CN110078122A - A kind of preparation method of p-type high purity niobium oxide - Google Patents
A kind of preparation method of p-type high purity niobium oxide Download PDFInfo
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- CN110078122A CN110078122A CN201910444405.7A CN201910444405A CN110078122A CN 110078122 A CN110078122 A CN 110078122A CN 201910444405 A CN201910444405 A CN 201910444405A CN 110078122 A CN110078122 A CN 110078122A
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
A kind of preparation method of p-type high purity niobium oxide, the preparation method is the following steps are included: (1) solution concentration is deployed；(2) ammonia neutralization precipitation；(3) pressure filtration washing；(4) drying screening；(5) calcining screening；(6) properties of product detect.P-type high purity niobium oxide product, the product either principal component content, or the content of every impurity, product grade FNb in better than professional standard " high-purity niobium pentaoxide " YS/T 548-2007 can be prepared in preparation method of the present invention2O5- 04 regulation, and show loose powders characteristic after mixing with phosphoric acid.
Description
Technical field
The present invention relates to a kind of preparation methods of p-type high purity niobium oxide.
Background technique
Niobium is in periodic table of chemical element Zhong Shu VB race, atomic number 41.P-type high purity niobium oxide product purity is
99.99%, there is the characteristic for becoming loose powders after mixing with phosphoric acid.
In the prior art, the preparation of high purity niobium oxide, usually using niobium concentrate as raw material, by hydrofluoric acid and sulfuric acid nitration mixture point
Solution, sec-octyl alcohol-HF-H2SO4In system niobium separated with other impurities elements by extraction, high-purity fluorine niobic acid solution ammonia neutralization precipitation, filters pressing
Washing, drying and calcining screening process high purity niobium oxide, process flow are as shown in Figure 1.It is " high in existing professional standard
Pure niobium pentaoxide " in YS/T548-2007, the product grade of high purity niobium oxide is FNb2O5- 04, wherein F indicates powder,
Nb2O5Indicate niobium pentaoxide (Nb2O5) molecular formula, 04 indicate product purity be 99.99%.Prior art produces high-purity
Niobium oxide product does not have the characteristic of p-type high purity niobium oxide.
Summary of the invention
Its purpose of the invention, which is that, provides a kind of preparation method of p-type high purity niobium oxide, solves prior art production
High purity niobium oxide product do not have p-type high purity niobium oxide characteristic the problem of, realizing p-type high purity niobium oxide produced has
Become the characteristic of loose powders after mixing with phosphoric acid.
It adopts the technical scheme that achieve the above object, a kind of preparation method of p-type high purity niobium oxide, the preparation side
Method the following steps are included:
(1) solution concentration is deployed: to Nb2O5Meter, oxide amount is >=the high-purity fluorine niobic acid solution of 90g/L in pure water is added,
Fluorine niobic acid feed liquid is obtained, fluorine niobic acid feed liquid is with Nb2O5Meter, oxide amount are 90 ~ 130g/L；
(2) ammonia neutralization precipitation: being added liquefied ammonia into fluorine niobic acid feed liquid, until pH=8.5 ~ 9.5, obtain high-purity niobium hydroxide slurry；
(3) pressure filtration washing: high-purity niobium hydroxide slurry is transferred to filter press, tune washing trough is put into after carrying out filters pressing, is contained with 60 ~ 75 DEG C
Ammonia hot pure water carries out the impurity such as washing fluorine removal, and pressure filtration washing fluorine content≤0.05g/L into washing raffinate is repeated, obtains height
Pure cerium hydroxide niobium filtrate, wherein the weight percent concentration of ammonia is 3 ~ 8% in hot pure water containing ammonia；
(4) drying screening: high-purity niobium hydroxide filtrate is dried in 150 ~ 220 DEG C of box drying box or microwave drying box,
Time is 8 ~ 15 hours, then is sieved by 60 mesh vibrating sieving machines, obtains High Purity Hydrogen niobium oxide powder；
(5) calcining screening: High Purity Hydrogen niobium oxide powder is pushed away in boat furnace in tunnel, and the control of low-temperature space temperature is 350 ~ 450 DEG C, in
The control of warm area temperature is to calcine at 650 ~ 750 DEG C, and the time is 10 ~ 15 hours, and the fltting speed of push-plate is 12 ~ 15 minutes/push-plate；
It is sieved again by 60 mesh vibrating sieving machines, obtains p-type high purity niobium oxide product；
(6) properties of product detect: providing to carry out analysis detection, p-type high purity niobium oxide product principal component and miscellaneous according to GB/T15076
Matter content meets in professional standard " high-purity niobium pentaoxide " YS/T548-2007 to product grade FNb2O5- 04 regulation, p-type
High purity niobium oxide product and phosphoric acid are mixed into loose sprills, and mixed proportion is p-type high purity niobium oxide: phosphoric acid=20g:15g.
Beneficial effect
The present invention has the following advantages that compared with prior art.
1. preparation method of the present invention, technology is stable, easy to operate, without changing to existing production equipment
The p-type high purity niobium oxide product made, and be prepared, either principal component content in chemical component, or every impurity contain
Amount, has all reached product grade FNb in professional standard " high-purity niobium pentaoxide " YS/T 548-20072O5- 04 regulation；
2. the p-type high purity niobium oxide product obtained using preparation method of the present invention becomes loose powders, tool after mixing with phosphoric acid
There is good p-type high purity niobium oxide characteristic, has reached same kind of products at abroad level, in practical applications, p-type of the present invention
High purity niobium oxide can be applied reliably.
With reference to the accompanying drawing, the invention will be further described for Detailed description of the invention.
Fig. 1 is the preparation flow figure of high purity niobium oxide in the prior art；
Fig. 2 is the preparation flow figure of the obtained p-type high purity niobium oxide of the present invention；
Fig. 3 is that the embodiment of the present invention 1 produces the p-type high purity niobium oxide product Electronic Speculum detection figure being prepared；
Fig. 4 is that the embodiment of the present invention 2 produces performance detection figure after the p-type high purity niobium oxide product being prepared is mixed with phosphoric acid.
Specific embodiment
Below by conjunction with the drawings and the specific embodiments, the present invention is described in further details.
A kind of preparation method of p-type high purity niobium oxide, as shown in Fig. 2, the preparation method the following steps are included:
(1) solution concentration is deployed: to Nb2O5Meter, oxide amount is >=the high-purity fluorine niobic acid solution of 90g/L in pure water is added,
Fluorine niobic acid feed liquid is obtained, fluorine niobic acid feed liquid is with Nb2O5Meter, oxide amount are 90 ~ 130g/L；
(2) ammonia neutralization precipitation: being added liquefied ammonia into fluorine niobic acid feed liquid, until pH=8.5 ~ 9.5, obtain high-purity niobium hydroxide slurry；
(3) pressure filtration washing: high-purity niobium hydroxide slurry is transferred to filter press, tune washing trough is put into after carrying out filters pressing, is contained with 60 ~ 75 DEG C
Ammonia hot pure water carries out the impurity such as washing fluorine removal, and pressure filtration washing fluorine content≤0.05g/L into washing raffinate is repeated, obtains height
Pure cerium hydroxide niobium filtrate, wherein the weight percent concentration of ammonia is 3 ~ 8% in hot pure water containing ammonia；
(4) drying screening: high-purity niobium hydroxide filtrate is dried in 150 ~ 220 DEG C of box drying box or microwave drying box,
Time is 8 ~ 15 hours, then is sieved by 60 mesh vibrating sieving machines, obtains High Purity Hydrogen niobium oxide powder；
(5) calcining screening: High Purity Hydrogen niobium oxide powder is pushed away in boat furnace in tunnel, and the control of low-temperature space temperature is 350 ~ 450 DEG C, in
The control of warm area temperature is to calcine at 650 ~ 750 DEG C, and the time is 10 ~ 15 hours, and the fltting speed of push-plate is 12 ~ 15 minutes/push-plate；
It is sieved again by 60 mesh vibrating sieving machines, obtains p-type high purity niobium oxide product；
(6) properties of product detect: providing to carry out analysis detection, p-type high purity niobium oxide product principal component and miscellaneous according to GB/T15076
Matter content meets in professional standard " high-purity niobium pentaoxide " YS/T548-2007 to product grade FNb2O5- 04 regulation, p-type
High purity niobium oxide product and phosphoric acid are mixed into loose sprills, and mixed proportion is p-type high purity niobium oxide: phosphoric acid=20g:15g.
High-purity fluorine niobic acid solution in the step (1), with Nb2O5Meter, oxide amount is preferably 90 ~ 150g/L；The fluorine niobium
Sour feed liquid, with Nb2O5Meter, oxide amount is preferably 90g/L ~ 110g/L.
Liquefied ammonia is added in the step (2) in fluorine niobic acid feed liquid to pH=9 ~ 9.5.
Fluorine content≤0.03g/L in raffinate is repeated after pressure filtration washing in high-purity niobium hydroxide slurry in the step (3).
High-purity niobium hydroxide filtrate is dried at 180 ~ 200 DEG C in the step (4), and the time is 10 ~ 12 hours.
High Purity Hydrogen niobium oxide powder pushes away in boat furnace in tunnel in the step (5), and the control of low-temperature space temperature is 400 ~ 450
DEG C, the control of middle warm area temperature is to calcine at 650 ~ 700 DEG C, and the time is 12 ~ 15 hours.
Experimental method in following embodiments is unless otherwise specified conventional method；It is as used in the following examples each
Kind chemical materials is commercially available products unless otherwise specified.
Embodiment 1
1, solution concentration is deployed:
(1) high-purity fluorine niobic acid solution 800L, after measured, oxide concentration is with Nb2O5It is calculated as 135.7g/L, is put into ammonia neutralization precipitation
In slot；
(2) by calculating, pure water 406.2L need to be added；
(3) pure water of the volume is added in ammonia neutralization precipitation slot, starting stirring 15min, the high-purity fluorine niobic acid material after allotment
Liquid total volume is 1206.2L, and oxide concentration is with Nb2O5It is calculated as 90g/L, oxide amount is with Nb2O5Meter=108.56kg.
2, ammonia neutralization precipitation:
In ammonia neutralization precipitation slot, opens liquefied ammonia valve and liquefied ammonia is added, neutralization precipitation to pH=9 forms high-purity niobium hydroxide slurry.
3, filters pressing tune is washed:
(1) high-purity niobium hydroxide slurry is transferred to filter press, is put into tune washing trough after carrying out filters pressing；
(2) in adjusting washing trough, 70 DEG C of 1500L of hot pure water containing ammonia are added, starting stirring system, which adjust, removes fluorine, hot pure water containing ammonia
The weight percentage of middle ammonia is 5%；
(3) filters pressing tune is washed till fluorine in raffinate (F)≤0.03g/L repeatedly, and filters pressing forms high-purity niobium hydroxide filtrate, oxide amount with
Nb2O5Meter=105.85kg.
4, drying screening:
(1) high-purity niobium hydroxide filtrate is contained in charging tray, is packed into box drying box；
(2) oven temperature control is 170 DEG C ~ 180 DEG C, and the time is 12 hours, and drying forms high-purity niobium hydroxide block powder；
(3) the high purity niobium oxide block powder after drying is sieved by 60 mesh vibrating sieving machines, extracting screen underflow, oxide amount is with Nb2O5Meter
=105.32kg。
5, calcining screening:
(1) the High Purity Hydrogen niobium oxide powder of drying screening is transferred to tunnel and pushes away boat furnace and calcines；
(2) control of calcining low-temperature space temperature is 400 ~ 450 DEG C, and calcining middle warm area temperature control is 650 ~ 700 DEG C, the propulsion of push-plate
Speed is 15 minutes/push-plate, and the time is 15 hours, and calcining forms high purity niobium oxide powder.
(3) calcined high purity niobium oxide powder is sieved by 60 mesh vibrating sieving machines, oxide amount is with Nb2O5Meter=
104.79kg。
6, performance detection:
Will calcining screening obtain p-type high purity niobium oxide product sampling, according to GB/T 15076 provide carry out analysis detection, it is main at
Divide and impurity content is shown in Table 1, p-type high purity niobium oxide product and phosphoric acid are mixed into loose sprills, and detection is qualified up to target production
Product p-type high purity niobium oxide, p-type high purity niobium oxide product Electronic Speculum testing result is as shown in Figure 3.
Embodiment 2
1, solution concentration is deployed:
(1) high-purity fluorine niobic acid solution 760L, after measured, oxide concentration is with Nb2O5It is calculated as 122.3g/L, is put into ammonia neutralization precipitation
In slot；
(2) by calculating, pure water 272.7L need to be added；
(3) pure water of the volume is added in ammonia neutralization precipitation slot, starting stirring 15min, the high-purity fluorine niobic acid material after allotment
Liquid total volume is 1032.7L, and oxide concentration is with Nb2O5It is calculated as 90g/L, oxide amount is with Nb2O5Meter=92.95kg.
2, ammonia neutralization precipitation:
In ammonia neutralization precipitation slot, opens liquefied ammonia valve and liquefied ammonia is added, neutralization precipitation to pH=9 forms high-purity niobium hydroxide slurry.
3, filters pressing tune is washed:
(1) high-purity niobium hydroxide slurry is transferred to filter press, is put into tune washing trough after carrying out filters pressing；
(2) in adjusting washing trough, 70 DEG C of 1500L of hot pure water containing ammonia are added, starting stirring system, which adjust, removes fluorine, hot pure water containing ammonia
The weight percentage of middle ammonia is 5%；
(3) filters pressing tune is repeated and is washed till fluorine in raffinate (F)≤0.03g/L, filters pressing forms high-purity niobium hydroxide filtrate, oxide
Amount is with Nb2O5Meter=90.63kg.
4, drying screening:
(1) high-purity niobium hydroxide filter cake is contained in charging tray, is packed into box drying box；
(2) oven temperature control is 160 DEG C ~ 170 DEG C, and the time is 13 hours, and drying forms high-purity niobium hydroxide block powder；
(3) the high purity niobium oxide block powder after drying is sieved by 60 mesh vibrating sieving machines, extracting screen underflow, oxide amount is with Nb2O5Meter
=90.18kg。
5, calcining screening:
(1) the High Purity Hydrogen niobium oxide powder of drying screening is transferred to tunnel and pushes away boat furnace and calcines；
(2) control of calcining low-temperature space temperature is 400 ~ 450 DEG C, and calcining middle warm area temperature control is 650 ~ 700 DEG C, the propulsion of push-plate
Speed is 15 minutes/push-plate, and the time is 15 hours, and calcining forms high purity niobium oxide powder；
(3) calcined high purity niobium oxide powder is sieved by 60 mesh vibrating sieving machines, oxide amount is with Nb2O5Meter=89.73kg.
6, performance detection:
Will calcining screening obtain p-type high purity niobium oxide product sampling, according to GB/T 15076 provide carry out analysis detection, it is main at
Divide and impurity content is shown in Table 1, p-type high purity niobium oxide product and phosphoric acid are mixed into loose sprills as shown in Figure 4, and detection qualification is
Obtain target product p-type high purity niobium oxide.
P-type high purity niobium oxide product quality testing result prepared by 1 embodiment 1 of table and example 2
It is shown from the data of table 1, impurity contains in the p-type high purity niobium oxide product being prepared according to preparation method of the present invention
Amount is better than existing professional standard.
Claims (6)
1. a kind of preparation method of p-type high purity niobium oxide, which is characterized in that the preparation method the following steps are included:
Solution concentration allotment: to Nb2O5Meter, oxide amount is >=the high-purity fluorine niobic acid solution of 90g/L in pure water is added, obtain
Fluorine niobic acid feed liquid, fluorine niobic acid feed liquid is with Nb2O5Meter, oxide amount are 90 ~ 130g/L；
Ammonia neutralization precipitation: being added liquefied ammonia into fluorine niobic acid feed liquid, until pH=8.5 ~ 9.5, obtain high-purity niobium hydroxide slurry；
Pressure filtration washing: being transferred to filter press for high-purity niobium hydroxide slurry, be put into tune washing trough after carrying out filters pressing, contains ammonia with 60 ~ 75 DEG C
Hot pure water carries out the impurity such as washing fluorine removal, and pressure filtration washing fluorine content≤0.05g/L into washing raffinate is repeated, obtains high-purity
Niobium hydroxide filtrate, wherein the weight percent concentration of ammonia is 3 ~ 8% in hot pure water containing ammonia；
Drying screening: high-purity niobium hydroxide filtrate is dried in 150 ~ 220 DEG C of box drying box or microwave drying box, the time
It is 8 ~ 15 hours, then is sieved by 60 mesh vibrating sieving machines, obtains High Purity Hydrogen niobium oxide powder；
Calcining screening: High Purity Hydrogen niobium oxide powder is pushed away in boat furnace in tunnel, and the control of low-temperature space temperature is 350 ~ 450 DEG C, medium temperature
Temperature control in area's is to calcine at 650 ~ 750 DEG C, and the time is 10 ~ 15 hours, and the fltting speed of push-plate is 12 ~ 15 minutes/push-plate；Again
It is sieved by 60 mesh vibrating sieving machines, obtains p-type high purity niobium oxide product；
Properties of product detection: it provides to carry out analysis detection, p-type high purity niobium oxide product main content and impurities according to GB/T15076
Content meets in professional standard " high-purity niobium pentaoxide " YS/T548-2007 to product grade FNb2O5- 04 regulation, p-type are high
Pure zirconia niobium product and phosphoric acid are mixed into loose sprills, and mixed proportion is p-type high purity niobium oxide: phosphoric acid=20g:15g.
2. a kind of preparation method of p-type high purity niobium oxide according to claim 1, which is characterized in that in the step (1)
High-purity fluorine niobic acid solution, with Nb2O5Meter, oxide amount is preferably 90 ~ 150g/L；The fluorine niobic acid feed liquid, with Nb2O5Meter, oxidation
Object amount is preferably 90g/L ~ 110g/L.
3. a kind of preparation method of p-type high purity niobium oxide according to claim 1, which is characterized in that in the step (2)
Liquefied ammonia is added in fluorine niobic acid feed liquid to pH=9 ~ 9.5.
4. a kind of preparation method of p-type high purity niobium oxide according to claim 1, which is characterized in that in the step (3)
Fluorine content≤0.03g/L in raffinate is repeated after pressure filtration washing in high-purity niobium hydroxide slurry.
5. a kind of preparation method of p-type high purity niobium oxide according to claim 1, which is characterized in that in the step (4)
High-purity niobium hydroxide filtrate is dried at 180 ~ 200 DEG C, and the time is 10 ~ 12 hours.
6. a kind of preparation method of p-type high purity niobium oxide according to claim 1, which is characterized in that in the step (5)
High Purity Hydrogen niobium oxide powder pushes away in boat furnace in tunnel, and the control of low-temperature space temperature is 400 ~ 450 DEG C, the control of middle warm area temperature for 650 ~
It is calcined at 700 DEG C, the time is 12 ~ 15 hours.
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Cited By (6)
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| CN110697775A (en) * | 2019-11-08 | 2020-01-17 | 广东广晟稀有金属光电新材料有限公司 | Preparation method of low-nitrogen niobium hydroxide |
| CN111977690A (en) * | 2020-09-07 | 2020-11-24 | 江西拓泓新材料有限公司 | Method for removing copper and other impurities in preparation of tantalum-niobium oxide |
| CN113526553A (en) * | 2021-08-30 | 2021-10-22 | 南京弘顺和生物科技有限公司 | Preparation method and production equipment of superfine niobium hydroxide |
| WO2021246111A1 (en) * | 2020-06-04 | 2021-12-09 | 三井金属鉱業株式会社 | Niobate compound and niobium-containing slurry |
| CN115818712A (en) * | 2022-09-08 | 2023-03-21 | 季华实验室 | Niobium oxide mixed with phosphoric acid in loose state and preparation method thereof |
| CN118307034A (en) * | 2024-05-14 | 2024-07-09 | 江西省定海钽铌有限公司 | Low-temperature calcination process of superfine niobium oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111977690A (en) * | 2020-09-07 | 2020-11-24 | 江西拓泓新材料有限公司 | Method for removing copper and other impurities in preparation of tantalum-niobium oxide |
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| CN115818712A (en) * | 2022-09-08 | 2023-03-21 | 季华实验室 | Niobium oxide mixed with phosphoric acid in loose state and preparation method thereof |
| CN115818712B (en) * | 2022-09-08 | 2024-05-07 | 季华实验室 | Niobium oxide in loose state mixed with phosphoric acid and preparation method thereof |
| CN118307034A (en) * | 2024-05-14 | 2024-07-09 | 江西省定海钽铌有限公司 | Low-temperature calcination process of superfine niobium oxide |
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