CN113104816A - Method for extracting sulfuric acid by recycling vanadium precipitation wastewater - Google Patents
Method for extracting sulfuric acid by recycling vanadium precipitation wastewater Download PDFInfo
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- C01B17/00—Sulfur; Compounds thereof
- C01B17/69—Sulfur trioxide; Sulfuric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B17/22—Alkali metal sulfides or polysulfides
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Abstract
The invention relates to a method for recycling vanadium precipitation wastewater and extracting sulfuric acid, belonging to the technical field of recycling vanadium extraction tailings. The method for recycling the vanadium precipitation wastewater to extract the sulfuric acid comprises the following steps: extracting V from vanadium slag after vanadium extraction by sodium roasting method2O5Will extract V2O5Carrying out gradient roasting on the vanadium precipitation wastewater, adding a reducing agent, mixing, reacting at 1000-1150 ℃ for 1.5-2 h, and reducing to obtain the product containing Na2Solids of S and SO2、NH3、CO2A gas; the gradient roasting is sequentially heating for 0.25-0.3 h at 1000-1075 ℃, for 0.5-0.6 h at 1085-1135 ℃ and for 0.75-0.8 h at 1145-1150 ℃; absorbing said gas with NH3Then, the residual gas reacts with oxygen under the action of a catalyst to obtain SO3(ii) a Adding SO3Absorbing to obtain H2SO4. The method has high recovery efficiency and saves time and energy cost.
Description
Technical Field
The invention relates to a method for recycling vanadium precipitation wastewater and extracting sulfuric acid, belonging to the technical field of recycling vanadium extraction tailings.
Background
Vanadium is an important rare metal in the industrial field and is mainly used in the steel industry. The vanadium-containing steel has the excellent characteristics of high strength, high toughness, good wear resistance and the like, so the vanadium-containing steel is widely applied to industries such as machinery, automobiles, shipbuilding, railways, aviation, bridges, electronic technology, national defense industry and the like, the consumption of the vanadium-containing steel accounts for about 85 percent of the vanadium consumption, and the consumption of the steel industry accounts for the maximum proportion in the application of the vanadium. The demand of the steel industry directly influences the market quotation of vanadium. About 10% of vanadium is used to produce titanium alloys required by the aerospace industry. Vanadium can be used as a stabilizer and a reinforcer in the titanium alloy, so that the titanium alloy has good ductility and plasticity. In addition, vanadium is used primarily as a catalyst and colorant in the chemical industry. Vanadium has also been used to produce rechargeable hydrogen or vanadium redox batteries. In addition, the new national steel standard regulations require that the vanadium content standard in steel is improved by 25 times. The demand of vanadium is increased sharply due to various reasons, so that the vanadium extraction enterprises can produce the vanadium in full, a large amount of solid waste generated by vanadium extraction is accumulated, and if the solid waste is not treated in time, the vanadium extraction enterprises can not only face the production stop crisis; the accumulation of the vanadium extraction tailings can cause serious pollution to the environment.
The treatment of the vanadium extraction tailings in the prior art is to carry out sodium roasting method on the vanadium extraction tailings to extract V2O5And accumulating the residual vanadium precipitation wastewater, wherein the residual vanadium precipitation wastewater mainly contains sodium sulfate and ammonium sulfate and other impurities. If proper treatment is not carried out, not only is the waste of resources caused and the requirement of clean production not met, but also the crystal liquid is placed in the environment to generate dust emission, leaching and the like, secondary pollution is formed, and the environment is obviously influenced.
Disclosure of Invention
The first purpose of the invention is to provide a method for extracting sulfuric acid by recycling vanadium precipitation wastewater.
