CN103194603A - Preparation method of high-purity vanadium pentoxide - Google Patents
Preparation method of high-purity vanadium pentoxide Download PDFInfo
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Abstract
The invention discloses a preparation method of high-purity vanadium pentoxide. The method comprises the following steps of: a, grinding a vanadium-containing raw material, and removing iron; b, performing sodium roasting on the raw material treated in the step a, and leaching to obtain the vanadium-containing solution; c, removing cation impurities and anion impurities from the vanadium-containing solution obtained in the step b, and filtering to obtain the purified vanadium-containing solution; d, adding ammonium sulfate into the purified vanadium-containing solution to perform molybdenum precipitation treatment, filtering, washing and removing impurities to obtain vanadate precipitate; and e, pulping and filtering the vanadate precipitate, washing, further removing impurities in the vanadate precipitate, drying and roasting to obtain a vanadium pentoxide product. By virtue of the strict and effective impurity removal treatment, the purity of the vanadium pentoxide product can be increased, and can be over 99 percent.
Description
Technical field
The invention belongs to field of metallurgy, be specifically related to a kind of preparation method of high purity vanadic anhydride.
Background technology
The high-purity mangesium oxide vanadium has higher added value, can be used for industries such as metallurgy, chemical industry, medicine, the energy, environmental protection, aerospace.According to statistics, 2007, domestic to high-purity vanadium oxide product consumption about 3500 tons, just reach about 1600 tons for the production of the Vanadium Pentoxide in FLAKES demand of vananum.Along with the development of new industry, estimate that domestic demand to high-purity vanadium oxide also will further increase.For example: domestic big aircraft project and vanadium cell project need high-purity vanadium oxide.Therefore domestic demand to the high-purity mangesium oxide vanadium also can further increase.Abroad, mainly be European Union, the U.S., Japan, Korea S to the bigger area of high purity Vanadium Pentoxide in FLAKES demand.
The raw material of vanadium extraction has a variety of, main vanadium extraction raw materials that vanadium titano-magnetite concentrate, vanadium slag, yeath etc. are arranged, and also has secondary resources such as spent catalyst, oil lime-ash.Comparatively ripe now process for extracting vanadium is: contain vanadium raw materials → grinding → sodium oxide roasting → leaching → removal of impurities → acid ammonium salt precipitation → calcining → Vanadium Pentoxide in FLAKES product.This technology is the ripe process for extracting vanadium of existing industrialization.Because existing impurity-removing method is mingled with impurity to the removal situation of impurity is undesirable with precipitation technology, the Vanadium Pentoxide in FLAKES purity that this technology is produced is generally 98%～99%.
In order to produce purity＞99% Vanadium Pentoxide in FLAKES product, domestic scientific effort has been carried out number of research projects, has formed the novel method of preparation high purity Vanadium Pentoxide in FLAKES, and these methods are in the laboratory study stage at present, do not carry out Industry Promotion.For example: (1) extraction process prepares high purity vanadic anhydride.Be extracted to the roasting Vanadium Pentoxide in FLAKES from vanadium liquid, product purity has reached more than 98%.Contain the foreign ion that can be extracted in the vanadium liquid, these foreign ions enter vanadium liquid after the back extraction, and influence the vanadium product purity, can't accomplish that a step removal of impurities makes high purity vanadic anhydride.(2) ion exchange method prepares high purity vanadic anhydride.This method can make 99.5% above high purity vanadic anhydride.Also need further removal of impurities after the ion-exchange, because resin adsorbs other impurity in the absorption vanadium, can not disposable removal of impurities make high purity vanadic anhydride.(3) alkali solution technique prepares high purity vanadic anhydride.With thick vanadium product after alkali is molten again with the method for producing Vanadium Pentoxide in FLAKES after ammonium hydroxide, calcium hydroxide, sodium metaaluminate, the water glass removal of impurities, this method must through alkali molten and the substep removal of impurities, still can not make the high purity Vanadium Pentoxide in FLAKES after the disposable removal of impurities.
In order to work out the method for suitable high purity vanadic anhydride, and can carry out Industry Promotion.Adopt the method for removal of impurities efficiently, the processing condition of optimizing precipitation reduce impurity carries secretly, to the vanadate that the settles out washing of pulling an oar, effectively removes impurity, can produce high-grade Vanadium Pentoxide in FLAKES product.
Summary of the invention
Technical problem to be solved by this invention provides a kind of novel preparation method of high purity vanadic anhydride.
