CN107298462A - A kind of method of the high purity molybdate from rough sodium molybdate solution - Google Patents
A kind of method of the high purity molybdate from rough sodium molybdate solution Download PDFInfo
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- CN107298462A CN107298462A CN201710530123.XA CN201710530123A CN107298462A CN 107298462 A CN107298462 A CN 107298462A CN 201710530123 A CN201710530123 A CN 201710530123A CN 107298462 A CN107298462 A CN 107298462A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/003—Preparation involving a liquid-liquid extraction, an adsorption or an ion-exchange
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- 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
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Abstract
The invention discloses a kind of method of the high purity molybdate from rough sodium molybdate solution, mainly include：Proper inorganic acid is added into rough sodium molybdate solution and carries out an acid adjustment, solution adjusts pH value to 45, stirs 5min；Add appropriate transition additive, stirring mixing 10min；The secondary acid adjustment of proper inorganic acid is added, solution adjusts pH to 12, stirs evenly 20 30min；Centrifugal filtration is carried out, obtained solid is washed with cleaning solution, then filtered again, dry obtained solid and produce high-purity molybdate；Centrifugal filtration liquid and cleaning solution alkalescent macropore negative resin are adsorbed, and reclaim valuable metal molybdenum.The present invention can realize that molybdenum and calcium in rough sodium molybdate solution, magnesium are efficiently separated, high purity molybdate.
Description
Technical field
The present invention relates to metallurgy of rare metal field, and in particular to one kind efficiently separated from rough sodium molybdate solution molybdenum and
Calcium, magnesium, and then the method for high purity molybdate.
Background technology
China is tungsten resource big country, but low molybdenum with high-quality, the increasingly reduction of the black tungsten resource of low impurity, Chinese tungsten
Raw materials for production center of gravity is gradually transferred to the tungsten ore resource containing high molybdenum, high impurity and utilizes field by molybdenum enterprise, and tungsten separation is difficult
The problem of being urgent need to resolve.With the breakthrough of technology in recent years, using primary amine as extractant, using solvent-extracted method, tungsten is realized
The technique of molybdenum separation is gradually ripe.Extraction process processing using the high molybdenum sodium tungstate solution of calcic, magnesium to extract during stoste, can be with
The separation of tungsten is realized, but can not carry out effectively removing the impurity such as calcium, magnesium, causes the product such as the sodium molybdate in later stage impurity to surpass
Mark, influences product quality.
The content of the invention
In view of the shortcomings of the prior art, the present invention is intended to provide one kind high purity molybdate from rough sodium molybdate solution
Method, molybdenum and calcium, magnesium can be separated, the molybdic acid product salt of high purity efficiently from rough sodium molybdate solution.
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of method of the high purity molybdate from rough sodium molybdate solution, comprises the following steps：
S1 takes rough sodium molybdate solution to be placed in glass beaker, plus inorganic acid regulation solution ph is 4-5, and stirring is obtained
Solution after preliminary acid adjustment；
The solution that S2 adds the additive that makes the transition after the preliminary acid adjustment obtained in step S1, is mixed；
S3 adds inorganic acid in the addition transition additive obtained in step S2 and the solution mixed, pH value of solution
Value control is 1-2, stirring；
The solution finally given in step S3 is carried out centrifugal filtration by S4, then with consolidating that cleaning solution is obtained to centrifugal filtration
Body is washed, and is filtered again, dries the solid being filtrated to get, as high-purity molybdate；Collect centrifugal filtration liquid and washing
Liquid, with the valuable metal molybdenum in alkalescent macropore negative resin adsorption recovery centrifugal filtration liquid and cleaning solution.
Further, in step S1, inorganic acid system includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.Stirring when
Between be 5min, temperature is 298K, and the speed of stirring is 50-80r/min.
Further, in step S2, the transition additive includes one kind or several in ammonium chloride, ammonium nitrate, ammonium sulfate
Kind.Make the transition the 2-10% that additive addition is molybdenum quality, and reaction temperature is 298K, and the time of stirring is 10min, the speed of stirring
Spend for 50-80r/min.
Further, the inorganic acid system used in step S3 includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.Stir
The time mixed is 20-30min, and temperature is 298K, and the speed of stirring is 50-80r/min.
Further, in step S4, the time of centrifugal filtration is 20min, and the rotating speed of centrifugation is 800-1000r/min.Wash
The acetum that liquid is the 5-10% that pH value is 2-3 is washed, cleaning solution consumption volume is using rough sodium molybdate solution as reference, about
The 5-10% of rough sodium molybdate solution volume.Drying uses drying baker, and temperature control is in 363-373K, and the time is 12h.
The beneficial effects of the present invention are：Solution ph is adjusted using inorganic acid, after solution ph stabilizes to 4-5, then
Appropriate transition additive is added, transition additive is mixed in solution, continuously adds inorganic acid, when solution ph reaches 1-2,
The molybdenum in reaction time, solution is controlled to start transition, reaction is completed, centrifugal filtration, the molybdenum in solution is sunk in the form of molybdate
Shallow lake is come out, and the calcium, magnesium in solution are stayed in filtrate in the form of divalent calcium ions, divalence magnesium ion, so as to realize rough molybdenum
Molybdenum and calcium in acid sodium solution, magnesium are efficiently separated, so as to realize the molybdic acid product salt of high purity.
Embodiment
The invention will be further described below, it is necessary to which explanation, following examples are using the technical program before
Carry, give detailed embodiment and specific operating process, but the scope of the present invention is not limited to the present embodiment.
A kind of method of the high purity molybdate from rough sodium molybdate solution, comprises the following steps：
S1 takes rough sodium molybdate solution to be placed in glass beaker, plus inorganic acid regulation solution ph is 4-5, and stirring is obtained
Solution after preliminary acid adjustment；
The solution that S2 adds the additive that makes the transition after the preliminary acid adjustment obtained in step S1, is mixed；
S3 adds inorganic acid in the addition transition additive obtained in step S2 and the solution mixed, pH value of solution
Value control is 1-2, stirring；
The solution finally given in step S3 is carried out centrifugal filtration by S4, then with consolidating that cleaning solution is obtained to centrifugal filtration
Body is washed, and is filtered again, dries the solid being filtrated to get, as high-purity molybdate；Collect centrifugal filtration liquid and washing
Liquid, with the valuable metal molybdenum in alkalescent macropore negative resin adsorption recovery centrifugal filtration liquid and cleaning solution.
Further, in step S1, inorganic acid system includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.Stirring when
Between be 5min, temperature is 298K, and the speed of stirring is 50-80r/min.
Further, in step S2, the transition additive includes one kind or several in ammonium chloride, ammonium nitrate, ammonium sulfate
Kind.Make the transition the 2-10% that additive addition is molybdenum quality, and reaction temperature is 298K, and the time of stirring is 10min, the speed of stirring
Spend for 50-80r/min.
Further, the inorganic acid system used in step S3 includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.Stir
The time mixed is 20-30min, and temperature is 298K, and the speed of stirring is 50-80r/min.
Further, in step S4, the time of centrifugal filtration is 20min, and the rotating speed of centrifugation is 800-1000r/min.Wash
The acetum that liquid is the 5-10% that pH value is 2-3 is washed, cleaning solution consumption volume is using rough sodium molybdate solution as reference, about
The 5-10% of rough sodium molybdate solution volume.Drying uses drying baker, and temperature control is in 363-373K, and the time is 12h.
Embodiment 1
1. an acid adjustment：Take the rough sodium molybdate solution 500mL obtained after primary amine extract and separate, the Molybdenum in Solution concentration
For 80g/L, calcium ion concentration is 0.05g/L, and magnesium ion concentration is 0.002g/L.Adding hydrochloric acid adjusts pH value to be 4, and mixing speed is
80r/min, mixing time 5min, temperature is 298K.
2. transition additive ammonium chloride is introduced, addition is stirred to test 5% (2g) of molybdenum quality in rough sodium molybdate solution
Speed is mixed for 80r/min, mixing time 10min, temperature is 298K；
3. secondary acid adjustment, transition precipitation：Solution ph is adjusted to be 1 with hydrochloric acid, mixing speed is 80r/min；Mixing time is
20min, temperature is 298K；
4. separation of solid and liquid, centrifugal filtration：Centrifugal filtration is carried out to the solution obtained in 3., centrifuge speed is 800r/
Min, the centrifugal filtration time is 20min；The solid that centrifugal filtration is obtained is washed with cleaning solution, filtered again.Cleaning solution
For 10% acetum, pH value is 2.26.Cleaning solution volume is using rough sodium molybdate solution as reference, and about rough sodium molybdate is molten
10% (50mL) of liquid product.It is 58.77%, calcium to dry molybdenum content in the solid finally obtained, sample preparation detection, high-purity molybdate
Content is 0.0005%, and content of magnesium is 0.0004%.Centrifugal filtration liquid and cleaning solution are collected, molybdenum concentration is 1g/L, uses weak base
Property the absorption of macropore negative resin, reclaim valuable metal molybdenum.
Embodiment 2
1. an acid adjustment：Take the rough sodium molybdate solution 500mL obtained after primary amine extract and separate, the Molybdenum in Solution concentration
For 80g/L, add nitric acid and adjust pH value to be 4, mixing speed is 80r/min, and mixing time 5min, temperature is 298K.
2. transition additive ammonium nitrate is introduced, addition is 10% (4g) for testing molybdenum quality in rough sodium molybdate solution,
Mixing speed is 80r/min, and mixing time 10min, temperature is 298K；
3. secondary acid adjustment, transition precipitation：Solution ph is adjusted to be 1 with nitric acid, mixing speed is 80r/min；Mixing time is
20min, temperature is 298K；
4. separation of solid and liquid, centrifugal filtration：Centrifugal filtration is carried out to the solution finally given in 3., centrifuge speed is
800r/min, the centrifugal filtration time is 20min；The solid that centrifugal filtration is obtained is washed with cleaning solution, filtered again.Wash
Liquid is washed for 8% acetum, pH value is 2.35, cleaning solution volume is 8% (40mL) of filtered fluid volume.Drying final filtration is obtained
Molybdenum content is 62.10% in the solid arrived, sample preparation detection, high-purity molybdate, and calcium content is 0.0003%, and content of magnesium is
0.0005%.Centrifugal filtration liquid and cleaning solution are collected, and molybdenum concentration is 1.1g/L, are adsorbed with alkalescent macropore negative resin, are reclaimed
Valuable metal molybdenum.
Embodiment 3
1. an acid adjustment：Take the rough sodium molybdate solution 500mL obtained after primary amine extract and separate, the Molybdenum in Solution concentration
For 80g/L, it is 4 to add sulfuric acid and adjust the pH value of rough sodium molybdate solution, and mixing speed is 80r/min, mixing time 5min, temperature
Spend for 298K.
2. transition additive ammonium sulfate is introduced, addition is 8% (3.2g) for testing molybdenum quality in rough sodium molybdate solution,
Mixing speed is 80r/min, and mixing time 10min, temperature is 298K；
3. secondary acid adjustment, transition precipitation：The solution ph obtained in being adjusted 2. with sulfuric acid is 2, and mixing speed is 80r/min；
Mixing time is 20min, and temperature is 298K；
4. separation of solid and liquid, centrifugal filtration：Centrifugal filtration is carried out to the solution obtained in 3., centrifuge speed is 800r/
Min, the centrifugal filtration time is 20min.The fixation that centrifugal filtration is obtained is washed with cleaning solution, filtered again.Cleaning solution is 5%
Acetum, pH value is 2.43, and cleaning solution volume is using rough sodium molybdate solution as reference, about rough sodium molybdate solution volume
5% (25mL).It is 61.52% to dry molybdenum content in the solid finally given, sample preparation detection, high-purity molybdate, and calcium content is
0.0003%, content of magnesium is 0.0003%.Centrifugal filtration liquid and cleaning solution are collected, and molybdenum concentration is 1.3g/L, big with alkalescent
Hole negative resin absorption, reclaims valuable metal molybdenum.
Embodiment 4
1. an acid adjustment：Take the rough sodium molybdate solution 500mL obtained after primary amine extract and separate, the Molybdenum in Solution concentration
For 80g/L, the nitration mixture for adding sulfuric acid and hydrochloric acid adjusts pH value to be 4, and mixing speed is 80r/min, mixing time 5min, and temperature is
298K。
2. the mixture of transition additive ammonium sulfate and ammonium chloride is introduced, total addition is in the rough sodium molybdate solution of experiment
10% (ammonium sulfate 2g, ammonium chloride 2g) of molybdenum quality, mixing speed is 80r/min, and mixing time 10min, temperature is 298K；
3. secondary acid adjustment, transition precipitation：Solution ph is adjusted to be 2 with the nitration mixture of sulfuric acid and hydrochloric acid, mixing speed is 80r/
min；Mixing time is 20min, and temperature is 298K；
4. separation of solid and liquid, centrifugal filtration：Solution centrifugal filtering to 3. finally giving, centrifuge speed is 800r/min,
The centrifugal filtration time is 20min.The solid that centrifugal filtration is obtained is washed with cleaning solution, filtered again.Cleaning solution is
10% acetum, pH value is 2.26, and cleaning solution volume is using rough sodium molybdate solution as reference, about rough sodium molybdate solution
10% (50mL) of volume.Molybdenum content is 63.23% in the solid that drying final filtration is obtained, sample preparation detection, high-purity molybdate,
Calcium content is 0.0005%, and content of magnesium is 0.0002%；Centrifugal filtration liquid and cleaning solution are collected, and molybdenum concentration is 1.2g/L, are used
Alkalescent macropore negative resin is adsorbed, and reclaims valuable metal molybdenum.
For those skilled in the art, technical scheme that can be more than and design, provide various corresponding
Change and deform, and all these change and deform, and should be construed as being included within the protection domain of the claims in the present invention.
Claims (10)
1. a kind of method of the high purity molybdate from rough sodium molybdate solution, it is characterised in that：Comprise the following steps：
S1 takes rough sodium molybdate solution to be placed in glass beaker, plus inorganic acid regulation solution ph is 4-5, and stirring obtains preliminary
Solution after acid adjustment；
The solution that S2 adds the additive that makes the transition after the preliminary acid adjustment obtained in step S1, is mixed；
S3 adds inorganic acid in the addition transition additive obtained in step S2 and the solution mixed, solution ph control
1-2 is made as, is stirred；
The solution finally given in step S3 is carried out centrifugal filtration by S4, and then the solid that centrifugal filtration is obtained is entered with cleaning solution
Row washing, is filtered again, dries the solid being filtrated to get, as high-purity molybdate；Centrifugal filtration liquid and cleaning solution are collected, is used
Valuable metal molybdenum in alkalescent macropore negative resin adsorption recovery centrifugal filtration liquid and cleaning solution.
2. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S1, inorganic acid system includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.
3. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that step
In rapid S1, the time of stirring is 5min, and temperature is 298K, and the speed of stirring is 50-80r/min.
4. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S2, the transition additive includes the one or more in ammonium chloride, ammonium nitrate, ammonium sulfate.
5. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S2, transition additive addition is the 2-10% of molybdenum quality, and reaction temperature is 298K, and the time of stirring is 10min, stirring
Speed be 50-80r/min.
6. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
The inorganic acid system used in rapid S3 includes the one or more in sulfuric acid, nitric acid, hydrochloric acid.
7. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S3, the time of stirring is 20-30min, and temperature is 298K, and the speed of stirring is 50-80r/min.
8. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S4, the time of centrifugal filtration is 20min, and the rotating speed of centrifugation is 800-1000r/min.
9. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：Step
In rapid S4, cleaning solution is the acetum for the 5-10% that pH value is 2-3, and cleaning solution consumption volume is to be made with rough sodium molybdate solution
It is the 5-10% of rough sodium molybdate solution volume for reference.
10. the method for the high purity molybdate according to claim 1 from rough sodium molybdate solution, it is characterised in that：
In step S4, drying uses drying baker, and temperature control is in 363-373K, and the time is 12h.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108179288A (en) * | 2017-12-28 | 2018-06-19 | 云南元晟新材料科技有限公司 | A kind of chemical industry metallurgical method for separating of wulfenite |
| CN110937633A (en) * | 2019-12-09 | 2020-03-31 | 天津科技大学 | Preparation method of needle-shaped sodium molybdate dihydrate crystal |
| CN114672670A (en) * | 2022-02-25 | 2022-06-28 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
| CN115072781A (en) * | 2022-05-07 | 2022-09-20 | 成都虹波钼业有限责任公司 | Ammonium tetramolybdate and preparation process thereof |
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| CN1074486A (en) * | 1992-01-18 | 1993-07-21 | 戴元宁 | The chemical sorting method of wulfenite |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108179288A (en) * | 2017-12-28 | 2018-06-19 | 云南元晟新材料科技有限公司 | A kind of chemical industry metallurgical method for separating of wulfenite |
| CN110937633A (en) * | 2019-12-09 | 2020-03-31 | 天津科技大学 | Preparation method of needle-shaped sodium molybdate dihydrate crystal |
| CN110937633B (en) * | 2019-12-09 | 2022-04-12 | 天津科技大学 | Preparation method of needle-shaped sodium molybdate dihydrate crystal |
| CN114672670A (en) * | 2022-02-25 | 2022-06-28 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
| CN114672670B (en) * | 2022-02-25 | 2023-10-10 | 信丰华锐钨钼新材料有限公司 | Method for efficiently precipitating Mo in low-concentration sodium molybdate solution |
| CN115072781A (en) * | 2022-05-07 | 2022-09-20 | 成都虹波钼业有限责任公司 | Ammonium tetramolybdate and preparation process thereof |
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