In order to achieve the first object of the invention, the method for recycling the vanadium precipitation wastewater to extract sulfuric acid comprises the following steps:
A. reduction of vanadium-precipitating waste water by sodium roasting method, namely extracting V from vanadium slag after vanadium extraction by sodium roasting method2O5Will extract V2O5Carrying out gradient roasting on the vanadium precipitation wastewater, adding a reducing agent, mixing, reacting at 1000-1150 ℃ for 1.5-2 h, and reducing to obtain the product containing Na2Solids of S and SO2、NH3、CO2A gas; the gradient roasting is sequentially heating for 0.25-0.3 h at 1000-1075 ℃, for 0.5-0.6 h at 1085-1135 ℃ and for 0.75-0.8 h at 1145-1150 ℃;
B.SO2oxidation of (2): absorbing NH in the gas in the step A3Then, the residual gas reacts with oxygen under the action of a catalyst to obtain SO3；
C. Subjecting the SO to3Absorbing to obtain H2SO4；
The reducing agent is preferably fly ash.
In a specific embodiment, the mass of the vanadium precipitation wastewater subjected to gradient roasting in the step A is M, and the mass ratio of M to the reducing agent is 3-5: 1.
In a specific embodiment, the water content in the vanadium precipitation wastewater in the step A is less than 9.5%, and the water in the vanadium precipitation wastewater after the gradient roasting is completely evaporated.
In one embodiment, the reducing agent has a particle size of less than 7 mesh.
In a specific embodiment, the gradient roasting is firstly heating for 0.25-0.3 h at 1000-1075 ℃; heating at 1085-1135 ℃ for 0.5-0.6 h; finally heating at 1145-1150 ℃ for 0.75-0.8 h.
In a specific embodiment, the temperature of the reaction in the step B is 550-650 ℃.
In one embodiment, the catalyst in step C is V2O5Platinum, oxygenIron melting; preferably V2O5。
In a specific embodiment, the method further comprises adding Na to the solution containing Na2And (3) leaching the solid of the S with an alkali solution, taking supernatant, concentrating and drying to obtain sodium sulfide.
In a specific embodiment, the alkali is 78-85% NaOH, the leaching temperature is 75-90 ℃, and the leaching time is preferably 4-4.3 h.
In one embodiment, the sodium sulfide is produced in a yield of 89.5-99.2% and a purity of 98.4-99.9%.
Has the advantages that:
the method for extracting sulfuric acid by recycling vanadium precipitation wastewater has high recovery efficiency and saves time and energy cost. The method disclosed by the invention has the advantages that the vanadium precipitation wastewater is treated, so that the subsequent yield of sodium sulfide can reach 89.5-99.2%, the sodium sulfide is easy to leach and purify, and the purity can reach 98.4-99.9% after concentration and drying through simple alkali leaching.
Drawings
FIG. 1 is a diagram of a process for carrying out the present invention.
Detailed Description
In order to achieve the first object of the invention, the method for recycling the vanadium precipitation wastewater to extract sulfuric acid comprises the following steps:
A. reduction of vanadium-precipitating waste water by sodium roasting method, namely extracting V from vanadium slag after vanadium extraction by sodium roasting method2O5Will extract V2O5Carrying out gradient roasting on the vanadium precipitation wastewater, adding a reducing agent, mixing, reacting at 1000-1150 ℃ for 1.5-2 h, and reducing to obtain the product containing Na2Solids of S and SO2、NH3、CO2A gas; the gradient roasting is sequentially heating for 0.25-0.3 h at 1000-1075 ℃, for 0.5-0.6 h at 1085-1135 ℃ and for 0.75-0.8 h at 1145-1150 ℃;
B.SO2oxidation of (2): absorbing NH in the gas in the step A3Then, the residual gas reacts with oxygen under the action of a catalyst to obtain SO3；
C. Subjecting the SO to3Absorbing to obtain H2SO4；
The reducing agent is preferably fly ash.
In a specific embodiment, the mass of the vanadium precipitation wastewater subjected to gradient roasting in the step A is M, and the mass ratio of M to the reducing agent is 3-5: 1.
In a specific embodiment, the water content in the vanadium precipitation wastewater in the step A is less than 9.5%, and the water in the vanadium precipitation wastewater after the gradient roasting is completely evaporated.
In one embodiment, the reducing agent has a particle size of less than 7 mesh.
In a specific embodiment, the gradient roasting is firstly heating for 0.25-0.3 h at 1000-1075 ℃; heating at 1085-1135 ℃ for 0.5-0.6 h; finally heating at 1145-1150 ℃ for 0.75-0.8 h.
