn till 18.4 tons of rare earth oxides, RE in the rare earth oxide product
2O
3%:93.5%, Al
2O
3%:1.3%, CaO%:1.5%.
Embodiment three
In mine-dipping pool, pour 500 kilograms of rare-earth original ores (Quannan County, Jiangxi Province rare-earth mineral raw ore into, grade 0.59 ‰), the ore deposit agent is soaked in the mixing of 1% ammonium chloride, 5% calcium chloride add mine-dipping pool for 500 liters, wait to soak the ore deposit agent and permeated 100 liters in adding top, back water substantially, leach liquor is collected, collect 455 liters in mother liquor altogether, RE
2O
3Content is 0.61g/L, and leaching yield is 93.8%, and receiving the liquid rate is 75.8%.
With weight ratio is that the size mixing milk of lime that makes of calcium oxide: water=1:8 adds to leach in the mother liquor and regulates pH5.4, the clarification after-filtration, filtrate continuation adds milk of lime to pH9.0, clarification place the ageing section after the time pH be 8.4, what this moment, filtration obtained is crystal formation rare-earth hydroxide precipitation, filtrate is replenished 1% ammonium chloride, and regulates pH to 5.5 with hydrochloric acid, does and soaks ore deposit agent use next time.Throw out filters with the clear water washing for several times, and 105 ℃ of oven dry obtain rare-earth hydroxide 254g, casting yield 77.9%, and rare-earth hydroxide advances incinerator, gets the mixed rare earth oxide product after 950 ℃ of calcinations.RE in the product
2O
3%:92.2%, Al
2O
3%:1.6%, CaO%:2.3%.
Embodiment four
In mine-dipping pool, pour 400 kilograms of rare-earth original ores (Quannan County, Jiangxi Province rare-earth mineral raw ore into, grade 0.59 ‰), in 400 liters of embodiment, three middle-weight rare earths post precipitation filtrates, add 4 kilograms of ammonium chlorides and add hydrochloric acid and regulate ore leachate pH5.5, ore leachate is injected mine-dipping pool, wait to soak the ore deposit agent and permeated 80 liters in adding top, back water substantially, leach liquor is collected, collected 352 liters in mother liquor altogether, RE
2O
3Content is 0.64g/L, and leaching yield is 95.1%, and receiving the liquid rate is 73.3%.
With weight ratio is that calcium oxide: water=1:8 sizes mixing and makes milk of lime and add the leaching mother liquor to pH5.4, the clarification after-filtration, the crystal formation rare-earth hydroxide 50g that obtains among adding 180g unslaked lime and the embodiment two in the filtrate is as mixed precipitant, fully stir, the clarification after-filtration, filtrate is replenished 1% ammonium chloride, and regulates pH to 5.5 with hydrochloric acid, continues to do and soaks ore deposit agent use next time.Throw out filters with the clear water washing for several times, and 105 ℃ of oven dry obtain rare-earth hydroxide 250g, casting yield 80%, and rare-earth hydroxide advances incinerator, gets mixed rare earth oxide product, RE in the product after 950 ℃ of calcinations
2O
3%:91.7%, Al
2O
3%:1.5%, CaO%:2.7%.
Claims (5)
1. the method for a leaching, impurity removing and precipitating ion type rare earth ore, it is made up of soak ore deposit, removal of impurities, precipitation and the rare earth calcination operation of ion type rareearth ore, it is characterized in that:
(1) soaks the ore deposit: soak in the rare-earth mineral pond or the original place is soaked in the ore deposit to add and formed mixing by calcium chloride and ammonium chloride and soak the ore deposit agent and soak the ore deposit, soak when leaching mother liquor rare earth concentration is lower than 0.3g/L in the ore deposit in the original place, all feed back and soak the ore deposit, leach the mother liquor rare earth concentration and enter impurity removal process after greater than 0.3g/L;
(2) removal of impurities: re dip solution is adjusted pH5.0～5.4 with milk of lime carry out removal of impurities and remove aluminium, ferrous metal impurity, the clear liquid of placing after the clarification enters depositing technology;
(3) precipitation: in settling tank, put into previously prepared crystal seed, squeeze into rare earth infusion solution after the removal of impurities, calcium oxide or milk of lime joined as precipitation agent carry out precipitin reaction in the settling tank, adding speed 0.5～2 hour, stirred 1～3 hour, to precipitate good slip again squeezes into the transition jar and carries out filter dehydration, the output filter cake; Filter cake adds water sizes mixing and carries out washing and filtering dehydration more for several times, and the solid phase prod after the dehydration is rare earth hydrate, the wash water recycling.
2. the method for a kind of leaching, impurity removing and precipitating ion type rare earth ore according to claim 1 is characterized in that: be made up of to mix calcium chloride and ammonium chloride and soak the ore deposit agent, its consumption is 1～10% calcium chloride, 0.5～2% ammonium chloride.
3. the method for a kind of leaching, impurity removing and precipitating ion type rare earth ore according to claim 1 is characterized in that: milk of lime is calcium oxide by add weight ratio in water: water=1: the unslaked lime of (2～20) is sized mixing under 20 ℃～60 ℃ and is made.
4. the method for a kind of leaching, impurity removing and precipitating ion type rare earth ore according to claim 1, it is characterized in that: utilize calcium oxide or milk of lime auxiliary down as the precipitation agent precipitating rare earth at crystal seed, when utilizing calcium oxide to make precipitation agent, its usage ratio is: rare earth content: calcium oxide=1: (2～3), the amount of seed ratio is: rare earth content: crystal seed=1: (1/3～3), it is auxiliary that precipitation needs to add crystal seed for the first time, and the back then need not to add because of retaining crystal seed in the settling tank again.
5. the method for a kind of leaching, impurity removing and precipitating ion type rare earth ore according to claim 1, it is characterized in that: crystal seed is the crystal formation rare-earth hydroxide of corresponding generation when utilizing calcium oxide to make the precipitation agent precipitating rare earth.
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Application publication date: 20090708 Assignee: Quannan Baotou Steel Jinghuan Rare Earth Co., Ltd. Assignor: Huang Riping|Zhong Yueming| Wu Yuanxu Contract record no.: 2012360000051 Denomination of invention: Novel method for leaching, impurity removing and precipitating ion type rare earth ore Granted publication date: 20110406 License type: Exclusive License Record date: 20120730 |
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Application publication date: 20090708 Assignee: Quannan Baotou Steel Jinghuan Rare Earth Co., Ltd. Assignor: Huang Riping|Zhong Yueming|Wu Yuanxu Contract record no.: 2012360000051 Denomination of invention: Novel method for leaching, impurity removing and precipitating ion type rare earth ore Granted publication date: 20110406 License type: Exclusive License Record date: 20120730 |
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