CN105776307A - Pretreatment method for rare earth oxide separation and purification - Google Patents
Pretreatment method for rare earth oxide separation and purification Download PDFInfo
- Publication number
- CN105776307A CN105776307A CN201610082065.4A CN201610082065A CN105776307A CN 105776307 A CN105776307 A CN 105776307A CN 201610082065 A CN201610082065 A CN 201610082065A CN 105776307 A CN105776307 A CN 105776307A
- Authority
- CN
- China
- Prior art keywords
- acid
- rare earth
- earth oxide
- treatment
- treating method
- 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.)
- Granted
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
-
- 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
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention discloses a pretreatment method for rare earth oxide separation and purification.The method mainly comprises the two steps of acid treatment and crystallization treatment; acid treatment is achieved through the steps that acid soaking is performed for 1-24 h with low-concentration inorganic acid, and then cleaning is performed with high purity water; crystallization treatment is achieved through the steps that after a sample obtained through acid treatment is heated in inorganic acid with the concentration higher than that of the inorganic acid used in acid treatment to obtain a clear solution, the clear solution is placed in ice water until crystals are completely separated out, and filtering is performed to obtain rare earth salt crystals.Through the pretreatment method for rare earth oxide separation and purification, the content of part of impurity elements can be decreased, the following purification process is simplified, and the purification time is shortened.
Description
Technical field
The present invention relates to rare earth material preparation field, be specifically related to the pre-treating method of a kind of rare earth oxide separation purification.
Background technology
Rare earth element has special performance, industrially there is important application, being considered as " industry monosodium glutamate ", high pure rare earth product is widely used in cast iron, steel alloy, nonferrous metallurgy, catalysis, purifying vehicle exhaust, heat preserving and insulating material, glass decolouring and painted and radioprotective, polishing powder, permanent magnet, fluorescent material, magneto-optic memory technique, laser material, magnetostriction materials, optical fibers, photoelectric material, piezoelectric, hydrogen storage material, superconductor, atomic pile control material and composite etc..Along with scientific development and technological progress, the demand of high-purity rare-earth also being got more and more, high-purity rare-earth occupies more and more consequence in national economy and people's lives.
High purity rare earth oxides is the basis preparing high pure rare earth product, and the main method preparing high purity rare earth oxides at present has extraction, chromes, ion exchange etc..Extraction is the important method of industrial acquisition high-purity rare-earth, and for a large amount of preparations, but its purity prepared is 4N (99.99%), and purity is difficult to improve；Adopt chromes, ion exchange can obtain 5N and the sample of above purity, but its complex disposal process, time are long, and metals content impurity affects its purge process, if metals content impurity is very big, it is difficult to reach satisfied result by single treatment.
Therefore, in order to obtain higher purity rare-earth oxidation matter sample (5N and more than), it is necessary to existing method is improved.
Summary of the invention
[solving the technical problem that]
Present invention aim to address above-mentioned prior art problem, it is provided that the pre-treating method of a kind of rare earth oxide separation purification.The method, by rare earth oxide is carried out pre-treatment, reduces the content of part of impurity elements in sample, it is simple to processes subsequently through single extraction chromatography or ion exchange and obtains high-purity sample.
[technical scheme]
In order to reach above-mentioned technique effect, the present invention takes techniques below scheme:
The pre-treating method of a kind of rare earth oxide separation purification, it mainly includes acid treatment and two steps of crystallization treatment.
According to the present invention further technical scheme, described acid treatment refers to that the mineral acid utilizing low concentration carries out acid soak 1～24h, then cleans with high purity water.
According to the present invention further technical scheme, the mineral acid of described low concentration refers to that the concentration of this mineral acid is: the concentration < 2M of 0M < mineral acid.
According to the present invention further technical scheme, described mineral acid is the one in hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid, acetic acid.
According to the present invention further technical scheme, described acid treatment adds the amount of mineral acid and adds in the ratio of the ratio >=1:3 of the hydrionic amount of substance of rare earth oxide and mineral acid.
