CN1008082B - Precipitating rare-earth by using ammonium bicarbonate - Google Patents
Precipitating rare-earth by using ammonium bicarbonateInfo
- Publication number
- CN1008082B CN1008082B CN86100671A CN86100671A CN1008082B CN 1008082 B CN1008082 B CN 1008082B CN 86100671 A CN86100671 A CN 86100671A CN 86100671 A CN86100671 A CN 86100671A CN 1008082 B CN1008082 B CN 1008082B
- Authority
- CN
- China
- Prior art keywords
- rare earth
- feed liquid
- precipitation
- rare
- bicarbonate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a method for precipitating and separating rare earth compounds from rare-earth liquid by using ammonium bicarbonate as precipitant, which is suitable for rare earth precipitation and separation from rare-earth liquid obtained by different approaches. The precipitation processes can be mainly divided into two stages of the pretreatment and the precipitation. The present invention has the advantages that the method can greatly reduce the cost of the rare earth production, and have no harm to human bodies or environment pollution, the precipitation rate can reach more than 95%, and the purity of the rare earth products can reach more than 92%.
Description
The present invention makes precipitation agent precipitates and isolates rare earth compound from rare earth feed liquid method with bicarbonate of ammonia.
A kind of method of using the yellow soda ash precipitating rare earth when aluminium exists is disclosed in CHem.Abstr.75.155470a, when making precipitation agent with yellow soda ash, because its alkalescence is stronger, pH value is higher during precipitating rare earth, very easily generate and be difficult for filtering subcarbonate, and the contamination precipitation amount is also more thereupon, local when excessive at yellow soda ash in addition, different rare earth components is easily generated the complex compound of double salt precipitation or solubility, so the purity of rare earth and loss amount all seldom arrive satisfied result.Disclosed in the clear 53-95900 of JP is a kind of method of making the rare earth carbonate powder with carbonate or hydrocarbonate precipitation, but it can not be separated impurity from rare earth.And at present industrial commonly used mainly be the oxalic acid precipitation agent, this precipitation agent also exists precipitation cost height, environmental pollution is big, sedimentation time is long and the rare earth loss more than shortcoming.
The method that the purpose of this invention is to provide effective precipitation agent of a kind of precipitate and separate and precipitate and separate.
Making precipitation agent with bicarbonate of ammonia can achieve the above object.The process of precipitation process is: at first the rare earth feed liquid that obtains through different approaches is carried out neutralizing treatment, make feed liquid PH=4.8-5.1 and add a small amount of (for feed liquid weight 0.001～0.003%) iron(ic) chloride (concentration 14～16%) or Tai-Ace S 150 (concentration 18～20%) reaction a quarter to half an hour, add 3～5% ammonium bicarbonate soln again, to feed liquid PH=5.2～5.5, make partial impurities produce precipitation, this is the pre-treatment of feed liquid in advance.Secondly add 5～10% ammonium bicarbonate soln in the feed liquid after removing precipitated impurities than the amount of (weight ratio of contained rare earth/bicarbonate of ammonia in the feed liquid) 1/3～4 by precipitation, and add the polyacrylamide flocculation agent of (about 1～2 gram of feed liquid per ton) on a small quantity, precipitate 1～2 hour.
Compare with the yellow soda ash precipitation agent, pH value during precipitating rare earth of the present invention is not high, the tendency that generates subcarbonate is much smaller, impurity is easy to separate, and bicarbonate of ammonia is local excessive, double salt complex compound or precipitation can be do not formed yet, thereby the purity and the yield of rare earth can be guaranteed.
Compare with the oxalic acid precipitation agent, it is low that the present invention has (1) precipitate and separate cost, and one ton of rare earth oxide of every production can reduce cost 4 to 5,000 yuan; (2) non-environmental-pollution; (3) sedimentation time being reduced to more than 12 hours 1～2 hour from the past; (4) the deposition rate height of rare earth (particularly heavy rare earths).
Adopt the present invention, the deposition rate of rare earth can reach more than 95%, and the purity of rare earth oxide is more than 92%, and the rare earth total recovery during the mother liquor recycling use can reach more than 85%.If be used for doing the rare earth feed liquid processing of eluent with ammonium sulfate, then can remake eluent after the mother liquor acidifying and use, production cost can further be reduced.
Inventive embodiment
To the precipitate and separate of ion type rareearth ore through the rare earth feed liquid of the full drip washing of ammonium sulfate, its treating processes as previously mentioned, following table is the main technical data that two test feed liquids are handled.
Test lot number A-32 3-1
Feed liquid situation material liquid PH value 4.85 4.65
Material liquid volume (liter) 1,100 150000
Content of rare earth (grams per liter) 1.140 0.825
Pre-treatment bicarbonate of ammonia concentration 5% 3%
Stage bicarbonate of ammonia consumption (liter) 8 3300
20% 3 liters of pre-addition of aluminum sulfate
The place
14% 0.03 liter of reason iron(ic) chloride consumption
Rank
Section is handled back material liquid PH value 5.2 5.45
Feed liquid middle-weight rare earths amount (kg) 1.1025 103
Bicarbonate of ammonia concentration 10% 10%
The precipitate phase precipitation was than 1: 3.54 1: 3.5
Flocculation agent consumption (liter) 0.1% 3 0.1% 740
Precipitate 1.5 hours 2 hours storage period
Precipitation result deposition rate (%) 98.25 96.24
Rare earth oxide purity (%) 94.14 93.53
Claims (4)
1, from rare earth feed liquid, precipitates and isolates the method for rare earth compound with the precipitation agent that contains carbonate, it is characterized in that making precipitation agent with bicarbonate of ammonia, after earlier material liquid PH value being neutralized to 4.8-5.1, add iron(ic) chloride or aluminum sulfate aqueous solution, adding bicarbonate of ammonia then, to make pH value be that 5.2-5.5 is to carry out part removal of impurities pre-treatment, in the last feed liquid after the part removal of impurities, be 1 by the weight ratio of contained rare earth and bicarbonate of ammonia in the feed liquid: the amount of 3-4, adding bicarbonate of ammonia precipitates.
2, method according to claim 1 is characterized in that the ferric chloride concn that adds is that 18-20%, amount are 100,000/1-3 of feed liquid weight to react 15-30 minute.
3, method according to claim 1 is characterized in that the Tai-Ace S 150 concentration that adds is that 14-16%, amount are 100,000/1-3 of feed liquid weight to react 15-30 minute.
According to claim 1,2,3 described methods, it is characterized in that in the rare-earth precipitation process that 4, rare earth feed liquid per ton adds 1-2 gram polyacrylamide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86100671A CN1008082B (en) | 1986-01-25 | 1986-01-25 | Precipitating rare-earth by using ammonium bicarbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN86100671A CN1008082B (en) | 1986-01-25 | 1986-01-25 | Precipitating rare-earth by using ammonium bicarbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN86100671A CN86100671A (en) | 1987-08-05 |
| CN1008082B true CN1008082B (en) | 1990-05-23 |
Family
ID=4801150
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN86100671A Expired CN1008082B (en) | 1986-01-25 | 1986-01-25 | Precipitating rare-earth by using ammonium bicarbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1008082B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1042146C (en) * | 1994-03-18 | 1999-02-17 | 冶金工业部长沙矿冶研究院 | Preparation method of crystal form rare earth carbonate |
| CN1054356C (en) * | 1995-07-05 | 2000-07-12 | 南昌大学 | Method for crystallizing and sedimenting rare-earth carbonate |
| CN100393623C (en) * | 2006-07-27 | 2008-06-11 | 江阴加华新材料资源有限公司 | Large particle rare-earth oxide and its preparing method |
| CN101037219B (en) * | 2007-04-28 | 2010-06-02 | 包头华美稀土高科有限公司 | Production process of magnesia used for rear earth solution precipitator |
| CN101200304B (en) * | 2007-09-19 | 2010-07-21 | 王洪志 | Technique for producing 99% praseodymium-neodymium oxides by using Nd-Fe-B smelting slag |
| CN102757080A (en) * | 2012-07-19 | 2012-10-31 | 山东齐鲁华信高科有限公司 | Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve |
| CN110184460B (en) * | 2019-06-28 | 2020-12-15 | 四川省乐山锐丰冶金有限公司 | Method for removing aluminum ions from praseodymium-neodymium chloride feed liquid |
| US11447397B1 (en) | 2021-03-19 | 2022-09-20 | Lynas Rare Earths Limited | Materials, methods and techniques for generating rare earth carbonates |
| CN115010165A (en) * | 2022-05-20 | 2022-09-06 | 全南县新资源稀土有限责任公司 | Preparation method of rare earth carbonate and preparation method of rare earth oxide |
-
1986
- 1986-01-25 CN CN86100671A patent/CN1008082B/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| CN86100671A (en) | 1987-08-05 |
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| C13 | Decision | ||
| GR02 | Examined patent application | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |