CN106430278B - A kind of preparation method of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide - Google Patents
A kind of preparation method of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide Download PDFInfo
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- CN106430278B CN106430278B CN201610858817.1A CN201610858817A CN106430278B CN 106430278 B CN106430278 B CN 106430278B CN 201610858817 A CN201610858817 A CN 201610858817A CN 106430278 B CN106430278 B CN 106430278B
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- 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
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The preparation method of a kind of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide, comprises the following steps：(a) thick scandium oxide is taken, strong acid is added, dissolved by heating, filtering obtains filtrate I；(b) under agitation, 0~100 DEG C of keeping temperature, ammonium hydrogen carbonate or sodium acid carbonate are added into filtrate I, during to pH 5~8, stop adding, after sediment pure water, and filtering obtains the carbonate deposition of scandium；(c) acetic acid is added into sediment, after dissolving, filtering obtains filtrate II；(d) 70~100 DEG C of II constant temperature of heating filtrate, has after crystal precipitation, ice acetic acid, 5~30min of constant temperature, crystal is filtered while hot, collects crystal and is washed with absolute ethyl alcohol；(e) dry, obtain high-pure anhydrous acetic acid scandium；Calcination obtains High-purity Sc Oxide；(f) by high-pure anhydrous acetic acid scandium calcination, or in the case of logical oxygen self-propagating combustion is carried out, obtains High-purity Sc Oxide.The present invention has the advantages that easy to operate, environmental pollution is small.
Description
Technical field
The present invention relates to a kind of high-pure anhydrous acetic acid scandium and the preparation method of High-purity Sc Oxide.
Background technology
Scandium and its compound have many excellent performances, there is wide in terms of energy and material, aerospace, electronics, superconduction
General application.Acetic acid scandium as intermediate can prepare nano scandium oxide, nano scandium oxide film, composite catalyst centre
The raw material of body, electronic ceramics raw material and High-purity Sc Oxide.
At present, the process for refining and purifying of High-purity Sc Oxide is largely thick scandium dissolving with hydrochloric acid, oxalic acid repeated precipitation calcination, or
Through reextraction, after scrubbed back extraction, calcination is into scandium oxide again after sour molten oxalic acid precipitation, and the former scandium loss is big, and step is more, the latter
Refining effect is not good.
It is prepared by a kind of purification of High-purity Sc Oxide disclosed in the Chinese patent application of Application No. 201110186520.2
Method, mentions repeated multiple times use hydrochloric acid and ammoniacal liquor acid is molten, precipitation scandium, to reach the purpose of removal of impurities, this method step repeatedly,
And general hydroxide filtering is slowly, the purity that the scandium oxide obtained after the final oxalic acid precipitation of this method reaches is also only
99.98%.
A kind of refined purification of High-purity Sc Oxide disclosed in the Chinese patent application of Application No. 201510161206.7
Method, this method is using thick scandium oxide as raw material, under high concentration of hydrochloric acid, add scandium solution quality percent by volume 1~
20% ammonium chloride and theoretical amount 180~200% plus oxalic acid, the heavy scandium of control and filtration time are completed within 10~60min, are passed through
Secondary refining purification obtains the scandium oxide of grade more than 99.99%.This method spent acidic water is big, and oxalic acid is largely wasted, anti-
Between seasonable it is short in the case of, heavy scandium filtering is completed in preferably 10 minutes, is adapted to experiment in-house operation, industrialized production is not suitable for,
And precipitated in very short time, sediment crystal formation is unformed, and parcel moisture or other impurity are more, is difficult to control.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of easy to operate, small high-pure anhydrous second of environmental pollution
The preparation method of sour scandium and High-purity Sc Oxide.
The technical solution adopted for the present invention to solve the technical problems is：A kind of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide
Preparation method, comprise the following steps：
(a) thick scandium oxide is taken, strong acid is added, 60~100 DEG C of dissolvings are heated to, filtering obtains filtrate I；
(b) under agitation, 0~100 DEG C of keeping temperature (preferably 30~50 DEG C), ammonium hydrogen carbonate is added into filtrate I
Or sodium acid carbonate, to (preferably pH 6.5~7.5) during pH 5~8, stop adding ammonium hydrogen carbonate or sodium acid carbonate, sediment is with pure
After water washing, filtering obtains the carbonate deposition of scandium；
(c) 1~10mol/L acetic acid is added into the carbonate deposition of scandium, acetic acid addition is with 1~3 times of theoretical amount
Add, after dissolving, filtering obtains filtrate II；
(d) 70~100 DEG C of II constant temperature of heating filtrate, filtrate II has after crystal precipitation, adds in glacial acetic acid, control solution
Acetic acid concentration is 1~10mol/L (preferably 2~6mol/L), and 5~30min of constant temperature, crystal is filtered while hot, and is washed with absolute ethyl alcohol
Wash；
(e) crystal is dried at 40~200 DEG C, obtains high-pure anhydrous acetic acid scandium；Crystal is obtained in 400~600 DEG C of calcinations
High-purity Sc Oxide；
(f) by high-pure anhydrous acetic acid scandium calcination at 400~600 DEG C of gained, or in the case of logical oxygen self- propagating is carried out
Burning, obtains High-purity Sc Oxide.
Further, in step (a), described strong acid is hydrochloric acid or nitric acid.
Further, in step (b), sediment pure water 2~3 times.
The present invention is using thick scandium oxide as raw material, after acid dissolving, is precipitated with ammonium hydrogen carbonate or sodium acid carbonate, sediment is scrubbed
Afterwards, the acetate solution that acetic acid becomes scandium is added, separates out crystal by heating, crystal calcination obtains High-purity Sc Oxide,
Crystal drying obtains high-pure anhydrous acetic acid scandium, high-pure anhydrous acetic acid scandium calcination or carries out self-propagating combustion in the case of logical oxygen and obtains
High-purity Sc Oxide.
The advantage of the invention is that according to solubility under the acetate high temperature of Rare Earth Impurities In Scandium Oxide and non-rare earth impurity
Big property, can once reduce Rare Earth Impurities In Scandium Oxide and non-rare earth impurity.Solution acidity is low in whole process of the present invention, after
Continuous step consumption amount of reagent is few, and the sewage of discharge is accordingly few, and agents useful for same is weak acid and weak base, and obtained waste water is essentially neutrality
Waste water, processing is easy；Obtained precipitate particles are larger, short texture, and the rate of filtration is fast, it is easy to wash, and saves the time.
Brief description of the drawings
Fig. 1 is process chart of the invention；
Fig. 2 is the heating differential analysis figure of the gained anhydrous acetic acid scandium of the embodiment of the present invention 2.
Embodiment
The invention will be further described with reference to embodiments.
Embodiment 1
Thick scandium oxide raw material 100g (with respect to Purity of Rare Earth 99.91%, non-rare earth impurity 1.2%) is taken, 6mol/L salt is added
Sour 260ml, is heated to 80 DEG C of dissolvings, and filtering obtains filtrate I；Under agitation, 30 DEG C of keeping temperature, carbon is added into filtrate I
Sour hydrogen ammonium, during to pH 6.5, stop add ammonium hydrogen carbonate, with pure water sediment twice after, filtering；By theoretical amount 1 again to
4mol/L acetic acid is added in sediment, stirring and dissolving, 25 DEG C of temperature after reaction, is filtered, and collects filtrate II, and the stirring of filtrate II adds
Heat has the precipitation of acetic acid scandium crystal, adds glacial acetic acid to 100 DEG C, and it is 1mol/L to control acetic acid concentration in solution, in 100 DEG C of situations
Lower constant temperature 5min, is filtered while hot, and acetic acid scandium crystal is washed twice with absolute ethyl alcohol；Crystal is dried at 100 DEG C, obtains high-pure anhydrous
Acetic acid scandium, high-pure anhydrous acetic acid scandium obtains High-purity Sc Oxide (with respect to Purity of Rare Earth 99.999%, non-rare earth in 600 DEG C of calcination 1h
Impurity 0.01%).
Embodiment 2
Thick scandium oxide raw material 100g (with respect to Purity of Rare Earth 99.5%, non-rare earth impurity 1.5%) is taken, 6mol/L nitric acid is added
260ml, is heated to 90 DEG C of dissolvings, and filtering obtains filtrate I；Under agitation, 50 DEG C of keeping temperature, carbonic acid is added into filtrate I
Hydrogen ammonium, during to pH 7.5, stops adding ammonium hydrogen carbonate, after being precipitated three times with pure water, filtering；By theoretical amount 1.2 again to heavy
6mol/L acetic acid is added in shallow lake, stirring and dissolving, 20 DEG C of temperature after reaction, filters, collects filtrate II, filtrate II is heated with stirring to
95 DEG C, there is the precipitation of acetic acid scandium crystal, then glacial acetic acid is added into solution, it is 2mol/L, constant temperature to control acetic acid concentration in solution
10min, is filtered while hot, and precipitation is washed three times with absolute ethyl alcohol, 80 DEG C of baking 2h of acetic acid acid scandium, anhydrous acetic acid scandium is obtained, in logical oxygen
In the case of, light and High-purity Sc Oxide is obtained after anhydrous acetic acid scandium, burning (with respect to Purity of Rare Earth 99.998%, non-rare earth impurity
0.011%).
Embodiment 3
Thick scandium oxide raw material 100g (with respect to Purity of Rare Earth 99.95%, non-rare earth impurity 0.92%) is taken, 5mol/L salt is added
Sour 260ml, is heated to 100 DEG C of dissolvings, and filtering obtains filtrate I；Under agitation, 40 DEG C of keeping temperature, are added into filtrate I
Sodium acid carbonate, during to pH 7.0, stops adding sodium acid carbonate, precipitation is washed with water three times, filtering；By theoretical amount 1.5 again to heavy
5mol/L acetic acid is added in shallow lake, stirring and dissolving, temperature 45 C after reaction, filters, collects filtrate II, filtrate II is heated with stirring to
90 DEG C, there is the precipitation of acetic acid scandium crystal, glacial acetic acid is added into solution, control acetic acid solubility for 4mol/L, constant temperature 15min, while hot
Filtering, precipitation is washed four times with absolute ethyl alcohol, and acetic acid scandium obtains High-purity Sc Oxide (with respect to Purity of Rare Earth in 550 DEG C of calcination 2h
99.999%, non-rare earth impurity 0.0091%).
Solubility of the acetic acid scandium of table 1 under different acetic acid molar concentrations
| Acetic acid concentration (mol/L) | 1 | 2 | 3 | 4 | 5 | 6 | 7 |
| Acetic acid scandium solubility g/L | 11.11 | 9.51 | 8.07 | 7.11 | 6.07 | 5.27 | 4.55 |
Claims (5)
1. the preparation method of a kind of high-pure anhydrous acetic acid scandium and High-purity Sc Oxide, it is characterised in that comprise the following steps：
(a) thick scandium oxide is taken, strong acid is added, 60~100 DEG C of dissolvings are heated to, filtering obtains filtrate I；
(b) under agitation, 0~100 DEG C of keeping temperature, ammonium hydrogen carbonate or sodium acid carbonate are added into filtrate I, to pH 5~
When 8, stop adding after ammonium hydrogen carbonate or sodium acid carbonate, sediment pure water, filtering obtains the carbonate deposition of scandium；
(c) 1~10mol/L acetic acid is added into the carbonate deposition of scandium, acetic acid addition is added with 1~3 times of theoretical amount,
After dissolving, filtering obtains filtrate II；
(d) 70~100 DEG C of II constant temperature of heating filtrate, filtrate II has after crystal precipitation, adds acetic acid in glacial acetic acid, control solution
Concentration is 1~10mol/L, and 5~30min of constant temperature, crystal is filtered while hot, collects crystal and is washed with absolute ethyl alcohol；
(e) crystal is dried at 40~200 DEG C, obtains high-pure anhydrous acetic acid scandium；
(f) by high-pure anhydrous acetic acid scandium calcination at 400~600 DEG C of gained, or in the case of logical oxygen self-propagating combustion is carried out,
Obtain High-purity Sc Oxide.
2. the preparation method of high-pure anhydrous acetic acid scandium according to claim 1 and High-purity Sc Oxide, it is characterised in that step
(a) in, described strong acid is hydrochloric acid or nitric acid.
3. the preparation method of high-pure anhydrous acetic acid scandium according to claim 1 or 2 and High-purity Sc Oxide, it is characterised in that
In step (b), 30~50 DEG C are maintained the temperature at, ammonium hydrogen carbonate or sodium acid carbonate are added into filtrate I.
4. the preparation method of high-pure anhydrous acetic acid scandium according to claim 1 or 2 and High-purity Sc Oxide, it is characterised in that
In step (b), sediment pure water 2~3 times.
5. the preparation method of high-pure anhydrous acetic acid scandium according to claim 1 or 2 and High-purity Sc Oxide, it is characterised in that
In step (d), it is 2~6mol/L to control acetic acid concentration in solution.
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| SU798044A1 (en) * | 1976-12-07 | 1981-01-23 | Белорусский Технологический Инсти-Тут Им.C.M.Кирова | Linear displacement-to-code converter |
| CN1005565B (en) * | 1987-12-12 | 1989-10-25 | 广西冶金研究所 | Method for extracting scandium oxide from artificial rutile |
| CN1009077B (en) * | 1988-03-18 | 1990-08-08 | 东南大学 | Method and equipment for dissolving scandia in hn03 |
| CN1032871C (en) * | 1990-11-07 | 1996-09-25 | 北京有色金属研究总院 | Method of extracting and separating zirconium from scandium oxide |
| RU2040471C1 (en) * | 1992-06-25 | 1995-07-25 | Юлия Васильевна Соколова | Method of preparing 99%-th scandium oxide from the fluoride concentrate |
| RU2069181C1 (en) * | 1993-07-23 | 1996-11-20 | Научно-производственная экологическая фирма "Экотехнология" | Process for preparing scandium oxide |
| JP3428292B2 (en) * | 1996-04-26 | 2003-07-22 | 大平洋金属株式会社 | Sc metal recovery method |
| RU2247788C1 (en) * | 2003-06-24 | 2005-03-10 | Институт химии твердого тела Уральского отделения Российской Академии наук | Method for preparation of scandium oxide from red mud |
| WO2005060610A2 (en) * | 2003-12-11 | 2005-07-07 | The Trustees Of Columbia University In The City Ofnew York | Nano-sized particles, processes of making, compositions and uses thereof |
| UA98118C2 (en) * | 2006-08-17 | 2012-04-25 | Х.К. Штарк Гмбх | Powdery zirconium oxide, method for its production and use, mold, substrate and fuel cell, containing it |
| CN100588615C (en) * | 2007-08-02 | 2010-02-10 | 复旦大学 | Process for preparing water-soluble rare earth nano material |
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| CN102863004A (en) * | 2011-07-05 | 2013-01-09 | 北京有色金属研究总院 | Purification and preparation method of high-purity scandium oxide |
| CN104229744B (en) * | 2014-08-26 | 2016-05-11 | 洛阳市方德新材料科技有限公司 | The preparation method of nanometer metal oxide powder |
| CN104760986B (en) * | 2015-04-07 | 2017-01-04 | 杨秋良 | A kind of process for refining and purifying of high-purity scandium oxide |
| US10029920B2 (en) * | 2015-06-25 | 2018-07-24 | Iowa State University Research Foundation, Inc. | Separation of terbium(III,IV) oxide |
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Denomination of invention: A preparation method for high-purity anhydrous scandium acetate and high-purity scandium oxide Effective date of registration: 20230731 Granted publication date: 20170825 Pledgee: Yiyang Ziyang sub branch of industrial and Commercial Bank of China Ltd. Pledgor: YIYANG HONGYUAN RARE EARTH Co.,Ltd. Registration number: Y2023980050420 |
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