CN105087932B - The preparation method of the minimizing technology of silicon and vanadium oxide in rich acidic vanadium liquid - Google Patents
The preparation method of the minimizing technology of silicon and vanadium oxide in rich acidic vanadium liquid Download PDFInfo
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Abstract
The invention belongs to field of iron and steel smelting, and in particular to the preparation method of the minimizing technology of impurity silicon and high-purity vanadium oxide in a kind of rich acidic vanadium liquid.The minimizing technology of silicon, comprises the following steps in rich acidic vanadium solution of the present invention：According to percentage by weight, by AlSnSi alloy 5~25%, bentonite 20~50%, additive 25~75%, mixing obtains compound；According to weight ratio, by binding agent:Compound=80~60:20~40, mixing, pelletizing is soaked in water, is dried, and porous flocculation adsorption agent is formed, according to solid-to-liquid ratio 1:40~60, it is added in rich vanadium liquid, stirs, stand, takes out flocculation adsorption agent, produce.The present invention can be carried out directly in acid condition, simultaneously, moreover it is possible to solved original flocculation and removed the problem of separation of solid and liquid is more difficult in silicon.The adsorbent that is prepared in the present invention is cheap, production method is simple, advantages of good adsorption effect, can continuously repeating use.
Description
Technical field
The invention belongs to field of iron and steel smelting, and in particular to the minimizing technology of impurity silicon and high-purity in a kind of rich acidic vanadium liquid
The preparation method of vanadium oxide.
Background technology
Vanadium is a kind of important strategic materials, and with the development of science and technology, vanadium application field constantly expands, while to vanadium
The purity requirement of product also more and more higher.Extract vanadium new technology it is different, but substantially processing step substantially all include roasting,
Five operations such as leaching, isolation of purified, precipitation, calcining, are entering subsequent processing with what the leaching of various techniques was obtained containing vanadium solution
Before be required for by purified treatment, the presence of impurity influences follow-up precipitation, and has a strong impact on product quality.Vanadium on current market
Product category is various, but silicon in most of vanadium product, and iron content is higher, so that high-purity vanadic anhydride is expensive, especially with low
Silicon, the vanadium valuable product of low iron.
The industrial purification containing vanadium leachate at present largely adds precipitating reagent except silicon under alkaline environment, and it is heavy to stand
Shallow lake method, the method has the disadvantage that time of repose is long, fine silica dioxide gel filtration difficulty, causes in vanadium product except silicon rate is low
Silicone content is exceeded.And show that vanadium cell industry has brighter development prospect, and market is to vanadium from now on according to available data research
The demand of battery electrolytic solution is very big.But impurity element silicon can damage battery diaphragm, reduce the vanadium cell life-span significantly.
For the problem, the country has carried out more linguistic term, common for addition one or more flocculants or multiple
Flocculant is closed to carry out except silicon, such as Zhang Xi, Zou Xiaoyong's《The research of desilicating process from vanadium-containing liquid》[J] inorganic chemicals industries,
2008,40 (4):The mechanism except silicon process has been inquired into 413. 1 texts, have studied the species of desiliconizing agent, consumption, pH value, temperature,
Time of repose is to the influence except silicon effect.As a result show：Under weak basic condition, addition desiliconizing agent A removes silicon mistake to solution containing vanadium body
Journey has good effect, except silicon rate is up to more than 90%, and except silicon process does not result in the precipitation loss of vanadium in solution.
Chen Cunguang, Shao Huiping's et al.《Application of the composite flocculation agent in pickling liquor of steel sheet silicon removing process》, carry in a text
To method can preferably remove impurity silicon, but because being that be directly added into flocculant need to be except in the solution of silicon, inorganic flocculating agent
Its impurity element carried, such as Fe, Al can be introduced, and there is the residual monomer of organic flocculant high polymer " three cause " effect (to cause
Rugged, carcinogenic, mutagenesis), thus its application is restricted, also it is unfavorable for sustainable development.
Application No. " 201510155152.3 ", entitled " a kind of silicon removing method of solution of silicon containing vanadium and application ",
A kind of silicon removing method of the solution of silicon containing vanadium is disclosed, this method includes：Under conditions of pH value is less than 5, vanadium silicon solution will be contained
Filtered after contacting and be co-precipitated with desiliconizing agent；Wherein, the desiliconizing agent contains containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain
Polycarboxylic acid polymer.The invention further relates to the polycarboxylic acid polymer containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain
It is used as the application of desiliconizing agent.The patent polymerize by using the polycarboxylic-acid containing carboxylic acid group, sulfonic group and polyoxyethylene base side chain
Thing in acid condition removes the silicon in vanadium-bearing hot metal as desiliconizing agent, and desiliconizing agent is complicated, and cost is high, non-renewable to utilize,
It is unfavorable for resources conservation, except silicon is not thorough, and vanadium has a certain degree of loss.
Therefore, a kind of pH value without adjusting solution is invented, directly can be carried out in acid condition.Meanwhile, it will can wad a quilt with cotton
The strong flocculant of solidifying effect is fixed in flocculation adsorption agent particle, and the impurity that flocculant has is not introduced, environmentally friendly, plus
Hazard residue is not had after entering into liquid, can carry out it is long-term it is substantial amounts of produce repeatedly, can effectively remove impurity silicon, and simultaneously
The method that high-purity vanadium oxide can be prepared is very necessary.
The content of the invention
First technical problem to be solved by this invention, which is to provide one kind, can overcome the existing solution of silicon containing vanadium to remove silicon
The solution system of silicon containing vanadium that method is dfficult to apply to acidity can be in acid condition to vanadium solution there is provided one kind except the defect of silicon
Carry out the method except silicon.
The minimizing technology of silicon in rich acidic vanadium solution, includes preparation and the removal step of impurity silicon of porous flocculation adsorption agent
Suddenly, wherein the preparation method of porous flocculation adsorption agent is：
A, raw material prepare：According to percentage by weight, by AlSnSi alloy 5~25%, bentonite 20~50%, additive 25
~75%, mixing；Wherein, 10 μm of the bentonitic particle diameter ＜；
B, granulation：According to weight ratio, the compound that a steps are obtained:Binding agent=20~40:80~60, mixing, with double
Extruding pelletization in screw extruder, obtains granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks 72~144h, vacuum in deionized water
Lower drying, obtains porous flocculation adsorption agent；
The minimizing technology of impurity silicon is：
The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:40~60, rich vanadium liquid is added, low speed is stirred
Mix, stand, take out flocculation adsorption agent, produce.
AlSnSi alloy described above contains inorganic aluminium flocculating agent to be conventional, for example aluminium hydroxide, alum, aluminum sulfate,
Poly- phosphorus aluminium chloride, PAFC etc. are inorganic to contain aluminium flocculating agent.
Above-mentioned bentonite needs to purify and early stage processing, is specially that bentonite origin mineral water is eluted into pure, drying, crushed, uses
Sieve, from grain diameter ＜ 10um powder body material.
Additive described above is at least one of soluble sodium salt and sylvite, such as sodium chloride, sodium sulphate, carbonic acid
Additive can be leached in later stage water logging at least one of sodium, potassium chloride, potassium sulfate, potassium carbonate, the present invention, make wadding
Solidifying dosage form is into the additive for playing skeleton function of loose structure, and the present invention is in order to cost-effective, preferred sodium chloride.
Further, in order to obtain the minimizing technology of silicon in preferred technical scheme, rich acidic vanadium solution described above, a
Raw material is preferably according to percentage by weight in step：AlSnSi alloy 5~15%, bentonite 20~40%, sodium chloride 55~
65%.
In rich acidic vanadium solution described above in the minimizing technology of silicon, b step binding agent be polypropylene PP, polythene PE in
At least one.
Further, in order to obtain the minimizing technology of silicon in preferred technical scheme, rich acidic vanadium solution described above, its
In, it is preferably that the flocculation adsorption agent particle after granulating is completely soaked 80~100h in deionized water in step c, every 24h
Change a water, it is ensured that the additive such as sodium chloride in particle is all soluble in water, form most flocculation adsorption holes.