According to the present invention further technical scheme, described crystallization treatment refer to the sample that acid treatment is obtained than acid treatment time the high mineral acid of inorganic acid concentration that uses in heat to after obtaining settled solution, again described settled solution is put in frozen water and precipitate out completely to crystal, be filtrated to get rare-earth salts crystal.
According to the present invention further technical scheme, described than acid treatment time the high mineral acid of the inorganic acid concentration that uses be the one in hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid, acetic acid.
According to the present invention further technical scheme, the amount of the mineral acid that described crystallization treatment adds adds in the ratio of the ratio≤1:3 of the hydrionic amount of substance of rare earth oxide and mineral acid.
The present invention is described in detail below.
The pre-treating method of the rare earth oxide separation purification of the present invention mainly includes acid treatment and two steps of crystallization treatment.Acid treatment refers to the acid soak of relatively low for purity rare-earth oxidation matter sample low concentration；Crystallization refers to the sample filtering after by acid soak, then by the sample obtained and the acid reaction of higher concentration, becomes rare-earth salts, then by rare-earth salts crystallization.When acid treatment, the amount of the mineral acid that necessary conservative control adds and concentration, and guarantee that its acid treatment time is in 1～24h, so that making other in rare-earth oxidation matter sample material of existing in the form of an oxide, while generating soluble salt with acid reaction, it is to avoid rare earth oxide is reacted for soluble salt.Meanwhile, according in order to the acid soak complete reaction of rare earth oxide Yu higher concentration is become rare-earth salts, then need to use the acid that acid that the acid treatment that compares uses is more.
[beneficial effect]
The present invention compared with prior art, has following beneficial effect:
Utilize the pre-treating method of the rare earth oxide separation purification of the present invention, it is possible to reduce the content of part of impurity elements, simplify subsequent purification process, shorten purification time.
Detailed description of the invention
Below in conjunction with embodiments of the invention, the invention will be further elaborated.
Embodiment 1:
The pre-treating method of rare-earth oxidation ytterbium separation purification, it comprises the following steps:
Taking the rare-earth oxidation ytterbium that 5g purity is 4N and be put in 250ml flask, adding concentration is 0.01M nitric acid 150ml, soaks about 6 hours, then filters and cleans with high purity water, obtaining white solid；
Being put in by this white solid in clean 250ml flask, adding 100ml concentration is 2M high pure nitric acid, heats to 90 degree of reactions about 6 hours, obtain settled solution, then settled solution is put in 0 degree of frozen water, has clear crystal to precipitate out after placing a period of time, be filtrated to get clear crystal.
This crystal can be used for follow-up purge process.The method adopting the present invention processes the constituent content contrast of rare earth sample front and rear part as shown in table 1, and constituent content test is completed by ICP-MS.Result is as shown in table 1:
The pre-treatment front and rear part constituent content comparison sheet of table 1 the present embodiment rare-earth oxidation ytterbium separation purification
From table 1 it follows that after the pre-treatment of the separated purification of rare-earth oxidation ytterbium, part metals unit have and significantly reduces, therefore the method is conducive to processing subsequently through single extraction chromatography or ion exchange obtaining more high-purity sample.
Embodiment 2
Clear crystal embodiment 1 pre-treatment obtained, after pure water is completely dissolved, adopts chromes to carry out further purification, obtains the high-purity rare-earth ytterbium oxide of purity > 5N.
Comparative example
Taking the rare-earth oxidation ytterbium that 5g purity is 4N directly adopts chromes to be purified, and obtains high-purity rare-earth ytterbium oxide.
Utilize the rare earth sample part constituent content of ICP-MS test comparison example and embodiment 2, obtain result as shown in table 2.
Part constituent content comparison sheet in the rare-earth oxidation matter sample that table 2 is embodiment 2 and comparative example obtains
As can be seen here, after the rare earth oxide continuous way of purification after bonding separating purification pre-treatment, the rare earth oxide purity obtained is higher.Impurity metallic elements content in its rare earth oxide is less.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, above-described embodiment is only the present invention preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, should be appreciated that, those skilled in the art can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will drop within spirit disclosed in the present application and spirit.
