CN102757080A - Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve - Google Patents
Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve Download PDFInfo
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- CN102757080A CN102757080A CN2012102513972A CN201210251397A CN102757080A CN 102757080 A CN102757080 A CN 102757080A CN 2012102513972 A CN2012102513972 A CN 2012102513972A CN 201210251397 A CN201210251397 A CN 201210251397A CN 102757080 A CN102757080 A CN 102757080A
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- rare earth
- rare
- molecular sieve
- recovery method
- sodium hydrogencarbonate
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Abstract
The invention relates to a rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve and belongs to the field of a chemical process. The rare earth recovery method is characterized by comprising the steps of: precipitating and separating out rare earth compound from rare-earth molecular sieve mother liquor by taking sodium bicarbonate as a precipitator, wherein the precipitating and separating process mainly comprises two stages of pretreatment and precipitation; the precipitation rate is over 98%; the precipitation yield is high, and no NH3-N (ammonia-nitrogen) exists in the discharged waste liquid; the sewage treatment cost is reduced; and the granularity of the sediment is large, and filtering and washing are easy.
Description
Technical field
The present invention relates to the rare earth recovery method of a kind of sodium hydrogencarbonate in rare earth Y type molecular sieve is produced, belong to the chemical technique field.
Background technology
The REY molecular sieve is through RECl by the NaY molecular sieve
3A kind of active height that exchanges modification and obtain, the molecular sieve of good stability are widely used.In the REY exchange, the RE utilization ratio is the highest by 90%.Industry at present goes up that precipitating rare earth mainly adopts oxalic acid, ammoniacal liquor and bicarbonate of ammonia to make precipitation agent from earth solution.Do precipitation agent with oxalic acid, the purity of rare-earth products is high, and but exist following deficiency: (1) price is more expensive, and production cost is high, and (2) are poisonous, and environmental pollution is big; (3) at normal temperatures ST is long; (4) rare-earth oxalate in water particularly in ammonium oxalate solution solubleness big, the loss of rare earth is many.Do precipitation agent with ammoniacal liquor, behind the adding ammoniacal liquor, generate rare earth hydrate in the rare earth feed liquid, add Hydrogen chloride then, generate the rare earth chloride reuse with the rare earth compound reaction.The deposition rate of this method, is difficult to carry out solid-liquid separation because the throw out of this method is a floss less than 90%, thereby makes the Na in the exchange mother liquor
+, Al
3 +, NH
4 +, Cl
-Again get into exchange liquid etc. objectionable constituent, and with the rare earth ion exchange effect of competing, exchange degree is reduced.Simultaneously, because the RE (OH) that reclaims
3In contain a large amount of NH4Cl, when adding dissolving with hydrochloric acid RE (OH)
3The time, can form certain NH in the dissolving tank
3-NH
4Cl buffered soln causes the salt acid consumption excessive, has slowed down RE (OH)
3Dissolution rate, and NH in institute's sewer
3-N content is high, has increased cost of sewage disposal.Do precipitation agent with bicarbonate of ammonia, this method precipitate and separate cost is low, non-environmental-pollution, and to human non-toxic, but the same with ammoniacal liquor, contain a large amount of NH in institute's removal waste fluid
3-N, cost of sewage disposal is high.Summary of the invention
According to the deficiency of prior art, the technical problem that the present invention will solve is: the rare earth recovery method of a kind of sodium hydrogencarbonate in rare earth Y type molecular sieve is produced is provided, and the precipitate and separate rare earth compound does not have NH in the waste liquid that is discharged from rare earth feed liquid
3-N composition, sedimentation effect is good
The technical solution adopted for the present invention to solve the technical problems is: the rare earth recovery method of a kind of sodium hydrogencarbonate in rare earth Y type molecular sieve is produced is provided; It is characterized in that comprising: do precipitation agent with sodium hydrogencarbonate and from the rare earth containing zeolite mother liquor, precipitate and isolate rare earth compound, the precipitate and separate process mainly comprises pre-treatment and two stages of deposition.
Said feed liquid pretreatment stage adds sodium hydrogencarbonate in the feed liquid, make the PH of rare earth feed liquid be adjusted to 7 ~ 9 by 3 ~ 5.
Said precipitate phase, rare earth feed liquid deposition 15-40 minute.
The rare earth of said post precipitation is through filtration washing.
When the rare earth that uses after reclaiming, press certain weight proportion and add Hydrogen chloride.
Advantage of the present invention is:
1, deposition rate reaches more than 98%, and precipitate recovery rate is high;
2, there is not NH in institute's removal waste fluid
3-N has reduced cost of sewage disposal;
3, the throw out granularity is bigger, is easy to filtration washing;
Adopt the present invention, the deposition rate of rare earth can reach more than 98%, and the throw out granularity is big, and the easy filtration washing does not have NH in institute's removal waste fluid
3-N effectively reduces cost of sewage disposal.
Embodiment
Below in conjunction with embodiment the present invention is done and to further describe:
Embodiment 1
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 2.6%), be warming up to 50 ℃, add sodium hydrogencarbonate 7g, continuously stirring 2 hours, quiescent setting 20 minutes filtered washing after 15 minutes, and 130 ℃ of dry 12.8g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 2
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 3.6%), be warming up to 60 ℃, add sodium hydrogencarbonate 9g, continuously stirring 1.5 hours, quiescent setting 30 minutes filtered washing after 20 minutes, and 150 ℃ of dry 15.5g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 3
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 5.2%), be warming up to 55 ℃, add sodium hydrogencarbonate 18g, continuously stirring 1.5 hours, quiescent setting 20 minutes filtered washing after 20 minutes, and 170 ℃ of dry 23.5g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 4
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 7.5%), be warming up to 60 ℃, add sodium hydrogencarbonate 25g, continuously stirring 1.5 hours, quiescent setting 25 minutes filtered washing after 20 minutes, and 150 ℃ of dry 32.2g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 5
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 1.2%), be warming up to 70 ℃, add sodium hydrogencarbonate 5g, continuously stirring 1.5 hours, quiescent setting 15 minutes filtered washing after 10 minutes, and 130 ℃ of dry 3.5g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 6
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 2.3%), be warming up to 70 ℃, add sodium hydrogencarbonate 7g, continuously stirring 1.5 hours, quiescent setting 20 minutes filtered washing after 15 minutes, and 160 ℃ of dry 10.6g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 7
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 0.8%), be warming up to 50 ℃, add sodium hydrogencarbonate 3g, continuously stirring 1.5 hours, quiescent setting 20 minutes filtered washing after 20 minutes, and 150 ℃ of dry 2.6g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Embodiment 8
Get rare earth containing zeolite mother liquor 500g (Re
2O
3Content 11.2%), be warming up to 70 ℃, add sodium hydrogencarbonate 50g, continuously stirring 2 hours, quiescent setting 15 minutes filtered washing after 15 minutes, and 170 ℃ of dry 52.6g carbonated rare earths that get are got dissolve with hydrochloric acid solution, get re chloride.
Claims (4)
1. the sodium hydrogencarbonate rare earth recovery method in rare earth Y type molecular sieve is produced; It is characterized in that comprising: do precipitation agent with sodium hydrogencarbonate and from the rare earth containing zeolite mother liquor, precipitate and isolate rare earth compound, the precipitate and separate process mainly comprises pre-treatment and two stages of deposition.
2. the rare earth recovery method of sodium hydrogencarbonate according to claim 1 in rare earth Y type molecular sieve is produced is characterized in that said feed liquid pretreatment stage, adds sodium hydrogencarbonate in the feed liquid, makes the PH of rare earth feed liquid be adjusted to 7 ~ 9 by 3 ~ 5.
3. the rare earth recovery method of sodium hydrogencarbonate according to claim 1 in rare earth Y type molecular sieve is produced is characterized in that said precipitate phase, rare earth feed liquid deposition 15-40 minute.
4. the rare earth recovery method of sodium hydrogencarbonate according to claim 1 in rare earth Y type molecular sieve is produced, the rare earth that it is characterized in that said post precipitation is through filtration washing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102513972A CN102757080A (en) | 2012-07-19 | 2012-07-19 | Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012102513972A CN102757080A (en) | 2012-07-19 | 2012-07-19 | Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve |
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| CN102757080A true CN102757080A (en) | 2012-10-31 |
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| CN2012102513972A Pending CN102757080A (en) | 2012-07-19 | 2012-07-19 | Rare earth recovery method of sodium bicarbonate in production of rare-earth Y-type molecular sieve |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878201A (en) * | 2014-02-28 | 2015-09-02 | 中国石油化工股份有限公司 | Method for recovering rare earth from rare earth-containing wastewater |
| RU2729573C1 (en) * | 2019-12-30 | 2020-08-07 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing carbonates of rare-earth elements |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4497785A (en) * | 1983-11-18 | 1985-02-05 | Union Oil Company Of California | Production of rare earth compounds |
| CN86100671A (en) * | 1986-01-25 | 1987-08-05 | 江西大学 | Use the Ammonium bicarbonate food grade precipitating rare earth |
| CN1807253A (en) * | 2006-01-18 | 2006-07-26 | 朴钟殷 | Method for treating tail gas and waste water from rare earth finished ore acid method burning process |
| CN101353178A (en) * | 2002-06-07 | 2009-01-28 | 昭和电工株式会社 | Process for recovering rare earth oxide, process for producing abrasive containing rare earth oxide and polishing method using abrasive |
-
2012
- 2012-07-19 CN CN2012102513972A patent/CN102757080A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4497785A (en) * | 1983-11-18 | 1985-02-05 | Union Oil Company Of California | Production of rare earth compounds |
| CN86100671A (en) * | 1986-01-25 | 1987-08-05 | 江西大学 | Use the Ammonium bicarbonate food grade precipitating rare earth |
| CN101353178A (en) * | 2002-06-07 | 2009-01-28 | 昭和电工株式会社 | Process for recovering rare earth oxide, process for producing abrasive containing rare earth oxide and polishing method using abrasive |
| CN1807253A (en) * | 2006-01-18 | 2006-07-26 | 朴钟殷 | Method for treating tail gas and waste water from rare earth finished ore acid method burning process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104878201A (en) * | 2014-02-28 | 2015-09-02 | 中国石油化工股份有限公司 | Method for recovering rare earth from rare earth-containing wastewater |
| CN104878201B (en) * | 2014-02-28 | 2017-06-30 | 中国石油化工股份有限公司 | A kind of method of the recovering rare earth from RE waste water is contained |
| RU2729573C1 (en) * | 2019-12-30 | 2020-08-07 | Федеральное государственное автономное образовательное учреждение высшего образования "Национальный исследовательский технологический университет "МИСиС" | Method of producing carbonates of rare-earth elements |
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Application publication date: 20121031 |