The technical solution adopted for the present invention to solve the technical problems is: the preparation method of high purity vanadic anhydride comprises the steps:
A, will to contain vanadium raw materials levigate and do deironing and handle;
B, the raw material after step a handled carry out sodium roasting, leach then and obtain containing vanadium solution;
C, the vanadium solution that contains that step b is obtained carry out decationize impurity and remove the anionic impurity processing, filter the vanadium solution that contains after being purified;
Add d, containing after purify ammonium sulfate in the vanadium solution and carry out precipitation and handle, then after filtration, obtain the vanadate throw out behind the washing impurity-removing;
E, the vanadate throw out is pulled an oar, filtered, carry out carrying out washing treatment again, further remove the impurity that is mingled with in the vanadate throw out, drying, roasting obtain the Vanadium Pentoxide in FLAKES product then.
Wherein, decationize impurity is to be adjusted to different pH values with containing vanadium solution among the aforesaid method step c, makes the metallic cation that contains in the vanadium solution change precipitation of hydroxide into and removes.
Wherein, removing anionic impurity among the aforesaid method step c is to remove phosphorus and the silicon that contains in the vanadium solution: dephosphorization agent is CaCl
2, CaCl
2Adding or be mixed with concentration with the solid particulate form is that 8～12% solution morphology adds, and add-on is 1m
3Contain vanadium solution and add 0.4～1.2kg calcium chloride, the dephosphorization temperature is controlled at 〉=85 ℃, and dephosphorization pH value is controlled 8～9, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min; Desiliconizing agent is Al
2(SO
4)
3, Al
2(SO
4)
3Add-on be 1m
3Contain vanadium solution and add 8.5～10.5kg, the silica removal temperature is controlled at 〉=85 ℃, and silica removal pH value is controlled 9～10, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min.
Wherein, contain no suspended substance in the vanadium solution, [V]=25～30g/L, [P]≤0.015g/L, [Si]≤0.05g/L, pH=8～11 after aforesaid method step c purifies.
Wherein, aforesaid method steps d precipitation processing controls precipitation temperature 〉=85 ℃; The additional proportion of ammonium sulfate is: precipitation adds the control of ammonium coefficient 1～2.8; Add acid through twice, once add acid back pH value of solution=5～7, secondary adds acid back pH value of solution=2～3.
Wherein, ammonium sulfate is before once adding acid, and secondary adds the acid back and adds.
Wherein, among the aforesaid method step e, when the vanadate throw out is pulled an oar, control making beating temperature 〉=80 ℃, beating time 10～40min.
Wherein, the vanadium raw materials that contains described in the aforesaid method step a is vanadium extraction by converter blowing gained vanadium slag.
Wherein, will contain among the aforesaid method step a vanadium raw materials levigate to granularity less than 0.1mm, and-120 order 〉=80%.
Wherein, during aforesaid method step b sodium roasting, allocate industrial sodium carbonate into by 1～2.5 times of vanadium quality in the raw material, 600～850 ℃ of control maturing temperatures, roasting time is no less than 1.5h.
Wherein, the liquid-solid ratio that leaches among the aforesaid method step b is 3～6 ︰ 1, and leaching agent is water, extraction temperature＞75 ℃, and extraction time＞15min leaches pH value and controls 7～9.5.Liquid-solid ratio is the ratio of liquid mass (kilogram) and solid masses (kilogram).
The invention has the beneficial effects as follows: the present invention carries out decationize impurity and anionic impurity processing to containing vanadium solution, washing impurity-removing after the precipitation, effectively remove solvable elements such as sodium, chromium, and carry out dispersion treatment again, i.e. making beating makes the impurity component stripping, filtration washing improves the Vanadium Pentoxide in FLAKES product purity that finally makes then.The concrete decationize impurity that adopts of the present invention and the measure of anionic impurity as specifically selecting which kind of dephosphorization agent, control temperature, pH value, constant temperature churning time and time of repose etc. for use, can effectively remove main impurity, guarantee the high purity of the finished product.The concrete precipitation measure of adopting of the present invention also can further improve the purity of product, adsorbs elements such as a large amount of silicon, sodium, chromium, iron when avoiding the ammonium vanadate precipitation, influences the impurity washing effect.The inventive method can fully be removed impurity, and the purity of Vanadium Pentoxide in FLAKES can reach more than 99%.
Embodiment
The present invention is further described below by embodiment.
The inventive method mainly is divided into next step:
1, raw material processing
Adopt crusher will contain vanadium raw materials earlier and be crushed to certain particle, adopt ball mill or Raymond mill will contain the vanadium raw materials grinding to certain fineness again, grinding fineness is less than 0.1mm, and granularity is greater than 120 orders 〉=80%.Improve the specific surface area that contains vanadium raw materials by grinding, can guarantee to contain vanadium raw materials fully oxidation in the process of oxidizing roasting.
2, deironing
Adopt magnetic method, sieve method or air blast process that the vanadium raw materials that contains after levigate is carried out the deironing processing, guarantee metallic iron residual volume＜8%, the main purpose of deironing: emit a large amount of heats when preventing the metallic iron oxidizing reaction, cause charging binding, what influence was produced normally carries out.
3, roasting
By certain proportion scale, with process contain vanadium raw materials and additive mixes (additive also can be allocated some sodium sulfate or sodium-chlor into mainly based on soda, determines the amount of allocating into of additive according to containing the content of vanadium in the vanadium raw materials).Send in rotary kiln or the Multiple hearth furnace and calcine, the vanadium that will contain in the vanadium raw materials by roasting is converted into water-soluble vanadic acid sodium.
4, leach
Adopt water seaoning to leach grog, mode of operation can be selected continous way or intermittent type, the solubility vanadic acid sodium in the grog is dissolved in the aqueous solution goes.Obtain containing vanadium solution by filtering solution separated with residue.
5, removal of impurities
Grog is in the process that leaches, and impurity is immersed in the solution with vanadic acid sodium and goes, and the existence of these impurity is bigger to the purity influence of Vanadium Pentoxide in FLAKES product.Cause the not high major cause of Vanadium Pentoxide in FLAKES product purity to be: because the removal of impurity is not thorough before the precipitation, in the process of precipitation, impurity enters in the particle of ammonium meta-vanadate precipitation, and is not thorough to the ammonium meta-vanadate washing of precipitate.Therefore, adopt effective impurity-removing method crucial for producing high-purity Vanadium Pentoxide in FLAKES product.The removal of impurities concrete grammar is regulated different pH values, makes the metal ion that contains in the vanadium solution become precipitation of hydroxide and removes; Add-on is 1m
3Contain vanadium solution and add 0.4～1.2kg calcium chloride, the dephosphorization temperature is controlled at 〉=85 ℃, and dephosphorization pH value is controlled 8～9, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min; Desiliconizing agent is Al
2(SO
4)
3, Al
2(SO
4)
3Add-on be 1m
3Contain vanadium solution and add 8.5～10.5kg, the silica removal temperature is controlled at 〉=85 ℃, and silica removal pH value is controlled 9～10, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min.
6, precipitation
The precipitation technology controlling and process is bad, and the vanadic acid ammonium salt is more abundant flaky crystalline grain agglomerating particles, likeness in form chrysanthemum shape, and elements such as a large amount of silicon, sodium, chromium, iron can be adsorbed in the surface when ammonium vanadate salt particle of this shape precipitated, and influenced the impurity washing and removed effect.Control suitable precipitation technology, precipitated product mainly is ammonium meta-vanadate, and more serious reunion takes place the ammonium meta-vanadate particle hardly, and solvable element such as the sodium during precipitation in the solution, chromium can less entering in the vanadate.During washing, the ammonium meta-vanadate particle is big and loose, and solvable elements such as sodium, chromium are easier to washing and remove.Therefore, the precipitation technology that research suits is crucial for the absorption that reduces impurity, precipitation processing controls precipitation temperature 〉=85 ℃; The additional proportion of ammonium sulfate is: precipitation adds the control of ammonium coefficient 1～2.8; Add acid through twice, once add acid back pH value of solution=5～7, secondary adds acid back pH value of solution=2～3.
7, disperse washing again
In order to produce high-purity Vanadium Pentoxide in FLAKES product, the vanadate behind the filtration washing is precipitated again redispersion (making beating), make the impurity component stripping, carry out filtration washing again, can effectively remove impurity component.
8, dry, calcining
Vanadate after the removal of impurities through calcining, can obtain higher-grade Vanadium Pentoxide in FLAKES product more earlier through super-dry.
Be further described below by the specific embodiment of the present invention of embodiment, but therefore protection scope of the present invention be not limited among the embodiment.
