CN105087932A - Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide - Google Patents
Method for removing silicon in acid vanadium-enriched liquid and preparation method of vanadium oxide Download PDFInfo
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Abstract
The invention belongs to the field of steel smelting and particularly relates to a method for removing silicon impurities in acid vanadium-enriched liquid and a preparation method of high-purity vanadium oxide. The method for removing silicon in the acid vanadium-enriched liquid comprises the following steps that by weight, 5-25% of an aluminum-type-flocculant, 20-50% of bentonite and 25-75% of an addition agent are mixed to obtain a mixture; a binding agent and the mixture are mixed according to the weight ratio of 80-60:20-40 for pepeletizing, the mixture is soaked in water and dried to form a porous flocculation adsorbing agent, the porous flocculation adsorbing agent is added into the vanadium-enriched liquid according to the solid-liquid rate of 1:40-60 for stirring and standing, and the flocculation adsorbing agent is taken out to obtain the adsorbing agent. The method can be directly implemented on the acidic condition and meanwhile the problem that solid-liquid separation is hard during existing flocculation silicon removal can be solved. The obtained adsorbing agent is low in price, simple in production method, good in adsorbing effect and capable of being continuously and repeatedly used.
Description
Technical field
The invention belongs to field of iron and steel smelting, be specifically related to the minimizing technology of impurity silicon and the preparation method of high-purity vanadium oxide in a kind of rich acidic vanadium liquid.
Background technology
Vanadium is a kind of important strategic materials, and along with the development of science and technology, vanadium Application Areas constantly expands, simultaneously also more and more higher to the purity requirement of vanadium product.The novel process extracting vanadium is different, but processing step substantially all comprises five operations such as roasting, leaching, isolation of purified, precipitation, calcining substantially, leach by various technique the vanadium solution that contains obtained all to need through purifying treatment before entering subsequent processing, the existence of impurity affects follow-up precipitation, and has a strong impact on quality product.On current market, vanadium product category is various, but silicon in most of vanadium product, iron level is higher, so that high-purity Vanadium Pentoxide in FLAKES is expensive, especially with low silicon, and the vanadium valuable product of low iron.
The industrial major part of the purification silica removal containing vanadium leachate adds precipitation agent under alkaline environment at present at present, and staticly settle method, this method shortcoming is that silica removal rate is low, and time of repose is long, fine silica dioxide gel filtration difficulty, causes silicone content in vanadium product to exceed standard.And show according to available data research, vanadium cell industry has brighter development prospect, and the demand of market to electrolyte for vanadium cell is very big from now on.But impurity element silicon can damage battery diaphragm, greatly reduce the vanadium cell life-span.
For this problem, domesticly carry out more linguistic term, common for adding one or more flocculation agents or composite flocculation agent carries out silica removal, such as Zhang Xi, " research of desilicating process from vanadium-containing liquid " [J] of Zou Xiaoyong. inorganic chemicals industry, inquire into the mechanism of silica removal process in 2008,40 (4): 413. one literary compositions, have studied the kind of desiliconizing agent, consumption, pH value, temperature, time of repose to the impact of silica removal effect.Result shows: under weak basic condition, and add desiliconizing agent A and have good effect to desilicating process from vanadium-containing liquid, silica removal rate can reach more than 90%, and silica removal process can not cause the precipitation of vanadium in solution to lose.
Chen Cunguang, " application of composite flocculation agent in pickling liquor of steel sheet silicon removing process " of the people such as Shao Huiping, the method mentioned in one literary composition can remove impurity silicon preferably, but because being flocculation agent is directly added need in the solution of silica removal, inorganic flocculating agent can introduce its impurity element carried, and as Fe, Al, and the residual monomer of organic floculant superpolymer has " three cause " effect (causing rugged, carcinogenic, mutagenesis), thus make its range of application be restricted, be also unfavorable for Sustainable development.
Application number is " 201510155152.3 ", denomination of invention is " a kind of silicon removing method containing vanadium silicon solution and application ", disclose a kind of silicon removing method containing vanadium silicon solution, the method comprises: be under the condition of less than 5 in pH value, filters after contacting also co-precipitation containing vanadium silicon solution with desiliconizing agent; Wherein, described desiliconizing agent contains the polycarboxylic acid polymer containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain.The invention still further relates to polycarboxylic acid polymer containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain as the application of desiliconizing agent.This patent is by adopting polycarboxylic acid polymer containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain as desiliconizing agent, in acid condition by the silicon removing in vanadium-bearing hot metal, desiliconizing agent is complicated, cost is high, non-renewable utilization, be unfavorable for resources conservation, silica removal is not thorough, and vanadium has loss to a certain degree.
Therefore, invent a kind of pH value without regulator solution, can directly carry out in acid condition.Simultaneously, flocculation agent strong for throwing out can be fixed in flocculation adsorption agent particle, do not introduce the impurity that flocculation agent has, environmentally friendly, join after in liquid and do not have hazard residue, can carry out production repeatedly a large amount of for a long time, can effectively remove impurity silicon, and the method simultaneously preparing high-purity vanadium oxide is very necessary.
Summary of the invention
First technical problem to be solved by this invention be to provide a kind of can overcome existingly be difficult to be applied to the acid defect containing vanadium silicon solution system silica removal containing vanadium silicon solution silicon removing method, a kind of method can carrying out silica removal in acid condition to vanadium solution is provided.
The minimizing technology of silicon in rich acidic vanadium solution, comprise the preparation of porous flocculation adsorption agent and the removal step of impurity silicon, the preparation method of wherein porous flocculation adsorption agent is:
A, raw material prepare: according to weight percent, by AlSnSi alloy 5 ~ 25%, wilkinite 20 ~ 50%, additive 25 ~ 75%, mixing; Wherein, described bentonitic particle diameter < 10 μm;
B, granulation: according to weight ratio, the compound by a step obtains: binding agent=20 ~ 40:80 ~ 60, mixing, with extruding pelletization in twin screw extruder, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 72 ~ 144h in deionized water, dry under vacuum, obtains the agent of porous flocculation adsorption;
The minimizing technology of impurity silicon is:
Porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:40 ~ 60, adds rich vanadium liquid, stirring at low speed, leaves standstill, and takes out flocculation adsorption agent, to obtain final product.
AlSnSi alloy described above is conventional containing inorganic aluminium flocculating agent, and such as aluminium hydroxide, potassium aluminium sulfate, Tai-Ace S 150, poly-phosphorus aluminum chloride, aluminium iron polychloride etc. are inorganic containing aluminium flocculating agent.
The purification of above-mentioned wilkinite needs and process in early stage, be specially pure for the elution of bentonite origin mineral water, oven dry, pulverize, by sieve, select the powder body material of grain diameter < 10um.
Additive described above is at least one in soluble sodium salt and sylvite, such as, at least one in sodium-chlor, sodium sulfate, sodium carbonate, Repone K, potassium sulfate, salt of wormwood, in the present invention, additive can be leached in later stage water logging, flocculation agent is made to form the additive playing skeleton function of vesicular structure, the present invention in order to cost-saving, preferred sodium-chlor.
Further, in order to obtain preferred technical scheme, the minimizing technology of silicon in rich acidic vanadium solution described above, a step Raw is preferably according to weight percent: AlSnSi alloy 5 ~ 15%, wilkinite 20 ~ 40%, sodium-chlor 55 ~ 65%.
The minimizing technology of silicon in rich acidic vanadium solution described above, in b step, binding agent is at least one in polypropylene PP, polythene PE.
Further, in order to obtain preferred technical scheme, the minimizing technology of silicon in rich acidic vanadium solution described above, wherein, preferably in deionized water the flocculation adsorption agent particle after granulating is soaked 80 ~ 100h completely in step c, change a water every 24h, guarantee that the additives such as the sodium-chlor in particle are all soluble in water, form maximum flocculation adsorption holes.
The minimizing technology of silicon in rich acidic vanadium solution described above, in step c, vacuum-drying is dry 8 ~ 24h under 80 ~ 120 DEG C of vacuum environments, and described vacuum environment can for dry in vacuum drying oven.
The removal of silicon in rich acidic vanadium solution described above, wherein, stirring at low speed 1 ~ 2h after rich vanadium liquid is added in described Step d, leave standstill 5 ~ 10h, stirring at low speed speed is 120 ~ 300r/min, stirring at low speed of the present invention is to ensure that desiliconizing agent compares fully with solution reaction, can also prevent from being destroyed by flucculation structure after the impurity after adsorbing at high speeds its flocculation.Take out the flocculation adsorption agent of having adsorbed silicon, namely achieve the present invention by the object of the removal of impurity silicon in rich acidic vanadium liquid.
Second technical problem to be solved by this invention is to provide a kind of preparation method of high-purity vanadium oxide.
The preparation method of vanadium oxide of the present invention, comprises the following steps:
1., the impurity silicon in rich vanadium liquid is removed according to the minimizing technology of silicon in rich acidic vanadium solution described above;
2., will remove the rich vanadium solution heating of silicon in 1. step, conventionally, add precipitation agent deposition, filter, washing, dry, calcining, obtains vanadium oxide.
The removal of silicon and the preparation method of vanadium oxide in this invention rich acidic vanadium solution, have following beneficial effect:
1. the silicon removing method that uses of the present invention with current prepare high-purity vanadium oxide product compared with the flocculent precipitation commonly used, without the pH value of regulator solution, can directly carry out in acid condition.Meanwhile, AlSnSi alloy strong for throwing out can be fixed in flocculation adsorption agent particle, not introduce the impurity that flocculation agent has.Wilkinite is environmentally friendly, joins after in liquid and does not have hazard residue.
2. the product that prepared by the present invention can remove impurity elemental silicon preferably, element silicon in sour environment can be become the throw out of large volume by aluminium flocculating agent from the tiny gelular ion bridging be polymerized to, adding bentonitic strong adsorption, the silica-based instinct in solution is less than 0.03g/L.Meanwhile, the problem that in original flocculation silica removal, solid-liquid separation is more difficult is also solved.
3. prepare Adsorber section in the present invention, the material price of use is cheap, the method for production is simple, advantages of good adsorption effect, can serialization, suitability for industrialized production.
4. the sorbent material in the present invention can Reusability, adsorbent to a certain extent after, can put it in alkali lye, until after the silicon impurities dissolves that adsorbs above of sorbent material, Yu Shuizhong cleans and can reuse after drying.
Embodiment
The minimizing technology of silicon in rich acidic vanadium solution of the present invention, comprise the preparation of porous flocculation adsorption agent and the removal step of impurity silicon, the preparation method of wherein porous flocculation adsorption agent is:
A, raw material prepare: according to weight percent, by AlSnSi alloy 5 ~ 25%, wilkinite 20 ~ 50%, additive 25 ~ 75%, mixing; Wherein, described bentonitic particle diameter < 10 μm;
B, granulation: according to weight ratio, the compound by a step obtains: binding agent=20 ~ 40:80 ~ 60, mixing, with extruding pelletization in twin screw extruder, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 72 ~ 144h in deionized water, dry under vacuum, obtains the agent of porous flocculation adsorption;
The minimizing technology of impurity silicon is:
Porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:40 ~ 60, adds rich vanadium liquid, stirring at low speed, leaves standstill, and takes out flocculation adsorption agent, to obtain final product.
AlSnSi alloy described above is conventional containing inorganic aluminium flocculating agent, and such as aluminium hydroxide, potassium aluminium sulfate, Tai-Ace S 150, poly-phosphorus aluminum chloride, aluminium iron polychloride etc. are inorganic containing aluminium flocculating agent.
The purification of above-mentioned wilkinite needs and process in early stage, be specially pure for the elution of bentonite origin mineral water, oven dry, pulverize, by sieve, select the powder body material of grain diameter < 10um.
Additive described above is at least one in soluble sodium salt and sylvite, such as, at least one in sodium-chlor, sodium sulfate, sodium carbonate, Repone K, potassium sulfate, salt of wormwood, in the present invention, additive can be leached in later stage water logging, flocculation agent is made to form the additive playing skeleton function of vesicular structure, the present invention in order to cost-saving, preferred sodium-chlor.
Further, in order to obtain preferred technical scheme, the minimizing technology of silicon in rich acidic vanadium solution described above, a step Raw is preferably according to weight percent: AlSnSi alloy 5 ~ 15%, wilkinite 20 ~ 40%, sodium-chlor 55 ~ 65%.
The minimizing technology of silicon in rich acidic vanadium solution described above, in b step, binding agent is at least one in polypropylene PP, polythene PE.
Further, in order to obtain preferred technical scheme, the minimizing technology of silicon in rich acidic vanadium solution described above, wherein, preferably in deionized water the flocculation adsorption agent particle after granulating is soaked 80 ~ 100h completely in step c, change a water every 24h, guarantee that the additives such as the sodium-chlor in particle are all soluble in water, form maximum flocculation adsorption holes.
The minimizing technology of silicon in rich acidic vanadium solution described above, in step c, vacuum-drying is dry 8 ~ 24h under 80 ~ 120 DEG C of vacuum environments, and described vacuum environment can for dry in vacuum drying oven.
The removal of silicon in rich acidic vanadium solution described above, wherein, stirring at low speed 1 ~ 2h after rich vanadium liquid is added in described Step d, leave standstill 5 ~ 10h, stirring at low speed speed is 120 ~ 300r/min, stirring at low speed of the present invention is to ensure that desiliconizing agent compares fully with solution reaction, can also prevent from being destroyed by flucculation structure after the impurity after adsorbing at high speeds its flocculation.Take out the flocculation adsorption agent of having adsorbed silicon, namely achieve the present invention by the object of the removal of impurity silicon in rich acidic vanadium liquid.
The preparation method of vanadium oxide of the present invention, comprises the following steps:
1., the impurity silicon in rich vanadium liquid is removed according to the minimizing technology of silicon in rich acidic vanadium solution described above;
2., will remove the rich vanadium solution heating of silicon in 1. step, conventionally, add precipitation agent deposition, filter, washing, dry, calcining, obtains vanadium oxide.
Below in conjunction with embodiment, the specific embodiment of the present invention is further described, does not therefore limit the present invention among described scope of embodiments.
Embodiment 1
A, raw material prepare: by pure for the elution of bentonite origin mineral water, oven dry, pulverize, by sieve, select the powder body material of grain diameter < 10um, according to weight percent, by AlSnSi alloy 5%, wilkinite 40%, sodium-chlor 55%, mixing, obtains compound;
B, granulation: according to weight ratio, the compound by a step obtains: PP=40:60, mixing, with extruding pelletization in twin screw extruder, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 90h in deionized water, then in vacuum drying oven dry 24h at 80 DEG C, obtain the agent of porous flocculation adsorption;
The removal of d, silicon: porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:45, adds rich vanadium liquid, low speed stirring at normal temperature 1.5h, leaves standstill 8h, filters, and takes out flocculation adsorption agent.
Measuring silicone content in rich vanadium solution is on pretreatment 1.256g/L, and vanadium solution concentration is 15.921g/L; After adding flocculation agent absorption silicon, recording silicone content in solution with ICP is 0.023g/L, and vanadium concentration is 15.732g/L.
Embodiment 2
A, raw material prepare: by pure for the elution of bentonite origin mineral water, oven dry, pulverize, by sieve, select the powder body material of grain diameter < 10um, according to weight percent, by AlSnSi alloy 10%, wilkinite 35%, sodium-chlor 55%, mixing, obtains compound;
B, granulation: according to weight ratio, the compound by a step obtains: PP=50:50, mixing, with extruding pelletization in twin screw extruder, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 80h in deionized water, then in vacuum drying oven dry 10h at 120 DEG C, obtain the agent of porous flocculation adsorption;
The removal of d, silicon: porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:55, adds rich vanadium liquid, low speed stirring at normal temperature 80mim, leaves standstill 7h, filters, and takes out flocculation adsorption agent.
Measuring silicone content in rich vanadium solution is on pretreatment 1.256g/L, and vanadium solution concentration is 15.921g/L; After adding flocculation agent absorption silicon, recording silicone content in solution is 0.019g/L, and vanadium concentration is 15.832g/L.
Embodiment 3
A, raw material prepare: by pure for the elution of bentonite origin mineral water, oven dry, pulverize, by sieve, select the powder body material of grain diameter < 10um, according to weight percent, by AlSnSi alloy 15%, wilkinite 20%, sodium-chlor 65%, mixing, obtains compound;
B, granulation: according to weight ratio, the compound by a step obtains: PP=30:70, mixing, with extruding pelletization in twin screw extruder, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 100h in deionized water, then in vacuum drying oven dry 15h at 100 DEG C, obtain the agent of porous flocculation adsorption;
The removal of d, silicon: porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:55, adds rich vanadium liquid, low speed stirring at normal temperature 70mim, leaves standstill 9h, filters, and takes out flocculation adsorption agent.
Measuring silicone content in rich vanadium solution is on pretreatment 1.256g/L, and vanadium solution concentration is 15.921g/L; After adding flocculation agent absorption silicon, recording silicone content in solution is 0.017g/L, and vanadium concentration is 15.815g/L.
Claims (9)
1. the minimizing technology of silicon in rich acidic vanadium solution, comprises the preparation of porous flocculation adsorption agent and the removal step of impurity silicon, it is characterized in that:
The preparation method of porous flocculation adsorption agent is:
A, raw material prepare: according to weight percent, by AlSnSi alloy 5 ~ 25%, wilkinite 20 ~ 50%, additive 25 ~ 75%, and mixing, obtains compound; Wherein, described bentonitic particle diameter < 10 μm;
B, granulation: according to weight ratio, the compound by a step obtains: binding agent=20 ~ 40:80 ~ 60, mixing, granulation, obtains the agent of granulating flocculation adsorption;
The formation in c, hole: granulating flocculation adsorption agent b step obtained, soaks 72 ~ 144h in water, dry under vacuum, obtains the agent of porous flocculation adsorption;
The minimizing technology of impurity silicon is:
Porous flocculation adsorption agent step c prepared, according to solid-to-liquid ratio 1:40 ~ 60, adds rich vanadium liquid, stirs, and leaves standstill, and takes out flocculation adsorption agent, to obtain final product.
2. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1, is characterized in that: a step Raw according to weight percent is: AlSnSi alloy 5 ~ 15%, wilkinite 20 ~ 40%, additive 55 ~ 65%.
3. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1 or 2, is characterized in that: described AlSnSi alloy is at least one in aluminium hydroxide, potassium aluminium sulfate, Tai-Ace S 150, poly-phosphorus aluminum chloride, aluminium iron polychloride.
4. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1 or 2, is characterized in that: described additive is at least one in sodium-chlor, sodium sulfate, sodium carbonate, Repone K, potassium sulfate, salt of wormwood, is preferably sodium-chlor.
5. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1, is characterized in that: in b step, binding agent is at least one in polypropylene, polyethylene.
6. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1, is characterized in that: granulating flocculation adsorption agent b step obtained in step c, soaks 80 ~ 100h, change a water every 24h in water.
7. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1, is characterized in that: dry in step c is 8 ~ 24h dry under 80 ~ 120 DEG C of vacuum environments.
8. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1, is characterized in that: after stirring 1 ~ 2h after adding rich vanadium liquid in Step d, leave standstill 5 ~ 10h, stir speed (S.S.) is 120 ~ 300r/min.
9. the preparation method of vanadium oxide, is characterized in that: comprise the following steps:
1., the impurity silicon in rich vanadium liquid is removed according to the minimizing technology of silicon in rich acidic vanadium solution described in any one of claim 1 ~ 8;
2., will remove the rich vanadium solution heating of silicon in 1. step, add precipitation agent deposition, filter, washing, dry, calcining, obtains vanadium oxide.
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