Vacuum drying is in 80~120 DEG C of vacuum rings in the minimizing technology of silicon, step c in rich acidic vanadium solution described above
8~24h is dried under border, the vacuum environment can be to be dried in vacuum drying chamber.
The removal of silicon in rich acidic vanadium solution described above, wherein, stirring at low speed 1 after rich vanadium liquid is added in the Step d
~2h, stand 5~10h, stirring at low speed speed be 120~300r/min, stirring at low speed of the present invention be in order to ensure desiliconizing agent with
Solution reaction is more abundant, be also prevented from it is adsorbed after impurity flocculent structure is destroyed after its flocculation at high speeds.Take out
The flocculation adsorption agent of silicon has been adsorbed, that is, has realized the present invention by the purpose 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., the rich vanadium solution that silicon is removed in 1. step is heated, conventionally, plus precipitation agent deposition, filtering, wash
Wash, dry, calcining produces vanadium oxide.
The removal of silicon and the preparation method of vanadium oxide, have the advantages that in the invention rich acidic vanadium solution：
1. the silicon removing method that the present invention is used compared with preparing the flocculent precipitation that high-purity vanadium oxide product is commonly used at present
Compared with, without adjust solution pH value, directly can carry out in acid condition.Meanwhile, the strong aluminium system of flocculation can be flocculated
Agent is fixed in flocculation adsorption agent particle, and the impurity that flocculant has is not introduced.Bentonite is environmentally friendly, is added to liquid
In after do not have hazard residue.
2. product prepared by the present invention can preferably remove impurity elemental silicon, aluminium flocculating agent can will in sour environment silicon member
Flocculate of the element from the tiny gelular ion bridging that is polymerized into large volume, plus bentonitic strong suction-operated, in solution
Silicon substrate instinct is less than 0.03g/L.Meanwhile, also solve original flocculation and remove the problem of separation of solid and liquid is more difficult in silicon.
3. preparing Adsorber section in the present invention, the material price used is cheap, production method is simple, adsorption effect
It is good, can serialization, industrialized production.
4. the adsorbent in the present invention after adsorbent absorption to a certain extent, be able to can be put it into Reusability
In alkali lye, until after the sila matter dissolving that adsorbent is adsorbed above, can be reused after cleaning and dry in water.
Embodiment
The minimizing technology of silicon in rich acidic vanadium solution of the present invention, including the preparation of porous flocculation adsorption agent and going for impurity silicon
Except step, wherein the preparation method of porous flocculation adsorption agent is：
A, raw material prepare：According to percentage by weight, by AlSnSi alloy 5~25%, bentonite 20~50%, additive 25
~75%, mixing；Wherein, 10 μm of the bentonitic particle diameter ＜；
B, granulation：According to weight ratio, the compound that a steps are obtained:Binding agent=20~40:80~60, mixing, with double
Extruding pelletization in screw extruder, obtains granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks 72~144h, vacuum in deionized water
Lower drying, obtains porous flocculation adsorption agent；
The minimizing technology of impurity silicon is：
The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:40~60, rich vanadium liquid is added, low speed is stirred
Mix, stand, take out flocculation adsorption agent, produce.
AlSnSi alloy described above contains inorganic aluminium flocculating agent to be conventional, for example aluminium hydroxide, alum, aluminum sulfate,
Poly- phosphorus aluminium chloride, PAFC etc. are inorganic to contain aluminium flocculating agent.
Above-mentioned bentonite needs to purify and early stage processing, is specially that bentonite origin mineral water is eluted into pure, drying, crushed, uses
Sieve, from grain diameter ＜ 10um powder body material.
Additive described above is at least one of soluble sodium salt and sylvite, such as sodium chloride, sodium sulphate, carbonic acid
Additive can be leached in later stage water logging at least one of sodium, potassium chloride, potassium sulfate, potassium carbonate, the present invention, make wadding
Solidifying dosage form is into the additive for playing skeleton function of loose structure, and the present invention is in order to cost-effective, preferred sodium chloride.
Further, in order to obtain the minimizing technology of silicon in preferred technical scheme, rich acidic vanadium solution described above, a
Raw material is preferably according to percentage by weight in step：AlSnSi alloy 5~15%, bentonite 20~40%, sodium chloride 55~
65%.
In rich acidic vanadium solution described above in the minimizing technology of silicon, b step binding agent be polypropylene PP, polythene PE in
At least one.
Further, in order to obtain the minimizing technology of silicon in preferred technical scheme, rich acidic vanadium solution described above, its
In, it is preferably that the flocculation adsorption agent particle after granulating is completely soaked 80~100h in deionized water in step c, every 24h
Change a water, it is ensured that the additive such as sodium chloride in particle is all soluble in water, form most flocculation adsorption holes.
Vacuum drying is in 80~120 DEG C of vacuum rings in the minimizing technology of silicon, step c in rich acidic vanadium solution described above
8~24h is dried under border, the vacuum environment can be to be dried in vacuum drying chamber.
The removal of silicon in rich acidic vanadium solution described above, wherein, stirring at low speed 1 after rich vanadium liquid is added in the Step d
~2h, stand 5~10h, stirring at low speed speed be 120~300r/min, stirring at low speed of the present invention be in order to ensure desiliconizing agent with
Solution reaction is more abundant, be also prevented from it is adsorbed after impurity flocculent structure is destroyed after its flocculation at high speeds.Take out
The flocculation adsorption agent of silicon has been adsorbed, that is, has realized the present invention by the purpose 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., the rich vanadium solution that silicon is removed in 1. step is heated, conventionally, plus precipitation agent deposition, filtering, wash
Wash, dry, calcining produces vanadium oxide.
The embodiment of the present invention is further described with reference to embodiment, not therefore by present invention limit
System is among described scope of embodiments.
Embodiment 1
A, raw material prepare：Bentonite origin mineral water is eluted into pure, drying, crushed, with sieve, from grain diameter ＜
10um powder body material, according to percentage by weight, by AlSnSi alloy 5%, bentonite 40%, sodium chloride 55%, mixing is obtained
Compound；
B, granulation：According to weight ratio, the compound that a steps are obtained:PP=40:60, mixing, with double screw extruder
Extruding pelletization, obtains granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks 90h in deionized water, then dry in vacuum
24h is dried in dry case at 80 DEG C, porous flocculation adsorption agent is obtained；
D, silicon removal：The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:45, rich vanadium liquid is added,
Low speed stirring at normal temperature 1.5h, stands 8h, and flocculation adsorption agent is taken out in filtering.
It is 1.256g/L that silicone content in rich vanadium solution is determined before experiment, and vanadium solution concentration is 15.921g/L；Add flocculation
After agent absorption silicon, it is 0.023g/L that silicone content in solution is measured with ICP, and vanadium concentration is 15.732g/L.
Embodiment 2
A, raw material prepare：Bentonite origin mineral water is eluted into pure, drying, crushed, with sieve, from grain diameter ＜
10um powder body material, according to percentage by weight, by AlSnSi alloy 10%, bentonite 35%, sodium chloride 55%, mixing is obtained
To compound；
B, granulation：According to weight ratio, the compound that a steps are obtained:PP=50:50, mixing, with double screw extruder
Extruding pelletization, obtains granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks 80h in deionized water, then dry in vacuum
10h is dried in dry case at 120 DEG C, porous flocculation adsorption agent is obtained；
D, silicon removal：The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:55, rich vanadium liquid is added,
Low speed stirring at normal temperature 80mim, stands 7h, and flocculation adsorption agent is taken out in filtering.
It is 1.256g/L that silicone content in rich vanadium solution is determined before experiment, and vanadium solution concentration is 15.921g/L；Add flocculation
After agent absorption silicon, it is 0.019g/L to measure silicone content in solution, and vanadium concentration is 15.832g/L.
Embodiment 3
A, raw material prepare：Bentonite origin mineral water is eluted into pure, drying, crushed, with sieve, from grain diameter ＜
10um powder body material, according to percentage by weight, by AlSnSi alloy 15%, bentonite 20%, sodium chloride 65%, mixing is obtained
To compound；
B, granulation：According to weight ratio, the compound that a steps are obtained:PP=30:70, mixing, with double screw extruder
Extruding pelletization, obtains granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks 100h in deionized water, then in vacuum
15h is dried in drying box at 100 DEG C, porous flocculation adsorption agent is obtained；
D, silicon removal：The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:55, rich vanadium liquid is added,
Low speed stirring at normal temperature 70mim, stands 9h, and flocculation adsorption agent is taken out in filtering.
It is 1.256g/L that silicone content in rich vanadium solution is determined before experiment, and vanadium solution concentration is 15.921g/L；Add flocculation
After agent absorption silicon, it is 0.017g/L to measure silicone content in solution, and vanadium concentration is 15.815g/L.
Claims (9)
1. the minimizing technology of silicon in rich acidic vanadium solution, includes preparation and the removal step of impurity silicon of porous flocculation adsorption agent,
It is characterized in that：
The preparation method of porous flocculation adsorption agent is：
A, raw material prepare：According to percentage by weight, by AlSnSi alloy 5~25%, bentonite 20~50%, additive 25~
75%, mixing obtains compound；Wherein, 10 μm of the bentonitic particle diameter ＜；
B, granulation：According to weight ratio, the compound that a steps are obtained:Binding agent=20~40:80~60, mix, granulation is obtained
To granulating flocculation adsorption agent；
C, the formation in hole：The granulating flocculation adsorption agent that b step is obtained, soaks under 72~144h, vacuum in water and dries, obtain
Porous flocculation adsorption agent；
The minimizing technology of impurity silicon is：
The porous flocculation adsorption agent that step c is prepared is according to solid-to-liquid ratio 1:40~60, rich vanadium liquid is added, is stirred, stands, takes
Go out flocculation adsorption agent, produce.
2. according to claim 1 in rich acidic vanadium solution silicon minimizing technology, it is characterised in that：In a steps raw material according to
Percentage by weight is：AlSnSi alloy 5~15%, bentonite 20~40%, additive 55~65%.
3. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1 or claim 2, it is characterised in that：The aluminium system flocculation
Agent is at least one of aluminium hydroxide, alum, aluminum sulfate, poly- phosphorus aluminium chloride, PAFC.
4. the minimizing technology of silicon in rich acidic vanadium solution according to claim 1 or claim 2, it is characterised in that：The additive is
At least one of sodium chloride, sodium sulphate, sodium carbonate, potassium chloride, potassium sulfate, potassium carbonate, preferably sodium chloride.
5. according to claim 1 in rich acidic vanadium solution silicon minimizing technology, it is characterised in that：Binding agent is in b step
At least one of polypropylene, polyethylene.
6. according to claim 1 in rich acidic vanadium solution silicon minimizing technology, it is characterised in that：B step is obtained in step c
The granulating flocculation adsorption agent arrived, soaks 80~100h in water, and a water is changed every 24h.
7. according to claim 1 in rich acidic vanadium solution silicon minimizing technology, it is characterised in that：In step c dry be
8~24h is dried under 80~120 DEG C of vacuum environments.
8. according to claim 1 in rich acidic vanadium solution silicon minimizing technology, it is characterised in that：Stirred after adding rich vanadium liquid
After 1~2h, 5~10h is stood, stir speed (S.S.) is 120~300r/min.
9. the preparation method of vanadium oxide, it is characterised in that：Comprise the following steps：
1. the impurity in rich vanadium liquid, is removed according to the minimizing technology of silicon in any one of the claim 1~8 rich acidic vanadium solution
Silicon；
2., the rich vanadium solution that silicon is removed in 1. step is heated, plus precipitation agent deposition, filter, wash, dry, calcining produces oxygen
Change vanadium.
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| CN111634952B (en) * | 2020-07-24 | 2022-07-19 | 中钢集团南京新材料研究院有限公司 | Method for preparing iron oxide red by using ferrous sulfate as byproduct of titanium dioxide, product and application |
| CN112646972B (en) * | 2020-11-13 | 2021-12-24 | 北京科技大学 | Method for separating vanadium and chromium from vanadium and chromium-containing material through chlorination-selective oxidation |
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