Claims (8)
1. the pre-treating method of a rare earth oxide separation purification, it is characterised in that it mainly includes acid treatment and two steps of crystallization treatment.
2. the pre-treating method of rare earth oxide separation purification according to claim 1, it is characterised in that described acid treatment refers to that the mineral acid utilizing low concentration carries out acid soak 1～24h, then cleans with high purity water.
3. the pre-treating method of rare earth oxide separation purification according to claim 2, it is characterised in that the mineral acid of described low concentration refers to that the concentration of this mineral acid is: the concentration < 2M of 0M < mineral acid.
4. the pre-treating method of rare earth oxide separation purification according to claim 1, it is characterised in that described mineral acid is the one in hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid, acetic acid.
5. the pre-treating method of rare earth oxide separation purification according to claim 4, it is characterised in that described acid treatment adds the amount of mineral acid and adds in the ratio of the ratio >=1:3 of the hydrionic amount of substance of rare earth oxide and mineral acid.
6. the pre-treating method of rare earth oxide separation purification according to claim 2, it is characterized in that described crystallization treatment refer to the sample that acid treatment is obtained than acid treatment time the high mineral acid of inorganic acid concentration that uses in heat to after obtaining settled solution, again described settled solution is put in frozen water and precipitate out completely to crystal, be filtrated to get rare-earth salts crystal.
7. the pre-treating method of rare earth oxide separation purification according to claim 6, it is characterised in that described than acid treatment time the high mineral acid of inorganic acid concentration that uses be the one in hydrochloric acid, sulphuric acid, nitric acid, Fluohydric acid., phosphoric acid, acetic acid.
8. the pre-treating method of rare earth oxide separation purification according to claim 6, it is characterised in that the amount of the mineral acid that described crystallization treatment adds adds in the ratio of the ratio≤1:3 of the hydrionic amount of substance of rare earth oxide and mineral acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610082065.4A CN105776307B (en) | 2016-02-05 | 2016-02-05 | The pre-treating method that a kind of rare earth oxide isolates and purifies |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610082065.4A CN105776307B (en) | 2016-02-05 | 2016-02-05 | The pre-treating method that a kind of rare earth oxide isolates and purifies |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105776307A true CN105776307A (en) | 2016-07-20 |
| CN105776307B CN105776307B (en) | 2018-05-01 |
Family
ID=56402544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610082065.4A Active CN105776307B (en) | 2016-02-05 | 2016-02-05 | The pre-treating method that a kind of rare earth oxide isolates and purifies |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105776307B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456219A (en) * | 2018-05-04 | 2018-08-28 | 中国工程物理研究院化工材料研究所 | The method for preparing ultra-pure volatile cerium chelate |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044635A (en) * | 1989-02-01 | 1990-08-15 | 包钢稀土二厂 | With the rare earth slag is the processing method of feedstock production rare earth chloride |
| JPH04130014A (en) * | 1990-09-20 | 1992-05-01 | Shin Etsu Chem Co Ltd | Production of rare earth phosphate |
| EP0548434A1 (en) * | 1990-11-22 | 1993-06-30 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide powder and method for the preparation thereof |
| CN1218007A (en) * | 1997-11-21 | 1999-06-02 | 淄博兆亿保健用品实业有限公司 | Production of rare earth nitrades |
| CN1907859A (en) * | 2005-08-03 | 2007-02-07 | 北京有色金属研究总院 | Method of preparing rare earth fluoride from rare earth oxide |
| US20150197826A1 (en) * | 2010-01-22 | 2015-07-16 | Molycorp Minerals, Llc | Hydrometallurgical process and method for recovering metals |
| CN105039725A (en) * | 2015-06-28 | 2015-11-11 | 包头市玺骏稀土有限责任公司 | Method for recycling rare earth elements from rare earth electrolytic slag |
