CN105039714A - Processing method for sodium treatment vanadium and chromium extracting residues and method for extracting vanadium and chromium through sodium salt roasting of vanadium and chromium residues - Google Patents
Processing method for sodium treatment vanadium and chromium extracting residues and method for extracting vanadium and chromium through sodium salt roasting of vanadium and chromium residues Download PDFInfo
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Abstract
The invention relates to a processing method for sodium treatment vanadium and chromium extracting residues. The method comprises the steps that the sodium treatment vanadium and chromium extracting residues, a calcium compound and water are mixed, the hydrothermal reaction is carried out, solid-liquid separation is carried out on the mixture obtained after the hydrothermal reaction, and a liquid phase and a solid phase are obtained, wherein the sodium treatment vanadium and chromium extracting residues are residues obtained after vanadium and chromium are extracted through the sodium salt roasting of vanadium and chromium residues. The invention further provides a method for extracting vanadium and chromium through sodium salt roasting of the vanadium and chromium residues with the liquid phase as an alkaline reagent to replace part of a sodium compound. By means of the processing method for the sodium treatment vanadium and chromium extracting residues, the liquid phase containing the enriched sodium element can be well separated out. According to the method for extracting vanadium and chromium through sodium salt roasting of the vanadium and chromium residues with the liquid phase as the alkaline reagent, the cost for extracting vanadium and chromium through sodium salt roasting of the vanadium and chromium residues is reduced.
Description
Technical field
The present invention relates to the treatment process of sodium vanadium extraction chromium residue and the method for vanadium chromium slag sodium roasting vanadium-extracting and chromium.
Background technology
In high-chromic vanadium-titanium ferroferrite comprehensive utilization process, the recycling main manifestations of vanadium and chromium is the separation and Extraction to vanadium chromium slag vanadium and chromium.Wherein, it is by adopting the soda salt of high mixture ratio to carry out roasting and water logging completes with common extraction vanadium chromium that sodium roasting vanadium chromium slag extracts vanadium chromium, when obtaining leach liquor, also creates solid residue and sodium vanadium extraction chromium residue simultaneously.Such residue contains the Na of 5 ~ 25 % by weight
2o, and vanadium, chromium, iron that part is residual.The basic metal of high-content does not utilize it to recycle, and directly stores up not only contaminate environment but also cause the wasting of resources.Such residue effectively utilizes at present.
Summary of the invention
The object of the invention is to overcome because sodium vanadium extraction chromium residue alkali metal is difficult to recycle the defect causing contaminate environment and the wasting of resources, a kind of method that can reclaim and utilize alkali metal in sodium vanadium extraction chromium residue is preferably provided, namely provides a kind for the treatment of process of sodium vanadium extraction chromium residue and a kind of method of vanadium chromium slag sodium roasting vanadium-extracting and chromium.
To achieve these goals, the invention provides a kind for the treatment of process of sodium vanadium extraction chromium residue, wherein, the method comprises: sodium vanadium extraction chromium residue, calcium containing compound and water are mixed and carry out hydro-thermal reaction, mixture after described hydro-thermal reaction is carried out solid-liquid separation, obtain liquid phase and solid phase, wherein, described sodium vanadium extraction chromium residue is the residue after vanadium chromium slag sodium roasting vanadium-extracting and chromium.
Present invention also offers a kind of method of vanadium chromium slag sodium roasting vanadium-extracting and chromium, the method comprises: vanadium chromium slag and compounds containing sodium are carried out roasting, and the material after described roasting is leached, wherein, described roasting is also carried out under alkaline reagents exists, and described alkaline reagents is the liquid phase of aforesaid method gained.
By the treatment process of sodium vanadium extraction chromium residue of the present invention, the liquid phase of the sodium element containing enrichment can be isolated preferably, and can be used as the solid phase of slag former etc., achieve the separation of the favourable resource to sodium vanadium extraction chromium residue, greatly reduce the possibility of sodium vanadium extraction chromium residue pollution on the environment and the wasting of resources.Further, present invention also offers and adopt gained liquid phase as the method for alkaline reagents for vanadium chromium slag sodium roasting vanadium-extracting and chromium, reduce the cost of vanadium chromium slag sodium roasting vanadium-extracting and chromium.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Embodiment
Below the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
The invention provides a kind for the treatment of process of sodium vanadium extraction chromium residue, wherein, the method comprises: sodium vanadium extraction chromium residue, calcium containing compound and water are mixed and carry out hydro-thermal reaction, mixture after described hydro-thermal reaction is carried out solid-liquid separation, obtain liquid phase and solid phase, wherein, described sodium vanadium extraction chromium residue is the residue after vanadium chromium slag sodium roasting vanadium-extracting and chromium.
According to the present invention, described sodium vanadium extraction chromium residue is the residue after vanadium chromium slag sodium roasting vanadium-extracting and chromium, also be after vanadium chromium slag sodium roasting, be separated after water logging and obtain leach liquor and residue, wherein, vanadium containing proposition in leach liquor and chromium are therefore for reclaiming vanadium chromium further, and residue is sodium vanadium extraction chromium residue here.In the present invention, described sodium vanadium extraction chromium residue can be the residue by the vanadium chromium slag sodium roasting vanadium-extracting of this area routine and the method gained of chromium, also can be the residue of the method gained of the vanadium chromium slag sodium roasting vanadium-extracting that provides of the present invention and chromium, the present invention be not particularly limited this.Preferably, in described sodium vanadium extraction chromium residue, with Na
2the content of the sodium element of O meter is 10-20 % by weight, and the content of v element is 0.2-1 % by weight, and the content of chromium element is 0.5-1.2 % by weight.More preferably, in described sodium vanadium extraction chromium residue, with Na
2the content of the sodium element (Na) of O meter is 13-17 % by weight, and the content of v element (V) is 0.3-0.7 % by weight, and the content of chromium element (Cr) is 0.7-0.9 % by weight.
According to the present invention, described calcium containing compound can provide active calcium ion for hydro-thermal reaction in the treatment process of sodium vanadium extraction chromium residue, therefore, the present invention is not particularly limited described calcium containing compound, as long as such object can be realized, preferably, described calcium containing compound is one or more in calcium oxide, calcium chloride, calcium hydroxide, nitrocalcite and Calcium hydrogen carbonate, is more preferably one or more in calcium oxide, calcium chloride and calcium hydroxide.
According to the present invention, in described hydro-thermal reaction, water can adopt the water resources of this area routine, such as tap water, service water, rainwater etc.
According to the present invention, as long as although sodium vanadium extraction chromium residue, calcium containing compound and the water treatment process by sodium vanadium extraction chromium residue of the present invention is processed, required liquid phase and solid phase can be obtained, described liquid phase and solid phase is obtained in order to be separated better, and obtain the alkaline reagents that can be used as in the method for vanadium chromium slag sodium roasting vanadium-extracting and chromium, preferably, relative to 100 weight parts with Na
2the sodium vanadium extraction chromium residue of O meter, in the consumption of the described calcium containing compound of CaO for 20-60 weight part, the consumption of water is 100-1000 weight part.More preferably, relative to 100 weight parts with Na
2the sodium vanadium extraction chromium residue of O meter, in the consumption of the described calcium containing compound of CaO for 30-50 weight part, the consumption of water is 500-700 weight part.Still more preferably, relative to 100 weight parts with Na
2the sodium vanadium extraction chromium residue of O meter, in the consumption of the described calcium containing compound of CaO for 37-50 weight part, the consumption of water is 500-700 weight part.
According to the present invention, described hydro-thermal reaction can realize sodium ion in sodium vanadium extraction chromium residue and calcium ion-exchanged effectively, to reach the object of sodium vanadium extraction chromium residue being carried out to de-sodium, in order to the effect of de-sodium can be reached better, under preferable case, the condition of described hydro-thermal reaction comprises: temperature is 95-300 DEG C, and the time is 0.5-5h.More preferably, the condition of described hydro-thermal reaction comprises: temperature is 160-300 DEG C, and the time is 1.5-3h.Still more preferably, the condition of described hydro-thermal reaction comprises: temperature is 160-240 DEG C, and the time is 2-3h.
According to the present invention, described hydro-thermal reaction can be carried out under agitation, and such as can adopt the modes such as magnetic agitation, mechanical stirring, gas stirring, described stirring velocity can be such as 300-900r/min.
According to the present invention, after hydro-thermal reaction, the mixture of gained is carried out solid-liquid separation, liquid phase and solid phase can be obtained, wherein, described solid-liquid separation can adopt the separation means of this area routine to carry out, such as, can adopt the modes such as the filtration of filter press, slot type, belt filtration, centrifuging.
According to the present invention, by adopting the treatment process of described sodium vanadium extraction chromium residue, the liquid phase that sodium element content is higher can be obtained, such liquid phase can have multiple use, such as can by evaporation concentration carry compounds containing sodium or for regulate pH with etc., most preferred purposes is used as the alkaline reagents in the method for vanadium chromium slag sodium roasting vanadium-extracting provided by the invention and chromium the liquid phase of gained here, the consumption of compounds containing sodium can be reduced thus, and obtain the extraction effect of good vanadium and chromium.Preferably, in gained liquid phase, with Na
2the content of the sodium element of O meter is 20-50g/L, and the content of v element is 0.01-0.1g/L, and the content of chromium element is 0.08-0.5g/L; More preferably, with Na
2the content of the sodium element of O meter is 30-50g/L, and the content of v element is 0.02-0.05g/L, and the content of chromium element is 0.1-0.3g/L.
According to the present invention, by adopting the treatment process of described sodium vanadium extraction chromium residue, can obtain and have higher ferro element and the solid phase of calcium element content, such solid phase can serve many purposes, such as can be used as the slag former in blast furnace ironmaking, also may be used for preparing in the building materials such as brick.Pass through, in described solid phase, the content of ferro element is 25-35 % by weight and in the 19-30 % by weight of the calcium element content of CaO.
Present invention also offers a kind of method of vanadium chromium slag sodium roasting vanadium-extracting and chromium, the method comprises: vanadium chromium slag and compounds containing sodium are carried out roasting, and the material after described roasting is leached, wherein, described roasting is also carried out under alkaline reagents exists, and described alkaline reagents is the liquid phase of above-mentioned treatment process gained.
According to the present invention, described vanadium chromium slag can be the vanadium chromium slag after blowing containing vanadium chromium hot melt.Further, method of the present invention is applicable to the process of the vanadium chromium slag to any vanadium and chromium content, and under preferable case, be specially adapted in the vanadium chromium slag of method process of the present invention, the content of v element is 4-8 % by weight, and the content of chromium element is 8-14 % by weight.
According to the present invention, owing to present invention employs the liquid phase of the treatment process gained of above-mentioned sodium vanadium extraction chromium residue as alkaline reagents, containing sodium element in this alkaline reagents, therefore can the compounds containing sodium of Substitute For Partial, thus reduce the consumption of compounds containing sodium, preferably, relative to the described vanadium chromium slag of 100 weight parts, with Na
2the consumption of the described compounds containing sodium of O meter is 15-30 weight part, is more preferably 17-25 weight part.Preferably, relative to the described vanadium chromium slag of 100 weight parts, the consumption of described alkaline reagents is 5-40mL, be more preferably 10-30mL (relative to the liquid phase of aforesaid method gained composition, for the words of the alkaline reagents of other compositions, suitable conversion can be carried out according to consumption here, particularly convert according to the amount of contained sodium element).
According to the present invention, to described compounds containing sodium, there is no particular limitation, and can adopt the compounds containing sodium for vanadium chromium slag sodium roasting that this area routine adopts, such as described compounds containing sodium can be Na
2cO
3, NaCl, Na
2o, NaNO
3and Na
2sO
4in one or more, be preferably Na
2cO
3and/or NaCl.
According to the present invention, to described roasting condition, there is no particular limitation, can adopt the roasting condition of this area routine, and consider from the leaching yield of the vanadium improved after a while and chromium, preferably, the condition of described roasting comprises: temperature is 700-900 DEG C, and the time is 0.5-3h.More preferably, the condition of described roasting comprises: temperature is 850-900 DEG C, and the time is 1.5-3h.
According to the present invention, described leaching preferably adopts water logging, and the water adopted is preferably the hot water that temperature is 85-100 DEG C, and the time of water logging is preferably 1-2h.The present invention is not particularly limited the water yield adopted, and can change in wider scope, preferably, relative to the material after the roasting of 100g, the consumption of water is 200-500mL.
According to the present invention, after described leaching, carry out solid-liquid separation, obtain leach liquor and sodium vanadium extraction chromium residue, in order to can Leaching Vanadium and chromium more, can also with hot wash sodium vanadium extraction chromium residue 2-3 time, merging gained liquid phase is soaks have the leach liquor of vanadium and chromium.
According to the present invention, although present invention employs the compounds containing sodium that described alkaline reagents instead of part, method of the present invention also can obtain higher vanadium and the leaching yield of chromium, such as, the leaching yield of vanadium can reach more than 93%, and the leaching yield of chromium can reach more than 92%.
Below will be described the present invention by embodiment.
In following examples and comparative example, the leaching yield of vanadium refers to that the v element content in leach liquor accounts for the v element weight percent in reaction mass (comprising in vanadium chromium slag and alkaline reagents); The leaching yield of chromium refers to that the chromium constituent content in leach liquor accounts for the chromium element weight percent in reaction mass (comprising in vanadium chromium slag and alkaline reagents).
Embodiment 1
The present embodiment is for illustration of the treatment process of sodium vanadium extraction chromium residue of the present invention.
Get 50g sodium vanadium extraction chromium residue (with Na
2the content of the sodium element of O meter is 14 % by weight, V element content is 0.5 % by weight, Cr constituent content is 0.8 % by weight), 12.6gCaO (AR) and 250ml tap water join in reaction vessel, and (rotating speed is 500r/min), temperature are contact reacts 100min at 160 DEG C under magnetic stirring, react rear filtered on buchner funnel, obtain 200ml filtrate A1 (with Na
2the concentration of sodium element of O meter is 31.7g/L, and the concentration of V element is the concentration of 0.024g/L, Cr element is 0.09g/L) and 59g filter residue (with Na
2the content of the sodium element of O meter is 1.18 % by weight, V element content is 0.086 % by weight, Cr constituent content is 0.092 % by weight, Fe constituent content is 29.46 % by weight, S constituent content is 0.007 % by weight, P element content is 0.008 % by weight, is 20.46 % by weight in the content of the calcium constituent of CaO).
Embodiment 2
The present embodiment is for illustration of the treatment process of sodium vanadium extraction chromium residue of the present invention.
Get 40g sodium vanadium extraction chromium residue (with Na
2the content of the sodium element of O meter is 20 % by weight, V element content is 0.4 % by weight, Cr constituent content is 0.7 % by weight), 21.6gCaO (AR) and 300ml tap water join in reaction vessel, and (rotating speed is 500r/min), temperature are contact reacts 180min at 200 DEG C under magnetic stirring, react rear filtered on buchner funnel, obtain 244ml filtrate A2 (with Na
2the concentration of sodium element of O meter is 30.5g/L, and the concentration of V element is the concentration of 0.028g/L, Cr element is 0.1g/L) and 58.5g filter residue (with Na
2the content of the sodium element of O meter is 1.18 % by weight, V element content is 0.086 % by weight, Cr constituent content is 0.092 % by weight, Fe constituent content is 29.46 % by weight, S constituent content is 0.007 % by weight, P element content is 0.008 % by weight, is 20.46 % by weight in the content of the calcium constituent of CaO).
Embodiment 3
The present embodiment is for illustration of the treatment process of sodium vanadium extraction chromium residue of the present invention.
Get 40g sodium vanadium extraction chromium residue (with Na
2the content of the sodium element of O meter is 10 % by weight, V element content is 0.6 % by weight, Cr constituent content is 0.9 % by weight), 15gCaO (AR) and 250ml tap water join in reaction vessel, and (rotating speed is 500r/min), temperature are contact reacts 240min at 240 DEG C under magnetic stirring, react rear filtered on buchner funnel, obtain 100ml filtrate A3 (with Na
2the concentration of sodium element of O meter is 37.5g/L, and the concentration of V element is the concentration of 0.04g/L, Cr element is 0.18g/L) and 50.9g filter residue (with Na
2the content of the sodium element of O meter is 0.48 % by weight, and V element content is 0.1 % by weight, Cr constituent content is 0.1 % by weight, Fe constituent content is 30 % by weight, S constituent content is 0.007 % by weight, and P element content is 0.008 % by weight, is 19 % by weight in the content of the calcium constituent of CaO).
Embodiment 4
The present embodiment is for illustration of the method for vanadium chromium slag sodium roasting vanadium-extracting of the present invention and chromium.
Get 100g vanadium chromium slag (V element content is 5.17 % by weight, Cr constituent contents is 9.85 % by weight), 30gNa
2cO
3(AR) and 20ml alkaline reagents (i.e. the filtrate A1 of embodiment 1) mix after in 900 DEG C of roasting 2h, 90 DEG C of hot water stirs of grog (about 130g) 300ml obtained after roasting leach 1h, filter and use 60ml hot water to wash filter residue at twice after leaching, merge liquid phase and obtain leach liquor, leaching yield=95.4% of vanadium, leaching yield=93.9% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 119g (with Na
2the content of the sodium element of O meter is 10.5 % by weight, and V element content is 0.2 % by weight, Cr constituent content is 0.5 % by weight).
Embodiment 5
The present embodiment is for illustration of the method for vanadium chromium slag sodium roasting vanadium-extracting of the present invention and chromium.
Get 100g vanadium chromium slag (V element content is 7.01 % by weight, Cr constituent contents is 11.66 % by weight), 42gNa
2cO
3(AR) and 10ml alkaline reagents (i.e. the filtrate A2 of embodiment 2) mix after in 850 DEG C of roasting 3h, 85 DEG C of hot water stirs of grog (about 140g) 400ml obtained after roasting leach 1.5h, filter and use 60ml hot water to wash filter residue at twice after leaching, merge liquid phase and obtain leach liquor, leaching yield=92.5% of vanadium, leaching yield=93.2% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 131g (with Na
2the content of the sodium element of O meter is 16.4 % by weight, and V element content is 0.3 % by weight, Cr constituent content is 0.6 % by weight).
Embodiment 6
The present embodiment is for illustration of the method for vanadium chromium slag sodium roasting vanadium-extracting of the present invention and chromium.
Get 100g vanadium chromium slag (V element content is 7.55 % by weight, Cr constituent contents is 13.44 % by weight), 35gNa
2cO
3(AR) and 30ml alkaline reagents (i.e. the filtrate A3 of embodiment 3) mix after in 900 DEG C of roasting 2.5h, 95 DEG C of hot water stirs of grog (about 135g) 500ml obtained after roasting leach 2h, filter and use 70ml hot water to wash filter residue at twice after leaching, merge liquid phase and obtain leach liquor, leaching yield=96.6% of vanadium, leaching yield=95.3% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 127g (with Na
2the content of the sodium element of O meter is 18.9 % by weight, and V element content is 0.2 % by weight, Cr constituent content is 0.5 % by weight).
Embodiment 7
Method according to embodiment 4, difference is, adopts the sodium oxide of 17.5g to replace Na
2cO
3, obtain leach liquor, leaching yield=95.5% of vanadium, leaching yield=94.1% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 116g (with Na
2the content of the sodium element of O meter is 10.4 % by weight, and V element content is 0.2 % by weight, Cr constituent content is 0.5 % by weight).
Comparative example 1
Method according to embodiment 4, difference is, does not adopt alkaline reagents, obtains leach liquor, leaching yield=85.2% of vanadium, leaching yield=84.2% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 118g (with Na
2the content of the sodium element of O meter is 10 % by weight, and V element content is 0.65 % by weight, Cr constituent content is 1.32 % by weight).
Comparative example 2
Method according to embodiment 5, difference is, does not adopt alkaline reagents, but adopts total amount to be the Na of 70g
2cO
3, obtain leach liquor, leaching yield=90.3% of vanadium, leaching yield=89.7% of chromium; Dry filter residue obtains sodium vanadium extraction chromium residue 157g (with Na
2the content of the sodium element of O meter is 20 % by weight, and V element content is 0.44 % by weight, Cr constituent content is 0.76 % by weight).
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. the treatment process of a sodium vanadium extraction chromium residue, it is characterized in that, the method comprises: sodium vanadium extraction chromium residue, calcium containing compound and water are mixed and carry out hydro-thermal reaction, mixture after described hydro-thermal reaction is carried out solid-liquid separation, obtain liquid phase and solid phase, wherein, described sodium vanadium extraction chromium residue is the residue after vanadium chromium slag sodium roasting vanadium-extracting and chromium.
2. treatment process according to claim 1, wherein, relative to 100 weight parts with Na
2the sodium vanadium extraction chromium residue of O meter, in the consumption of the described calcium containing compound of CaO for 20-60 weight part, the consumption of water is 100-1000 weight part;
Preferably, relative to 100 weight parts with Na
2the sodium vanadium extraction chromium residue of O meter, in the consumption of the described calcium containing compound of CaO for 30-50 weight part, the consumption of water is 500-700 weight part;
Preferably, described calcium containing compound is one or more in calcium oxide, calcium chloride, calcium hydroxide, nitrocalcite and Calcium hydrogen carbonate.
3. treatment process according to claim 1 and 2, wherein, in described sodium vanadium extraction chromium residue, with Na
2the content of the sodium element of O meter is 10-20 % by weight, and the content of v element is 0.2-1 % by weight, and the content of chromium element is 0.5-1.2 % by weight.
4. according to the treatment process in claim 1-3 described in any one, wherein, the condition of described hydro-thermal reaction comprises: temperature is 95-300 DEG C, and the time is 0.5-5h.
5. according to the treatment process in claim 1-4 described in any one, wherein, in gained liquid phase, with Na
2the content of the sodium element of O meter is 20-50g/L, and the content of v element is 0.01-0.1g/L, and the content of chromium element is 0.08-0.5g/L.
6. the method for a vanadium chromium slag sodium roasting vanadium-extracting and chromium, the method comprises: vanadium chromium slag and compounds containing sodium are carried out roasting, and the material after described roasting is leached, it is characterized in that, described roasting is also carried out under alkaline reagents exists, and described alkaline reagents is the liquid phase of the treatment process gained in claim 1-5 described in any one.
7. method according to claim 6, wherein, relative to the described vanadium chromium slag of 100 weight parts, with Na
2the consumption of the described compounds containing sodium of O meter is 15-30 weight part, and the consumption of described alkaline reagents is 5-40mL.
8. the method according to claim 6 or 7, wherein, described compounds containing sodium is Na
2cO
3, NaCl, Na
2o, NaNO
3and Na
2sO
4in one or more.
9. according to the method in claim 6-8 described in any one, wherein, the condition of described roasting comprises: temperature is 700-900 DEG C, and the time is 0.5-3h.
10. according to the method in claim 6-9 described in any one, wherein, in described vanadium chromium slag, the content of v element is 4-8 % by weight, and the content of chromium element is 8-14 % by weight.
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