CN106241871A - High vanadium concentrations liquid acid ammonium salt precipitation method - Google Patents
High vanadium concentrations liquid acid ammonium salt precipitation method Download PDFInfo
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- CN106241871A CN106241871A CN201610557600.7A CN201610557600A CN106241871A CN 106241871 A CN106241871 A CN 106241871A CN 201610557600 A CN201610557600 A CN 201610557600A CN 106241871 A CN106241871 A CN 106241871A
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- ammonium salt
- acid
- ammonium
- high vanadium
- concentrations liquid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The present invention relates to a kind of high vanadium concentrations liquid acid ammonium salt precipitation method, comprise the following steps: a. configures finite concentration ammonium salt solution, and with acid, its pH value is adjusted to 2～3；B. heating, stirring are kept；C. it is slowly added to high vanadium concentrations liquid and acid adding keeps pH value 2～3；D. sustained response filters to precipitation is rear, i.e. obtains ammonium poly-vanadate.The high vanadium concentrations liquid acid ammonium salt precipitation method of the present invention has the advantage that (1) can effectively reduce wastewater flow rate；(2) technique is simple, and precipitation rate and product purity are high.
Description
Technical field
The method that the present invention relates to the precipitation of a kind of chemistry, is specifically related to a kind of for high vanadium concentrations liquid acid ammonium salt precipitation
Method, belongs to chemical field.
Background technology
In existing acid ammonium salt precipitation technique, the height of vanadium liquid concentration affects sedimentary composition, and concentration height is conducive to
The crystal grain of APV is grown up, and accelerates settling velocity.But excessive concentration can bring the problem that precipitation impurity in products is high, permit in general industry
The maximum concentration permitted is 30g/L, often produces 1t vanadic anhydride and will produce the waste water of about 20t.Before raising precipitation, liquid is dense
Degree is to reduce the fundamental way that waste water produces.The inventive method is simple, can effectively reduce vanadium wastewater amount, and to evade heavy simultaneously
The problem that vanadium impurity in products is high, has huge environment, economic benefit.
Summary of the invention
It is an object of the invention to provide a kind of high vanadium concentrations liquid acid ammonium salt precipitation method.
High vanadium concentrations liquid acid ammonium salt precipitation method of the present invention, comprises the following steps:
A. configuration finite concentration ammonium salt solution, and with acid, its pH value is adjusted to 2～3；
B. heating, stirring are kept；
C. it is slowly added to high vanadium concentrations liquid and acid adding keeps pH value 2～3；
D. sustained response filters to precipitation is rear, i.e. obtains ammonium poly-vanadate.
Further illustrating, ammonium salt used by step a includes in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate and ammonium hydrogen carbonate
At least one.
Further illustrating, acid used is at least one in sulphuric acid, hydrochloric acid, nitric acid.
Further illustrating, TV (full vanadium) content in described high vanadium concentrations liquid is not less than 30g/L.
The high vanadium concentrations liquid acid ammonium salt precipitation method of the present invention has the advantage that (1) is due to vanadium liquid dense before precipitation
Degree height, therefore can effectively reduce wastewater flow rate；(2) technique is simple, and precipitation rate is high, and product impurity is low.
Detailed description of the invention
Hereinafter, the high vanadium concentrations liquid acid ammonium salt precipitation side of the exemplary embodiment specific descriptions present invention will be combined
Method.
Method comprises the following steps according to an exemplary embodiment of the present invention:
Step a:
Configuration finite concentration ammonium salt solution, and with acid, its pH value is adjusted to 2～3.
Wherein, ammonium salt used is at least one in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate and ammonium hydrogen carbonate, and it adds
Enter quality and control (ammonium vanadium ratio=ammonium salt weight: vanadium quality in solution) by ammonium vanadium than 1～1.2.
Step b:
Keep heating, stirring.
Step c:
It is slowly added to high vanadium concentrations liquid and acid adding keeps pH value 2～3.
The most continuously stirred and heating, temperature controls boiling for optimum.
Step d:
Sustained response filters to precipitation is rear, i.e. obtains ammonium poly-vanadate.
Wherein, after high vanadium concentrations liquid adds, continue keep reaction 30～60min, in course of reaction Sustainable Control pH=2～
3, heat and stir.
Below in conjunction with concrete example, the detailed description of the invention of the present invention is further described, the most therefore by the present invention
It is limited among described example ranges.Further, unless otherwise noted, the percentage ratio related in this specification is weight percent
Ratio.
Embodiment 1:
Prepare high vanadium concentrations liquid (TV=50g/L) 200ml standby.Weigh 12g ammonium sulfate in 20ml water, fully dissolve also
With sulphuric acid, its pH value is modulated 2.5.Continuously stirred heating, and it is slowly added to the high vanadium concentrations liquid got ready in advance.Continue with sulphuric acid
Control pH value in reaction 2～3.After 200ml vanadium liquid adds completely, continue reaction 60min.Filter, wash, be dried the many vanadium of acquisition
Acid ammonium (APV) 19.91g.The wherein 49.76wt% Han V.
Embodiment 2:
Prepare high vanadium concentrations liquid (TV=38g/L) 200ml standby.Weigh 7.6g ammonium chloride in 10ml water, fully dissolve
And with hydrochloric acid, its pH value is modulated 2.5.Continuously stirred heating, and it is slowly added to the high vanadium concentrations liquid got ready in advance.Hold with hydrochloric acid
The continuous pH value in reaction that controls is 2～3.After 200ml vanadium liquid adds completely, continue reaction 30min.Filter, wash, be dried obtain many
Ammonium vanadate (APV) 15.13g.The wherein 49.71wt% Han V.
Embodiment 3:
Prepare high vanadium concentrations liquid (TV=100g/L) 200ml standby.Weigh 22g ammonium nitrate in 25ml water, fully dissolve
And with nitric acid, its pH value is modulated 2.5.Continuously stirred heating, and it is slowly added to the high vanadium concentrations liquid got ready in advance.Hold with nitric acid
The continuous pH value in reaction that controls is 2～3.After 200ml vanadium liquid adds completely, continue reaction 60min.Filter, wash, be dried obtain many
Ammonium vanadate (APV) 39.75g.The wherein 49.81wt% Han V.
The inventive method can effectively reduce wastewater flow rate, technique is simple, and precipitation rate is high, and product impurity is low.
Although reference be made herein to invention has been described for the explanatory embodiment of the present invention, and above-described embodiment is only this
Bright preferably embodiment, embodiments of the present invention are also not restricted to the described embodiments, it should be appreciated that people in the art
Member can be designed that a lot of other amendments and embodiment, and these amendments and embodiment will fall in principle disclosed in the present application
Within scope and spirit.
Claims (6)
1. high vanadium concentrations liquid acid ammonium salt precipitation method, it is characterised in that comprise the following steps:
A. configuration finite concentration ammonium salt solution, and with acid, its pH value is adjusted to 2～3；
B. heating, stirring are kept；
C. it is slowly added to high vanadium concentrations liquid and acid adding keeps pH value 2～3；
D. sustained response filters to precipitation is rear, i.e. obtains ammonium poly-vanadate.
High vanadium concentrations liquid acid ammonium salt precipitation method the most according to claim 1, it is characterised in that: ammonium salt bag used by step a
Include at least one in ammonium sulfate, ammonium chloride, ammonium nitrate, ammonium carbonate and ammonium hydrogen carbonate.
High vanadium concentrations liquid acid ammonium salt precipitation method the most according to claim 1, it is characterised in that: described acid is sulphuric acid, salt
At least one in acid, nitric acid.
High vanadium concentrations liquid acid ammonium salt precipitation method the most according to claim 1, it is characterised in that: in described high vanadium concentrations liquid
Full content of vanadium not less than 30g/L.
High vanadium concentrations liquid acid ammonium salt precipitation method the most according to claim 1, it is characterised in that: ammonium salt solution and high concentration
Vanadium liquid is according to ammonium salt weight: in solution vanadium quality be 1～1.2 ratio be controlled.
High vanadium concentrations liquid acid ammonium salt precipitation method the most according to claim 1, it is characterised in that: step d reaction 30～
60min, Sustainable Control pH=2～3 in course of reaction, heats and stirs.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610557600.7A CN106241871A (en) | 2016-07-15 | 2016-07-15 | High vanadium concentrations liquid acid ammonium salt precipitation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610557600.7A CN106241871A (en) | 2016-07-15 | 2016-07-15 | High vanadium concentrations liquid acid ammonium salt precipitation method |
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| CN106241871A true CN106241871A (en) | 2016-12-21 |
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| CN201610557600.7A Pending CN106241871A (en) | 2016-07-15 | 2016-07-15 | High vanadium concentrations liquid acid ammonium salt precipitation method |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815547A (en) * | 2017-11-08 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
| CN108190955A (en) * | 2018-03-28 | 2018-06-22 | 河钢股份有限公司承德分公司 | A kind of recovery process of ammonium vanadate sodium production waste water |
| CN109081374A (en) * | 2018-10-19 | 2018-12-25 | 河钢股份有限公司承德分公司 | A method of preparing the spherical ammonium poly-vanadate of big granularity |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
| CN115676886A (en) * | 2022-11-15 | 2023-02-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium precipitation method for reducing vanadium precipitation wastewater by using high-concentration vanadium liquid |
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| CN1202823A (en) * | 1995-11-28 | 1998-12-23 | B·布朗·梅尔松根有限公司 | Hydrolysis-optimized lipid emulsions and uses thereof |
| CN104760996A (en) * | 2015-03-16 | 2015-07-08 | 河北钢铁股份有限公司承德分公司 | Low-temperature crystallization method of ammonium polyvanadate |
| CN105174308A (en) * | 2015-10-20 | 2015-12-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of ammonium polyvanadate |
-
2016
- 2016-07-15 CN CN201610557600.7A patent/CN106241871A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1202823A (en) * | 1995-11-28 | 1998-12-23 | B·布朗·梅尔松根有限公司 | Hydrolysis-optimized lipid emulsions and uses thereof |
| CN104760996A (en) * | 2015-03-16 | 2015-07-08 | 河北钢铁股份有限公司承德分公司 | Low-temperature crystallization method of ammonium polyvanadate |
| CN105174308A (en) * | 2015-10-20 | 2015-12-23 | 攀钢集团攀枝花钢铁研究院有限公司 | Preparation method of ammonium polyvanadate |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107815547A (en) * | 2017-11-08 | 2018-03-20 | 攀钢集团攀枝花钢铁研究院有限公司 | The clean method of acid precipitation foulant in Leaching of Vanadium from Vanadium slag technique |
| CN108190955A (en) * | 2018-03-28 | 2018-06-22 | 河钢股份有限公司承德分公司 | A kind of recovery process of ammonium vanadate sodium production waste water |
| CN109081374A (en) * | 2018-10-19 | 2018-12-25 | 河钢股份有限公司承德分公司 | A method of preparing the spherical ammonium poly-vanadate of big granularity |
| CN112047379A (en) * | 2020-09-14 | 2020-12-08 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for precipitating ammonium polyvanadate |
| CN115676886A (en) * | 2022-11-15 | 2023-02-03 | 攀钢集团攀枝花钢铁研究院有限公司 | Vanadium precipitation method for reducing vanadium precipitation wastewater by using high-concentration vanadium liquid |
| CN115676886B (en) * | 2022-11-15 | 2024-05-14 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for reducing vanadium precipitation wastewater of high-concentration vanadium solution |
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Application publication date: 20161221 |