In a specific embodiment, the temperature of the reaction in the step B is 550-650 ℃.
In one embodiment, the catalyst in step C is V2O5Platinum, iron oxide; preferably V2O5。
In a specific embodiment, the method further comprises adding Na to the solution containing Na2And (3) leaching the solid of the S with an alkali solution, taking supernatant, concentrating and drying to obtain sodium sulfide.
In a specific embodiment, the alkali is 78-85% NaOH, the leaching temperature is 75-90 ℃, and the leaching time is preferably 4-4.3 h.
In one embodiment, the sodium sulfide is produced in a yield of 89.5-99.2% and a purity of 98.4-99.9%.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
And conveying the vanadium precipitation wastewater to a reaction workshop for roasting. And (3) performing step-by-step gradient continuous roasting in a rotary chamber, sequentially roasting at 1054 ℃ for 0.28h, 1100 ℃ for 0.55h and 1148 ℃ for 0.77h, and completely evaporating water in the vanadium precipitation wastewater after the step roasting. The model number of the rotary furnace KY-LQ is 600-10m, and then the rotary furnace KY-LQ is mixed with high-quality coal powder (the granularity of the coal powder is less than 7 meshes) with high carbon content, and the weight ratio of the solid mass after the wastewater is dried to the coal powder is 5: 1. Reacting for 1.8h at 1020 ℃ by taking coal gas as a heat source. The model of the reaction rotary furnace is QC-M1800-18 IK. The equipment processing capacity is 5 t/h.
The reduced gas after the reaction in the rotary furnace is directly led to an absorption chamber, and NH generated by the reaction is absorbed by a titanium type catalyst at the temperature of 300 DEG C3Then, the residual SO2With CO2Introducing the mixed gas into a contact chamber, SO2At V2O5At 620 ℃ with O2Reaction to form SO3SO formed3Directly introducing into an absorption tower, and using 98.3% concentrated sulfuric acid as SO3Absorption of (2). Generation of H2SO4The reaction rate of (A) was 1.2 t/stage · h.
Cooling the residual solid after the reaction in the rotary furnace to 700 ℃, putting the solid into 80 ℃ NaOH solution with the concentration of 80 percent for leaching for 4 hours, taking supernatant fluid after leaching, concentrating and drying to obtain the sodium sulfide.
The yield of the obtained sodium sulfide is 99.2%; the purity of the sodium sulfide is detected to be 99.8%.
Example 2
a. 1kg of vanadium precipitation wastewater is continuously roasted by adopting a step gradient, wherein the mass fraction of Na in the vanadium precipitation wastewater is calculated2SO4 68.0％，(NH4)2SO4 20.2％，H2O 9.1％，NH40.8 percent of Cl0.9 percent and the rest 1.9 percent. The process of the sectional gradient continuous roasting comprises the following steps: firstly, heating for 0.25h at 1054 ℃; heating at 1100 deg.C for 0.5 h; finally heating at 1148 deg.C for 0.75 h. After the step gradient continuous roasting and sintering, completely evaporating the water in the vanadium precipitation wastewater;
b. pulverizing coal powder until the particle size is less than 7 meshes;
c. mixing the raw materials subjected to the sectional gradient continuous roasting and the coal powder according to the weight ratio of 5:1, heating by using coal gas for reduction reaction at the reaction temperature of 1000 ℃ for 2 hours to obtain a solid pre-product and mixed gas;
d. cooling the pre-product to 700 ℃, putting the pre-product into 80 ℃ NaOH solution with the concentration of 80 percent, leaching for 4 hours, taking supernatant fluid after leaching, concentrating and drying to obtain the sodium sulfide.
The weight of the obtained sodium sulfide was 371.2g, and the yield was 99.2%; the purity of the sodium sulfide is detected to be 99.9%.
The mixed gas passes through a titanium type catalyst to absorb NH3The remaining gas is passed into V2O5Blowing pure oxygen into a catalyst absorption chamber, controlling the reaction temperature at 620 ℃, and adding SO2Oxidation to SO3Finally, 98.3% concentrated sulfuric acid is used as SO3The absorption of (3) produced 143g of sulfuric acid.
Comparative example 1
a. Taking 1kg of vanadium precipitation wastewater, wherein Na is contained in the wastewater2SO468.0％，(NH4)2SO420.2 percent, and after the vanadium precipitation wastewater is heated for 6 hours at the temperature of 1150 ℃, the water content of the vanadium precipitation wastewater is 0 percent.
b. Pulverizing coal powder until the particle size is less than 7 meshes;
c. mixing the dried raw materials and coal powder according to a weight ratio of 5:1, heating by using coal gas for reduction reaction at 1000 ℃, and controlling the reaction time to be 2 hours to obtain a pre-product;
d. cooling the pre-product to 700 ℃, putting the pre-product into 80 ℃ NaOH solution with the concentration of 80 percent, leaching for 4 hours, taking supernatant fluid after leaching, concentrating and drying to obtain the sodium sulfide.
The weight of sodium sulfide obtained was 208.3g, the yield was 61.3%, and the purity was found to be 91%.
Absorption of the SO produced2: absorption of NH by a titanium-type catalyst3Introducing SO2Let in V2O5Blowing pure oxygen into a catalyst absorption chamber, controlling the reaction temperature at 620 ℃, and adding SO2Oxidation to SO3Finally, 98.3% concentrated sulfuric acid is used as SO3The absorption of (2) produced 86g of sulfuric acid.
Claims (10)
1. The method for recycling the vanadium precipitation wastewater to extract sulfuric acid is characterized by comprising the following steps:
A. sodium roasting processReduction of vanadium-precipitating waste water, namely extracting V from vanadium slag after vanadium extraction by a sodium salt roasting method2O5Will extract V2O5Carrying out gradient roasting on the vanadium precipitation wastewater, adding a reducing agent, mixing, reacting at 1000-1150 ℃ for 1.5-2 h, and reducing to obtain the product containing Na2Solids of S and SO2、NH3、CO2A gas; the gradient roasting is sequentially heating for 0.25-0.3 h at 1000-1075 ℃, for 0.5-0.6 h at 1085-1135 ℃ and for 0.75-0.8 h at 1145-1150 ℃;
B.SO2oxidation of (2): absorbing NH in the gas in the step A3Then, the residual gas reacts with oxygen under the action of a catalyst to obtain SO3；
C. Subjecting the SO to3Absorbing to obtain H2SO4；
The reducing agent is preferably fly ash.
2. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to claim 1, wherein the mass of the vanadium precipitation wastewater subjected to gradient roasting in the step A is M, and the mass ratio of M to a reducing agent is 3-5: 1.
3. The method for recycling the waste water after vanadium precipitation according to claim 1 or 2 and extracting sulfuric acid, wherein the water content in the waste water after vanadium precipitation in step A is less than 9.5%, and the water in the waste water after vanadium precipitation is completely evaporated after gradient roasting.
4. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to any one of claims 1 to 3, wherein the particle size of the reducing agent is less than 7 meshes.
5. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to any one of claims 1 to 4, wherein the gradient roasting is performed by heating at 1000-1075 ℃ for 0.25-0.3 h; heating at 1085-1135 ℃ for 0.5-0.6 h; finally heating at 1145-1150 ℃ for 0.75-0.8 h.
6. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to any one of claims 1 to 5, wherein the reaction temperature in the step B is 550 to 650 ℃.
7. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to any one of claims 1 to 6, wherein the catalyst in the step C is V2O5Platinum, iron oxide; preferably V2O5。
8. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to any one of claims 1 to 7, further comprising the step of adding Na to the wastewater2And (3) leaching the solid of the S with an alkali solution, taking supernatant, concentrating and drying to obtain sodium sulfide.
9. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to claim 8, wherein the alkali is 78-85% NaOH, the leaching temperature is 75-90 ℃, and the leaching time is preferably 4-4.3 h.
10. The method for recycling and extracting sulfuric acid from vanadium precipitation wastewater according to claim 9, wherein the yield of sodium sulfide is 89.5-99.2%, and the purity is 98.4-99.9%.
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