-
2016
- 2016-02-05 CN CN201610082065.4A patent/CN105776307B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1044635A (en) * | 1989-02-01 | 1990-08-15 | 包钢稀土二厂 | With the rare earth slag is the processing method of feedstock production rare earth chloride |
| JPH04130014A (en) * | 1990-09-20 | 1992-05-01 | Shin Etsu Chem Co Ltd | Production of rare earth phosphate |
| EP0548434A1 (en) * | 1990-11-22 | 1993-06-30 | Shin-Etsu Chemical Co., Ltd. | Rare earth oxide powder and method for the preparation thereof |
| CN1218007A (en) * | 1997-11-21 | 1999-06-02 | 淄博兆亿保健用品实业有限公司 | Production of rare earth nitrades |
| CN1907859A (en) * | 2005-08-03 | 2007-02-07 | 北京有色金属研究总院 | Method of preparing rare earth fluoride from rare earth oxide |
| US20150197826A1 (en) * | 2010-01-22 | 2015-07-16 | Molycorp Minerals, Llc | Hydrometallurgical process and method for recovering metals |
| CN105039725A (en) * | 2015-06-28 | 2015-11-11 | 包头市玺骏稀土有限责任公司 | Method for recycling rare earth elements from rare earth electrolytic slag |
Non-Patent Citations (4)
| Title |
|---|
| 冯宇川等: "沉淀除杂法提高稀土纯度的研究", 《江西科技师范学院学报》 * |
| 王莲贞: "废弃CRT荧光粉中提取稀土的研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 * |
| 罗永等: "高纯单一稀土提取技术研究", 《稀土》 * |
| 高胜利等: "稀土硝酸盐的制法、性质及结构", 《稀土》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108456219A (en) * | 2018-05-04 | 2018-08-28 | 中国工程物理研究院化工材料研究所 | The method for preparing ultra-pure volatile cerium chelate |
| CN108456219B (en) * | 2018-05-04 | 2020-06-16 | 中国工程物理研究院化工材料研究所 | Method for preparing ultra-pure volatile rare earth cerium chelate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105776307B (en) | 2018-05-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106319218B (en) | Method for recovering rare earth, aluminum and silicon from rare earth-containing aluminum-silicon waste | |
| KR102441721B1 (en) | Method for extraction and separation of rare earth elements | |
| Wang et al. | Application of citric acid as eluting medium for titanium type lithium ion sieve | |
| Wang et al. | Enrichment of trace rare earth elements from the leaching liquor of ion-absorption minerals using a solid complex centrifugal separation process | |
| CN103343235B (en) | Method for recovering neodymium and iron from neodymium iron boron oil sludge through two-step co-precipitation | |
| CN104928475A (en) | Recycling method of rare earth-containing aluminum silicon waste material | |
| WO2012140998A1 (en) | Method for recovering heavy rare earth element | |
| EP2902512A1 (en) | Method for collecting scandium | |
| CN111298760A (en) | Preparation method of flower-like aluminum oxide-magnesium oxide composite adsorbent, product and application thereof | |
| CN105776307A (en) | Pretreatment method for rare earth oxide separation and purification | |
| Sun et al. | Recycling rare earth from ultrafine NdFeB waste by capturing fluorine ions in wastewater and preparing them into nano-scale neodynium oxyfluoride | |
| CN104925844A (en) | Method for refining high-purity cerium carbonate | |
| WO2020138137A1 (en) | Method for purifying vanadium oxide | |
| CN112125316A (en) | Purification method of low-purity amorphous boron powder | |
| CN113772715B (en) | Anhydrous samarium chloride and preparation method thereof | |
| KR101865262B1 (en) | Method for refining carbon concentration using edta | |
| CN103667706B (en) | The separating and purifying method of gold in a kind of plation waste material | |
| CN106430278B (en) | A kind of preparation method of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide | |
| CN108330291A (en) | A kind of process for separating and purifying of platinum | |
| CN114957029A (en) | Preparation method and application of extracting agent | |
| TW201436948A (en) | Method for recycling scraped polishing powder | |
| CN112941327A (en) | Method for selectively separating vanadium and iron from red mud | |
| CN112981123A (en) | Method for recovering rare earth elements by using low-purity silicon and rare earth oxide-containing material | |
| JP4351912B2 (en) | Method for purifying niobium compound and / or tantalum compound | |
| US9797028B2 (en) | Method of purifying yttrium |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |