CN103708553A - Method for improving industrial-grade ammonium vanadate quality - Google Patents
Method for improving industrial-grade ammonium vanadate quality Download PDFInfo
- Publication number
- CN103708553A CN103708553A CN201310730775.XA CN201310730775A CN103708553A CN 103708553 A CN103708553 A CN 103708553A CN 201310730775 A CN201310730775 A CN 201310730775A CN 103708553 A CN103708553 A CN 103708553A
- Authority
- CN
- China
- Prior art keywords
- vanadate
- ammonium meta
- technical grade
- grade ammonium
- quality
- 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
Landscapes
- Inorganic Compounds Of Heavy Metals (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a method for improving industrial-grade ammonium vanadate quality. The method comprises the following steps: by taking industrial-grade ammonium vanadate as a raw material, dissolving in low-concentration ammonium hydroxide; removing impurities by ammonium sulfate; adsorbing collected feed liquid by strongly basic anion exchange resin, and adding ammonium chloride to dissolve; separating out crystal under cooling; filtering, washing and drying, so as to obtain the ammonium vanadate with improved quality. Impurities metal ions can be effectively removed by using ammonium sulfate edulcoration; new impurities metal ions are avoided; the quality of the final product is ensured by absorption of the strongly basic anion exchange resin; the content of the impurity metal ions in the obtained ammonium vanadate is lower than 5ppm; the purity of the ammonium vanadate can be up to 99.5% or more after the quality is improved; the product quality can be up to the standard of the HG/T3445-2003 reagent-grade ammonium vanadate. Therefore, the method is applicable to industrial production.
Description
Technical field
The present invention relates to a kind of method that promotes technical grade ammonium meta-vanadate quality, particularly a kind of ammonium sulfate removal of impurities, method of strongly basic anion exchange resin absorption lifting ammonium meta-vanadate quality utilized.
Background technology
Ammonium meta-vanadate is a kind of broad-spectrum inorganic salt, and mainly, as chemical reagent, catalyzer, siccative, mordant etc., ceramic industry is widely used as glaze, and ammonium meta-vanadate is the raw material of synthetic high purity vanadic anhydride still.Therefore along with scientific and technical development, more harsh to the quality control requirement of ammonium meta-vanadate, developing SILVER REAGENT ammonium meta-vanadate, to promote the quality of ammonium meta-vanadate product imperative.
Conventional ammonium meta-vanadate industrial process has two kinds: the one, adopt alkaline hydrolysis, vanadium iron powder is mixed with wood charcoal powder and carried out after roasting, generate vanadic acid sodium with liquid caustic soda effect, the clear liquid that filtration is obtained, through concentrated, filtration, neutralization, crystallization, prepares ammonium meta-vanadate; The 2nd, from navajoite, extract trivalent, tetravalence containing vanadic salts class, by processing such as oxidation, extraction, absorption, neutralization, crystallizatioies, prepare quality-improving ammonium meta-vanadate, but the ammonium meta-vanadate that this method obtains is vulnerable to the impact of initial feed, water quality and the limitation of production technique in preparation process, foreign metal ion content in product is higher, and the quality of ammonium meta-vanadate is difficult to get a promotion.
In prior art, the purifying of technical grade ammonium meta-vanadate is adopted to absorption method and impurity removal method conventionally.
It is raw material that Chinese patent CN102430266A be take containing vanadium solution, adopt acidic cation-exchange resin absorption impurity, then with ammoniacal liquor, regulate pH value, add bicarbonate of ammonia to make ammonium meta-vanadate crystallization, reach the object that promotes technical grade ammonium meta-vanadate quality, but it is higher to adopt in the ammonium meta-vanadate product obtaining in this way foreign metal ion.
Chinese patent CN102531054A, CN102730757A be take technical grade ammonium meta-vanadate as raw material, after dissolving, add the cleaners such as magnesium chloride, calcium chloride, nitrocalcite, magnesium sulfate, then crystallization obtains ammonium meta-vanadate product, this method has been introduced new impurity when promoting technical grade ammonium meta-vanadate quality, is difficult to solve the higher problem of foreign metal ion.The target product of above-mentioned two pieces of patents is all with Vanadium Pentoxide in FLAKES, and ammonium meta-vanadate, as intermediate, does not have concrete analytical data.
Summary of the invention
The object of the present invention is to provide a kind of method that promotes technical grade ammonium meta-vanadate quality, to overcome prior art, to promote in ammonium meta-vanadate quality foreign metal ion content higher, the deficiency that ammonium meta-vanadate purity is on the low side.
Technical conceive of the present invention is such:
Take technical grade ammonium meta-vanadate as raw material, in lower concentration ammoniacal liquor, dissolve, through ammonium sulfate removal of impurities, after strongly basic anion exchange resin absorption, collect in the feed liquid obtaining and add ammonium chloride to dissolve, cooling lower crystallize out, after filtration, washing, dry, obtains the ammonium meta-vanadate of quality-improving.
Technical scheme of the present invention comprises the steps:
Technical grade ammonium meta-vanadate is dissolved at normal temperatures in the ammoniacal liquor of 2-10wt%, when stirring, add ammonium sulfate, the feed liquid obtaining with 2-4 times of column volume/hour speed pass through strongly basic anion exchange resin, the feed liquid that collection is obtained is warming up to 40-60 ℃, add ammonium chloride, be stirred to chloride leach, be cooled to 0-5 ℃, the crystal of separating out after filtration, washing, air seasoning under the condition of 20-30 ℃, obtain the ammonium meta-vanadate product of quality-improving.
Wherein, the size of described column volume is variable, actual flow velocity is controlled according to the volume change of used resin column, size and the handled reduction of feed volume of general resin column match, being similar to some container water fillings is to control by the speed of container the same according to the flow velocity of tap water, and laboratory and factory column volume used differs larger, in addition different resins post, due to material difference, cause actual flow velocity to have very big-difference, in actually operating, conventionally according to actual column volume size, adjust.
Wherein, described technical grade ammonium meta-vanadate is the ammonium meta-vanadate that meets GB7315-87 standard.
Further, described technical grade ammonium meta-vanadate and the mass volume ratio of 2-10wt% ammoniacal liquor are 1:20-30, g/ml, the mass ratio of technical grade ammonium meta-vanadate and ammonium sulfate is 1:0.02-0.10, g/g, wherein strongly basic anion exchange resin is macroporous type strongly basic anion exchange resin, preferred resin model is D201, the mass ratio of technical grade ammonium meta-vanadate and ammonium chloride is 1:2-5, g/g.
The present invention adopts the 2-10wt% ammonia scrubbing 2 times of 0-5 ℃ in washing process, the high purity water that adopts again 0-5 ℃ of specific impedance to be greater than 17M Ω cm washs 2 times, technical grade ammonium meta-vanadate is 1:2-3 with wash at every turn with the mass volume ratio of ammoniacal liquor, g/ml, technical grade ammonium meta-vanadate and to wash be 1:2-3 with the mass volume ratio of high purity water at every turn, g/ml.
The inventive method promotes the product that ammonium meta-vanadate quality obtains and adopts ICP-MS to analyze, the content of foreign metal ion below 5ppm, ammonium meta-vanadate purity reach 99.5% and more than, reach the standard of HG/T3445-2003 SILVER REAGENT ammonium meta-vanadate.
The present invention's beneficial effect compared with prior art:
Technical grade ammonium meta-vanadate raw material of the present invention adds a small amount of ammonium sulfate effectively to remove foreign metal ion as cleaner while dissolving in lower concentration ammoniacal liquor (2-10wt%), does not introduce new foreign metal ion simultaneously, has promoted the quality of ammonium meta-vanadate.
The inventive method adopts strongly basic anion exchange resin to adsorb in the feed liquid obtaining to add ammonium chloride to dissolve, crystallize out under the low temperature of 0-5 ℃, guaranteed the quality of the finished product, analytical results shows that impurity-eliminating effect is obvious, the content of foreign metal ion is all lower than 5ppm, after quality-improving the purity of ammonium meta-vanadate 99.5% and more than, reach the standard of HG/T3445-2003 SILVER REAGENT ammonium meta-vanadate.
Strongly basic anion exchange resin used in the present invention can be recycled through regeneration, meets the requirement of green chemical industry.
The inventive method is easy and simple to handle, good impurity removing effect, and the ammonium meta-vanadate constant product quality obtaining, is suitable for suitability for industrialized production.
Embodiment
Below by specific embodiment, the present invention is described further, but embodiment does not limit the scope of the invention.
Embodiment 1
100g technical grade ammonium meta-vanadate is dissolved in the ammoniacal liquor of 2000ml10wt% at normal temperatures, under stirring, add 2g ammonium sulfate, feed liquid with 2 times of column volumes/hour speed by D201 type strongly basic anion exchange resin post, adsorb, feed liquid after absorption is warming up to 40 ℃, under stirring, add 200g ammonium chloride, after dissolving, be cooled to 5 ℃, the crystal of separating out adopts the 10wt% ammonia scrubbing 2 times of 5 ℃ successively after filtering, 20ml/ time, then the high purity water that adopts 5 ℃ of specific impedances to be greater than 17M cm washs 2 times, 200ml/ time, the solid formation obtaining air seasoning under the condition of 20-30 ℃, obtain the ammonium meta-vanadate product 84g of quality-improving.
Embodiment 2
100g technical grade ammonium meta-vanadate is dissolved in the ammoniacal liquor of 3000ml2wt% at normal temperatures, under stirring, add 10g ammonium sulfate, feed liquid with 4 times of column volumes/hour speed by D201 type strongly basic anion exchange resin post, adsorb, feed liquid after absorption is warming up to 50 ℃, under stirring, add 500g ammonium chloride, after dissolving, be cooled to 0 ℃, the crystal of separating out adopts the 2wt% ammonia scrubbing 2 times of 0 ℃ successively after filtering, then the high purity water that adopts for 30ml/ time 0 ℃ of specific impedance to be greater than 17M Ω cm washs 2 times, 300ml/ time, the solid formation obtaining air seasoning under the condition of 20-30 ℃, obtain the ammonium meta-vanadate product 81g of quality-improving.
Result shows, products obtained therefrom meets the standard of HG/T3445-2003 SILVER REAGENT ammonium meta-vanadate, and the content of foreign metal ion is all below 5ppm.Embodiment detected result is as follows:
| Test item | Standard value | Embodiment 1 | Embodiment 2 |
| Content (NH 4VO 3)，% | ≥99.0 | 99.6 | 99.8 |
| Clarity test | Qualified | Qualified | Qualified |
| Muriate (Cl), % | ≤0.005 | 0.0005 | 0.0003 |
| Vitriol (SO 4)，% | ≤0.01 | 0.0004 | 0.0002 |
| Iron (Fe), % | ≤0.005 | 0.0002 | 0.0001 |
| Sodium (Na), ppm | — | 5 | 4 |
| Calcium (Ca), ppm | — | 4 | 5 |
| Magnesium (Mg), ppm | — | 2 | 3 |
| Manganese (Mn), ppm | — | 3 | 1 |
| Zinc (Zn), ppm | — | 4 | 2 |
| Plumbous (Pb), ppm | — | 2 | 1 |
| Copper (Cu), ppm | — | 3 | 1 |
| Chromium (Cr), ppm | — | 1 | 1 |
| Titanium (Ti), ppm | — | 1 | 1 |
| Molybdenum (Mo), ppm | — | 2 | 1 |
It should be noted that, above embodiment is only unrestricted in order to technical scheme of the present invention to be described.Although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement the technical scheme of invention, and not depart from the scope of technical solution of the present invention, it all should be encompassed in claim scope of the present invention.
Claims (9)
1. promote a method for technical grade ammonium meta-vanadate quality, it is characterized in that comprising the steps:
Technical grade ammonium meta-vanadate is dissolved in 2-10wt% ammoniacal liquor at normal temperatures, when stirring, add ammonium sulfate, the feed liquid obtaining with 2-4 times of column volume/hour speed pass through strongly basic anion exchange resin, the feed liquid obtaining is warming up to 40-60 ℃, add ammonium chloride, be stirred to chloride leach, be cooled to 0-5 ℃, the crystal of separating out after filtration, air seasoning under the condition of washing, 20-30 ℃, obtain the ammonium meta-vanadate of quality-improving.
2. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described technical grade ammonium meta-vanadate is the ammonium meta-vanadate that meets GB7315-87 standard.
3. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described technical grade ammonium meta-vanadate and the mass volume ratio of 2-10wt% ammoniacal liquor are 1:20-30, g/ml.
4. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described technical grade ammonium meta-vanadate and the mass ratio of ammonium sulfate are 1:0.02-0.10, g/g.
5. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described strongly basic anion exchange resin is macroporous type strongly basic anion exchange resin, and resin model is D201.
6. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described technical grade ammonium meta-vanadate and the mass ratio of ammonium chloride are 1:2-5, g/g.
7. the method for lifting technical grade ammonium meta-vanadate quality according to claim 1, is characterized in that, described washing adopts the 2-10wt% ammonia scrubbing 2 times of 0-5 ℃, then adopts 0-5 ℃ of specific impedance to be greater than the high purity water washing 2 times of 17M Ω .cm.
8. according to the method for the lifting technical grade ammonium meta-vanadate quality described in claim 1 or 7, it is characterized in that, described technical grade ammonium meta-vanadate is 1:2-3 with wash at every turn with the mass volume ratio of ammoniacal liquor, g/ml.
9. according to the method for the lifting technical grade ammonium meta-vanadate quality described in claim 1 or 7, it is characterized in that, described technical grade ammonium meta-vanadate is 1:2-3 with wash at every turn with the mass volume ratio of high purity water, g/ml.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310730775.XA CN103708553B (en) | 2013-12-26 | 2013-12-26 | A kind of method promoting technical grade ammonium meta-vanadate quality |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310730775.XA CN103708553B (en) | 2013-12-26 | 2013-12-26 | A kind of method promoting technical grade ammonium meta-vanadate quality |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103708553A true CN103708553A (en) | 2014-04-09 |
| CN103708553B CN103708553B (en) | 2016-01-06 |
Family
ID=50401956
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310730775.XA Active CN103708553B (en) | 2013-12-26 | 2013-12-26 | A kind of method promoting technical grade ammonium meta-vanadate quality |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103708553B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298461A (en) * | 2017-08-17 | 2017-10-27 | 芜湖人本合金有限责任公司 | The method of purification of ammonium metavanadate and high-purity ammonium metavanadate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430266A (en) * | 2010-09-29 | 2012-05-02 | 攀钢集团钢铁钒钛股份有限公司 | Method for purifying liquid with vanadium and method for preparing ammonium metavanadate and vanadium oxide |
| CN102531054A (en) * | 2010-12-27 | 2012-07-04 | 邓时胜 | Purification method of ammonium metavanadate and preparation method of high-purity vanadium pentoxide |
| CN102730757A (en) * | 2011-04-03 | 2012-10-17 | 崇阳县恒通工贸有限公司 | Method for preparing high purity vanadium pentoxide through using ammonium metavanadate |
-
2013
- 2013-12-26 CN CN201310730775.XA patent/CN103708553B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102430266A (en) * | 2010-09-29 | 2012-05-02 | 攀钢集团钢铁钒钛股份有限公司 | Method for purifying liquid with vanadium and method for preparing ammonium metavanadate and vanadium oxide |
| CN102531054A (en) * | 2010-12-27 | 2012-07-04 | 邓时胜 | Purification method of ammonium metavanadate and preparation method of high-purity vanadium pentoxide |
| CN102730757A (en) * | 2011-04-03 | 2012-10-17 | 崇阳县恒通工贸有限公司 | Method for preparing high purity vanadium pentoxide through using ammonium metavanadate |
Non-Patent Citations (2)
| Title |
|---|
| 侯海军: ""高纯偏钒酸铵的制备技术研究"", 《钢铁钒钛》, vol. 34, no. 3, 30 June 2013 (2013-06-30), pages 29 - 32 * |
| 李静等: ""硫酸镁去除工业偏钒酸铵中磷和硅的研究"", 《广州化工》, vol. 40, no. 22, 30 November 2012 (2012-11-30) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107298461A (en) * | 2017-08-17 | 2017-10-27 | 芜湖人本合金有限责任公司 | The method of purification of ammonium metavanadate and high-purity ammonium metavanadate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103708553B (en) | 2016-01-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101973871B (en) | Electronic grade citric acid and production method thereof | |
| CN106430307B (en) | A kind of high purity vanadic anhydride preparation method | |
| CN104805303B (en) | A kind of method that vanadium chromium slag acid system synchronously reclaims vanadium chromium | |
| CN104404274B (en) | A kind of method from reclaiming vanadium containing precipitate and separate vanadium solution | |
| CN104058456A (en) | Ammonium metavanadate preparation method | |
| CN102336437A (en) | Process for producing vanadium pentoxide by vanadium-contained solution | |
| CN106987732A (en) | A kind of method for separating and recovering vanadium chromium | |
| CN104692461A (en) | Method for preparing high-purity powdered vanadium oxide | |
| CN102295308A (en) | Method for preparing zinc oxide by using zinc-containing waste liquid as raw material | |
| CN105366722B (en) | The method of normal temperature extraction production high purity vanadic anhydride | |
| CN1850623A (en) | Method for producing ammonium molybdate from high-impurity ferro-molybdenum | |
| CN112607777A (en) | Production process of ammonium molybdate | |
| CN103014377B (en) | Vanadium liquid purification method | |
| CN103708553B (en) | A kind of method promoting technical grade ammonium meta-vanadate quality | |
| CN109161701A (en) | The method that vanadium manganese solution separates, recycles vanadium manganese | |
| CN105060332A (en) | Iron-removal easy-filtering process for copper sulfate solution | |
| CN111717930A (en) | Method for producing basic copper carbonate based on copper-containing etching waste liquid | |
| CN114477282B (en) | Method for preparing low-silicon red cakes through reduction, hydrolysis, vanadium precipitation and desilication | |
| CN1326772C (en) | Production method of medical sodium iodide | |
| CN101016171A (en) | Preparation process for high-purity alpha-Fe2O3 by ferrous sulfate-ammonium carbonate method | |
| CN105621495A (en) | Method for preparing high purity iron oxide red from picking waste liquid | |
| CN104694769B (en) | A kind of production method of clean vanadium liquid | |
| JP2013245159A (en) | Method for comprehensively treating claus tail gas and producing manganese sulfate | |
| CN110004292B (en) | Process for purifying waste manganese sulfate solution to reduce content of calcium and magnesium | |
| CN106892455A (en) | The green clean method for preparing of vanadium compounds |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |