CN110423901B - Method for separating sodium vanadium chromium from vanadium chromium solution - Google Patents
Method for separating sodium vanadium chromium from vanadium chromium solution Download PDFInfo
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- CN110423901B CN110423901B CN201910859685.8A CN201910859685A CN110423901B CN 110423901 B CN110423901 B CN 110423901B CN 201910859685 A CN201910859685 A CN 201910859685A CN 110423901 B CN110423901 B CN 110423901B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D7/00—Carbonates of sodium, potassium or alkali metals in general
- C01D7/22—Purification
- C01D7/24—Crystallisation
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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
- C01G31/02—Oxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G37/00—Compounds of chromium
- C01G37/02—Oxides or hydrates thereof
- C01G37/033—Chromium trioxide; Chromic acid
-
- 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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
-
- 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
- C22B34/20—Obtaining niobium, tantalum or vanadium
- C22B34/22—Obtaining vanadium
-
- 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
- C22B34/32—Obtaining chromium
-
- 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 invention belongs to the field of chemical industry, and particularly relates to a method for separating vanadium-chromium-sodium from a vanadium-chromium solution. The invention aims to solve the technical problem of providing a method for separating sodium vanadium chromium from a vanadium chromium solution, which comprises the following steps: a. adjusting the pH value of the vanadium-chromium solution to 2.0-4.0 by using organic acid, then adding a vanadium precipitation agent for reaction, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain vanadium pentoxide; b. adding organic acid into the liquid obtained by solid-liquid separation in the step a, concentrating to 1/3-1/2 volume, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain chromium sesquioxide; c. and c, concentrating the liquid obtained in the step b through solid-liquid separation to obtain sodium carbonate. The method adopts organic acid to adjust the pH value of the chromium vanadium solution, does not carry sulfate radicals and chloride ions, and adopts ammonium bicarbonate to precipitate vanadium at low temperature, thereby reducing energy consumption. The method can simultaneously recover the vanadium-chromium-sodium, has short process, easy operation and good separation effect of vanadium and chromium.
Description
Technical Field
The invention belongs to the field of chemical industry, and particularly relates to a method for separating sodium vanadium chromium from a vanadium chromium solution.
Background
Many researches on the separation of vanadium and chromium in the vanadium-chromium solution are carried out, such as a precipitation method, an extraction method, an ion exchange method or a combination of several methods are adopted, and different methods are selected according to the content of vanadium and chromium in the vanadium-chromium solution. The general precipitation method is more for separating vanadium from a vanadium-chromium solution, such as ammonium sulfate precipitation of vanadium, calcium salt precipitation of vanadium, and iron salt precipitation of vanadium; vanadium and chromium are respectively precipitated.
For example, CN105506285A "a method for separating and recovering vanadium and chromium from a solution containing vanadium or/and chromium" discloses adding a precipitating agent a to the solution containing vanadium or/and chromium to selectively precipitate vanadium therein, adding a precipitating agent B to precipitate chromium therein, and introducing CO into the solution after chromium precipitation2Crystallizing to separate out sodium bicarbonate, and finally separating and recovering vanadium and chromium from the vanadium-enriched slag and the chromium-enriched slag respectively.
The vanadium and chromium precipitated in the existing processes need to be extracted again, and the process flow is long.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for separating sodium vanadium chromium from a vanadium chromium solution. The method comprises the following steps:
a. adjusting the pH value of the vanadium-chromium solution to 2.0-4.0 by using organic acid, then adding a vanadium precipitation agent for reaction, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain vanadium pentoxide;
b. adding organic acid into the liquid obtained by solid-liquid separation in the step a, concentrating to 1/3-1/2 volume, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain chromium sesquioxide;
c. and c, concentrating and crystallizing the liquid obtained by solid-liquid separation in the step b to obtain sodium carbonate.
Specifically, in step a of the method for separating sodium vanadium chromium from a vanadium chromium solution, the vanadium chromium solution is a vanadium chromium solution obtained by sodium roasting water leaching or alkali leaching. Further, the vanadium content in the vanadium-chromium solution is 5-80 g/L, and the chromium content is 5-80 g/L.
Preferably, in step a of the method for separating sodium vanadium chromium from a solution of vanadium chromium, the organic acid is at least one of formic acid, acetic acid, propionic acid, butyric acid, octanoic acid, maleic acid, valeric acid or acrylic acid.
Preferably, in step a of the method for separating sodium vanadium chromium from a solution of vanadium chromium, the vanadium precipitation agent is at least one of ammonium bicarbonate or ammonium carbonate.
Preferably, in step a of the method for separating sodium vanadium chromium from a vanadium chromium solution, the addition amount of the vanadium precipitation agent is
Preferably, in the step a of the method for separating sodium vanadium chromium from the vanadium chromium solution, the reaction temperature is 0-60 ℃. The reaction time is 0.5-3 h.
Further, in the step a of the method for separating sodium vanadium chromium from the vanadium chromium solution, a standing step is further included before solid-liquid separation. Standing for 1-2 h.
Preferably, in the step a of the method for separating sodium vanadium chromium from the vanadium chromium solution, the calcination temperature is 500-550 ℃.
Preferably, in step b of the method for separating sodium vanadium chromium from the solution of vanadium chromium, the organic acid is added in a molar ratio, nC/nCr＝1～3。
Preferably, in the step b of the method for separating sodium vanadium chromium from the vanadium chromium solution, the concentration temperature is 90-120 ℃. Further 100 to 110 ℃.
Preferably, in the step b of the method for separating sodium vanadium chromium from the vanadium chromium solution, the calcination temperature is 300-1000 ℃.
Preferably, in the step c of the method for separating sodium vanadium chromium from the vanadium chromium solution, the concentration temperature is 150 to 300 ℃.
The method adopts organic acid to adjust the pH value of the vanadium-chromium solution, does not carry sulfate radicals and chloride ions, and adopts ammonium bicarbonate to precipitate vanadium at low temperature, thereby reducing energy consumption. The method of the invention generates no additional sodium sulfate and ammonium sulfate, thereby greatly reducing the treatment cost. The method can simultaneously recover vanadium, chromium and sodium, has short process, easy operation and good vanadium and chromium separation effect.
Detailed Description
The method adopts organic acid to adjust the pH value, ammonium bicarbonate precipitates vanadium at low temperature under the acidic condition, and the vanadium product is obtained after solid-liquid separation; adding organic acid into the vanadium precipitation wastewater, concentrating, and carrying out solid-liquid separation to obtain a chromium product; the liquid is continuously concentrated and crystallized to obtain the sodium carbonate. In the method, the vanadium precipitation is adjusted by organic acid at low temperature, the precipitated vanadium does not carry sulfate radical plasma, the organic acid is decomposed under subsequent high-temperature concentration to play a role of reduction, a chromium product is obtained after the reduction, and sodium carbonate obtained after the liquid is re-concentrated can return to a system for roasting.
The invention discloses a method for cleanly separating vanadium-chromium sodium from a vanadium-chromium solution, which comprises the following steps: a. regulating the pH value of the vanadium-chromium solution to a certain range by using organic acid; b. adding a certain amount of vanadium precipitation agent while stirring; c. stirring for a certain time at a certain temperature after the addition; d. standing for a certain time, and performing solid-liquid separation; e. washing, drying and calcining the obtained solid to obtain vanadium pentoxide; f. adding a certain amount of organic acid into the liquid, and continuously concentrating at a certain temperature; concentrating until the volume is 1/3-1/2 of the original volume, and performing solid-liquid separation; g. washing and calcining the solid to obtain chromium sesquioxide; i. and (c) continuously concentrating and crystallizing the liquid at a certain temperature to obtain sodium carbonate, and returning a small amount of crystallized liquid to the step (a).
The invention discloses a method for cleanly separating vanadium-chromium sodium from a vanadium-chromium solution, which comprises the following steps:
a. adjusting the pH value of the vanadium-chromium solution to 2.0-4.0 by using organic acid, and stirring while stirring
Adding a vanadium precipitation agent, stirring for 0.5-3 h at 0-60 ℃, standing for 1-2 h, performing solid-liquid separation to obtain solid, washing, drying and calcining at 500-550 ℃ to obtain vanadium pentoxide;
b. the liquid obtained in step a is expressed by nC/nCrAdding organic acid into the mixture 1-3 (the molar weight ratio is 1 mol, for example, C/1 mol of Cr), concentrating the mixture at 90-120 ℃ until the volume of the concentrated mixture is 1/3-1/2 of the original volume, carrying out solid-liquid separation, washing the solid, and calcining the solid at 300-1000 ℃ to obtain chromium sesquioxide;
c. and c, continuously concentrating and crystallizing the liquid obtained in the step b at the temperature of 150-300 ℃ to obtain sodium carbonate.
In the method of the present invention, the organic acid is at least one of formic acid, acetic acid, propionic acid, butyric acid, caprylic acid, maleic acid, valeric acid, or acrylic acid. In the method, organic acid is added to adjust the pH value of the vanadium-containing liquid, if the pH value is lower than 2.0, the acidity is too strong, and partial precipitated vanadium can be re-dissolved, so that the vanadium precipitation rate is reduced; if the pH is higher than 4.0 and lower than 6.5, the precipitate generally carries sodium, and the quality of the vanadium product is affected by the increase of the sodium content in the vanadium product. Therefore, the pH value of the vanadium-containing liquid needs to be adjusted to 2.0-4.0 by controlling the organic acid.
In the method, the vanadium precipitation agent is at least one of ammonium bicarbonate or ammonium carbonate. In the method of the present invention, the step of,
for example, when the vanadium precipitation agent is ammonium bicarbonate and the molecular formula thereof has 1N atom, the denominator in the above formula is 1, and when the vanadium precipitation agent is ammonium carbonateWhen the molecular formula has 2N atoms, the denominator in the above formula is 2. The mass of the vanadium precipitation agent added is calculated by the formula and is the mass of the pure vanadium precipitation agent.
In the method, organic acid is added and then concentrated, and if the concentration is lower than 1/3, more sodium salt is brought, which brings difficulty to the preparation of chromium products; above 1/2, the chromium remaining in the sodium salt increases, which causes difficulty in the preparation of the sodium salt. Therefore, it is preferable to concentrate the solution to 1/3-1/2 volumes.
Example 1
Regulating the pH value of 1000mL of vanadium-chromium solution (the vanadium content is 5g/L, and the chromium content is 5g/L) to 2.0 by formic acid and propionic acid; adding 11.61g of ammonium bicarbonate while stirring; stirring for 0.5h at 40 ℃; standing for 1h, performing solid-liquid separation to obtain ammonium polyvanadate, washing, drying, and calcining at 500 ℃ to obtain vanadium pentoxide; chromium solution nC/nCrPropionic acid was added and concentration continued at 90 ℃; concentrating to 1/3 volume, and filtering; after washing, calcining the filter cake at 300 ℃ to obtain chromium sesquioxide; and (c) continuously concentrating and crystallizing the filtrate at 150 ℃ to obtain sodium carbonate, and returning a small amount of crystallized liquid to the step (a).
The vanadium precipitation rate is 98.5 percent, and the calcined vanadium pentoxide meets the standard requirement of quality YB/T5304-2017; the yield of the chromium sesquioxide is 95 percent, and the quality meets the requirement of HG/T2775-2010 standard.
Example 2
Regulating the pH value of 1000mL of vanadium-chromium solution (the vanadium content is 35g/L, and the chromium content is 25g/L) to 3.0 by using formic acid; adding 24.7g of ammonium carbonate while stirring; stirring for 1.5h at 40 ℃; standing for 1.5h, performing solid-liquid separation to obtain ammonium polyvanadate, washing, drying, and calcining at 520 ℃ to obtain vanadium pentoxide; chromium solution nC/nCrFormic acid was added 1.5 and concentration continued at 110 ℃; concentrating to 2/5 volume, and filtering; after washing, calcining the filter cake at 600 ℃ to obtain chromium sesquioxide; and (c) continuously concentrating and crystallizing the filtrate at 200 ℃ to obtain sodium carbonate, and returning a small amount of crystallized liquid to the step (a).
The vanadium precipitation rate is 99.1 percent, and the calcined vanadium pentoxide meets the standard requirement of quality YB/T5304-2017; the yield of the chromium sesquioxide is 97 percent, and the quality meets the requirement of HG/T2775-2010 standard.
Example 3
Regulating the pH value of 1000mL of vanadium-chromium solution (the vanadium content is 80g/L, and the chromium content is 80g/L) to 4.0 by using acrylic acid; adding a mixture of 223g of ammonium bicarbonate and 203g of ammonium carbonate while stirring; stirring for 3h at 60 ℃; standing for 2h, performing solid-liquid separation to obtain ammonium polyvanadate, washing, drying, and calcining at 550 ℃ to obtain vanadium pentoxide; chromium solution nC/nCrA mixture of propionic acid and acrylic acid was added and concentration continued at 120 ℃; concentrating to 1/2 volume, and filtering; after washing the filter cake, calcining at 1000 ℃ to obtain chromium sesquioxide; and (c) continuously concentrating and crystallizing the filtrate at 300 ℃ to obtain sodium carbonate, and returning a small amount of crystallized liquid to the step (a).
The vanadium precipitation rate is 99.35 percent, and the calcined vanadium pentoxide meets the standard requirement of quality YB/T5304-2017; the yield of the chromium sesquioxide is 98.5 percent, and the quality meets the requirement of HG/T2775-2010 standard.
Claims (11)
1. The method for separating the vanadium-chromium-sodium from the vanadium-chromium solution is characterized by comprising the following steps: the method comprises the following steps:
a. adjusting the pH value of the vanadium-chromium solution to 2.0-4.0 by using organic acid, then adding a vanadium precipitation agent for reaction, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain vanadium pentoxide;
b. adding organic acid into the liquid obtained by solid-liquid separation in the step a, concentrating to 1/3-1/2 volume, carrying out solid-liquid separation, and washing, drying and calcining the solid to obtain chromium sesquioxide; the organic acid is at least one of propionic acid, butyric acid, caprylic acid, maleic acid, valeric acid or acrylic acid;
c. and c, concentrating and crystallizing the liquid obtained by solid-liquid separation in the step b to obtain sodium carbonate.
2. The process of separating sodium vanadium chromium from a solution of vanadium chromium according to claim 1, characterized in that: in the step a, the vanadium-chromium solution is obtained by sodium roasting water leaching or alkali leaching.
3. The process of separating sodium vanadium chromium from a solution of vanadium chromium according to claim 2, characterized in that: the vanadium-chromium solution contains 5-80 g/L of vanadium and 5-80 g/L of chromium.
4. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step a, the reaction temperature is 0-60 ℃; the reaction time is 0.5-3 h.
5. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step a, a standing step is also included before solid-liquid separation.
6. The process of separating sodium vanadium chromium from a solution of vanadium chromium according to claim 5, characterized in that: and standing for 1-2 h.
7. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step a, the calcining temperature is 500-550 ℃; in the step b, the calcining temperature is 300-1000 ℃.
8. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step b, the adding amount of the organic acid is in molar ratio, nC/ n Cr=1～3。
9. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step b, the concentration temperature is 90-120 ℃.
10. The process of separating sodium vanadium chromium from a solution of vanadium chromium according to claim 9, characterized in that: in the step b, the concentration temperature is 100-110 ℃.
11. A process for the separation of sodium vanadium chromium from a solution of vanadium chromium according to any one of claims 1 to 3 characterized in that: in the step c, the concentration temperature is 150-300 ℃.
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| CN111534698A (en) * | 2020-06-12 | 2020-08-14 | 攀钢集团研究院有限公司 | Method for preparing vanadium product from sodium vanadium solution without ammonium precipitation |
| CN112079507A (en) * | 2020-08-27 | 2020-12-15 | 河钢承德钒钛新材料有限公司 | Method for producing anhydrous sodium sulphate from vanadium extraction wastewater |
| CN113582244A (en) * | 2021-06-29 | 2021-11-02 | 南通金通储能动力新材料有限公司 | Method for reducing sodium content in high-sodium nickel cobalt manganese hydroxide |
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