Embodiment one
Earlier that vanadium extraction by converter blowing gained vanadium slag is levigate through ball mill, granularity is less than 0.1mm, and granularity is controlled 90% greater than 120 orders; The vanadium raw materials that contains after levigate is done the deironing processing, and the metallic iron residual volume is 6%; The vanadium raw materials that contains after the deironing is allocated industrial sodium carbonate (soda) into, the control of the amount of allocating into of yellow soda ash exists: allocate into by 1～2.5 times of content of vanadium, maturing temperature control is at 780 ℃, roasting time control is at 3h, the vanadium raw materials that contains after the roasting adds water logging and goes out, and the solid mass ratio control of leach liquor is at 4:1, and extraction temperature is controlled at 85 ℃, extraction time control was leached pH value control 8 at 25 minutes; Carry out the decationize processing to containing vanadium solution, will contain vanadium solution and be adjusted to different pH values, make GOLD FROM PLATING SOLUTION belong to ion and become precipitation of hydroxide.Remove anionic treatments to containing vanadium solution, select CaCl
2Make dephosphorization agent, adding or be mixed with concentration with the solid particulate form is that the form of about 10% solution adds, and add-on is 1m
3Qualifying liquid adds 1kg calcium chloride, and the dephosphorization temperature is controlled at 85 ℃, and the dephosphorization pH value is controlled 8.5, and the constant temperature churning time is controlled at 40min, and the constant temperature time of repose is controlled at 40min.Desiliconizing agent is selected Al
2(SO4)
3, Al
2(SO4)
3The amount of allocating into control at 9.5g/l, the silica removal temperature is controlled at 90 ℃, the silica removal pH value is controlled 9.5, the constant temperature churning time is controlled at 40min, the constant temperature time of repose is controlled at 40min; The vanadium solution of removing behind the impurity that contains is carried out precipitation and handles, and qualifying liquid control exists: [V]=27g/l, [P]≤0.015g/l, [Si]≤0.05g/l, pH=10, solution clear, no suspended substance.The control of precipitation temperature is at 85 ℃, and the control of the additional proportion of ammonium sulfate exists: precipitation adds ammonium coefficient 1.5, and the precipitation temperature is controlled at 〉=85 ℃, once adds acid back pH value of solution=5～7, and secondary adds acid back pH value of solution=2～3; To vanadate disperse, carrying out washing treatment, discrete volume than control an amount of, jitter time was controlled at 30 minutes, dispersion temperature is controlled at 80 ℃.The purity of the Vanadium Pentoxide in FLAKES that obtains by above art breading is 99.2%.
Embodiment two
Earlier that vanadium extraction by converter blowing gained vanadium slag is levigate through ball mill, granularity is less than 0.1mm, and granularity is controlled about 90% greater than 120 orders; The vanadium raw materials that contains after levigate is done the deironing processing, and the metallic iron residual volume is respectively 5%; The vanadium raw materials that contains after the deironing is allocated industrial sodium carbonate (soda) into, the control of the amount of allocating into of yellow soda ash exists: allocate into by 1～2.5 times of content of vanadium, maturing temperature control is at 780 ℃, roasting time control is at 3h, the vanadium raw materials that contains after the roasting adds water logging and goes out, and the solid mass ratio control of leach liquor is at 4:1, and extraction temperature is controlled at 85 ℃, extraction time control was leached pH value control 8 at 25 minutes; Carry out the decationize processing to containing vanadium solution, will contain vanadium solution and be adjusted to different pH values, make GOLD FROM PLATING SOLUTION belong to ion and become precipitation of hydroxide.Remove anionic treatments to containing vanadium solution, select CaCl
2Make dephosphorization agent, adding or be mixed with concentration with the solid particulate form is that the form of about 10% solution adds, and add-on is 1m
3Qualifying liquid adds 1.2kg calcium chloride respectively, and the dephosphorization temperature is controlled at 85 ℃, and the dephosphorization pH value is controlled 8.5, and the constant temperature churning time is controlled at 40min, and the constant temperature time of repose is controlled at 40min.Desiliconizing agent is selected Al
2(SO4)
3, Al
2(SO4)
3The amount of allocating into control at 10g/l, the silica removal temperature is controlled at 90 ℃, the silica removal pH value is controlled 9.5, the constant temperature churning time is controlled at 40min, the constant temperature time of repose is controlled at 40min; The vanadium solution of removing behind the impurity that contains is carried out precipitation and handles, and qualifying liquid control exists: [V]=27g/l, [P]≤0.015g/l, [Si]≤0.05g/l, pH=10, solution clear, no suspended substance.The control of precipitation temperature is at 85 ℃, and the control of the additional proportion of ammonium sulfate exists: it is 2 that precipitation adds the ammonium coefficient, and the precipitation temperature is controlled at 〉=85 ℃, once adds acid back pH value of solution=5～7, and secondary adds acid back pH value of solution=2～3; To vanadate disperse, carrying out washing treatment, discrete volume than control an amount of, jitter time was controlled at 30 minutes, dispersion temperature is controlled at 80 ℃.The purity of the Vanadium Pentoxide in FLAKES that obtains by above art breading is 99.5%.
Claims (10)
1. the preparation method of high purity vanadic anhydride is characterized in that comprising the steps:
A, will to contain vanadium raw materials levigate and do deironing and handle;
B, the raw material after step a handled carry out sodium roasting, leach then and obtain containing vanadium solution;
C, the vanadium solution that contains that step b is obtained carry out decationize impurity and remove the anionic impurity processing, filter the vanadium solution that contains after being purified;
Add d, containing after purify ammonium sulfate in the vanadium solution and carry out precipitation and handle, then after filtration, obtain the vanadate throw out behind the washing impurity-removing;
E, the vanadate throw out is pulled an oar, filtered, carry out carrying out washing treatment again, further remove the impurity that is mingled with in the vanadate throw out, drying, roasting obtain the Vanadium Pentoxide in FLAKES product then.
2. the preparation method of high purity vanadic anhydride according to claim 1, it is characterized in that: decationize impurity is to be adjusted to different pH values with containing vanadium solution among the step c, makes the metallic cation that contains in the vanadium solution change precipitation of hydroxide into and removes.
3. the preparation method of high purity vanadic anhydride according to claim 1 is characterized in that: be to remove phosphorus and the silicon that contains in the vanadium solution except anionic impurity among the step c: dephosphorization agent is CaCl
2, CaCl
2Adding or be mixed with concentration with the solid particulate form is that 8～12% solution morphology adds, and add-on is 1m
3Contain vanadium solution and add 0.4～1.2kg calcium chloride, the dephosphorization temperature is controlled at 〉=85 ℃, and dephosphorization pH value is controlled 8～9, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min; Desiliconizing agent is Al
2(SO
4)
3, Al
2(SO
4)
3Add-on be 1m
3Contain vanadium solution and add 8.5～10.5kg, the silica removal temperature is controlled at 〉=85 ℃, and silica removal pH value is controlled 9～10, and the constant temperature churning time is not less than 30min, and the constant temperature time of repose is not less than 30min.
4. according to the preparation method of claim 1,2 or 3 described high purity vanadic anhydrides, it is characterized in that: contain no suspended substance in the vanadium solution, [V]=25～30g/L, [P]≤0.015g/L, [Si]≤0.05g/L, pH=8～11 after step c purifies.
5. the preparation method of high purity vanadic anhydride according to claim 4 is characterized in that: steps d precipitation processing controls precipitation temperature 〉=85 ℃; The additional proportion of ammonium sulfate is: precipitation adds the control of ammonium coefficient 1～2.8; Add acid through twice, once add acid back pH value of solution=5～7, secondary adds acid back pH value of solution=2～3.
6. according to the preparation method of each described high purity vanadic anhydride in the claim 1 to 5, it is characterized in that: among the step e, when the vanadate throw out is pulled an oar, control making beating temperature 〉=80 ℃, beating time 10～40min.
7. according to the preparation method of each described high purity vanadic anhydride in the claim 1 to 5, it is characterized in that: the vanadium raw materials that contains described in the step a is vanadium extraction by converter blowing gained vanadium slag.
8. according to the preparation method of each described high purity vanadic anhydride in the claim 1 to 5, it is characterized in that: will contain among the step a vanadium raw materials levigate to granularity less than 0.1mm, and-120 order 〉=80%.
9. according to the preparation method of each described high purity vanadic anhydride in the claim 1 to 5, it is characterized in that: during step b sodium roasting, allocate industrial sodium carbonate into by 1～2.5 times of vanadium quality in the raw material, 600～850 ℃ of control maturing temperatures, roasting time is no less than 1.5h.
10. according to the preparation method of each described high purity vanadic anhydride in the claim 1 to 5, it is characterized in that: the liquid-solid ratio that leaches among the step b is 3～6 ︰ 1, and leaching agent is water, extraction temperature＞75 ℃, extraction time＞15min leaches the control of pH value 7～9.5.
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2013
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Effective date of registration: 20181119 Address after: 617000 Panzhihua City, Sichuan Province, Vanadium and Titanium High-tech Development Zone, Panzhihua City, Yangrun Technology Co., Ltd. Patentee after: Panzhihua Yangrun Technology Co., Ltd. Address before: 617000 Airport Road, East District, Panzhihua, Sichuan Province, No. 10 Patentee before: Panzhihua University |
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