CN108358243A - A kind of preparation method of vanadic anhydride of the tetravalence content of vanadium less than 5/100000ths - Google Patents
A kind of preparation method of vanadic anhydride of the tetravalence content of vanadium less than 5/100000ths Download PDFInfo
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- CN108358243A CN108358243A CN201810343816.2A CN201810343816A CN108358243A CN 108358243 A CN108358243 A CN 108358243A CN 201810343816 A CN201810343816 A CN 201810343816A CN 108358243 A CN108358243 A CN 108358243A
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- vanadic anhydride
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Abstract
A kind of preparation method of vanadic anhydride the present invention provides tetravalence content of vanadium less than 0.005wt%, the preparation method include the following steps：Ammonium metavanadate is heated up in oxidizing atmosphere, constant temperature is pre-processed at 150~280 DEG C, continues to heat up later, carries out calcination processing, obtains the vanadic anhydride that the tetravalence content of vanadium is less than 0.005wt%.The present invention before conventional calcination technique by introducing pretreated step, obtained vanadic anhydride product purity has further raising compared to traditional handicraft, in the industrial production, the present invention can be applied by adjusting calcination process, without separately purchasing other equipment, and, method of the present invention can obtain the vanadic anhydride product of the content ＜ 0.005wt% of purity >=99.95wt% and tetravalence vanadium, disclosure satisfy that demand of each field for the vanadic anhydride product of the low tetravalence content of vanadium of high-purity.
Description
Technical field
Five oxidations two the invention belongs to the field of chemical synthesis more particularly to a kind of tetravalence content of vanadium less than 0.005wt%
The preparation method of vanadium.
Background technology
Vanadium is a kind of important strategic reserves metal, and there is very extensive purposes, vanadium can be used as additive that steel is added
Performance in the metal materials such as iron for enhancing metal material, can also be used as battery material and is used to prepare the high density such as vanadium cell
Energy storage material belongs to indispensable raw material in fields such as aerospace, energy project, biological medicine, intermetallic composite coatings.Gold
Belong to vanadium mainly to be restored to obtain by vfanadium compound such as vanadic anhydrides, in recent years, with advances in technology, some vanadium downstreams
The industrialized production of high-end technology product has higher requirement for the quality of vfanadium compound, especially vanadic anhydride, especially
It is with the development of vanadium cell and vanadium energy storage device, and the supply of domestic high-purity vanadium pentoxide is far from meeting market need
It asks, relies primarily on import, therefore, the production of high-purity vanadium pentoxide has broad prospects in China, and high-purity five aoxidizes
The production technology exploitation of two vanadium has great application value and social effect.
In addition to some conventional foreign metal ions in vanadic anhydride, there is also there is the higher problem of tetravalence content of vanadium,
The producer of the existing domestic technique for producing vanadium pentoxide for grasping the low tetravalence content of vanadium of high-purity is few, and technical merit is compared
Foreign countries lag far behind and unstable product quality.There are mainly two types of high-purity vanadium pentoxide production technologies, the first is to containing
Vanadium solution carries out deep impurity-removing, and second is that calcination method prepares high-purity vanadium, wherein calcination method prepares the application of high-purity vanadium more
Extensively, it is divided by calcination mode and equipment：Static electric furnace calcination method, dynamic rotary kiln calcination method, microwave static state calcination method etc..It is quiet
State electric furnace calcination method is more traditional, its advantage is that equipment investment is few, easy to operate, technical maturity, but calcination is usually incomplete, moves
It is uniform in quality that state rotary kiln, which is calcined the advantages of method, but equipment investment is big, high energy consumption and is also easy to produce environmental pollution, microwave
The advantages of static calcination method is that energy consumption is relatively low, product quality is stablized, but can not carry out industrialized production, moreover, above-mentioned several
Kind method deposits the higher problem of tetravalence content of vanadium in the product, therefore needs to be improved calcine technology.
In the prior art, someone has attempted to obtain the vanadic anhydride of high-purity, but its by improving calcine technology
The purity of the vanadic anhydride of preparation is still relatively low, and the content of wherein tetravalence vanadium is still higher, for example, public in CN101811734A
A kind of method that microwave calcinations of ammonium metavanadate prepares vanadic anhydride is opened, by by the ammonium metavanadate and five oxygen of 10 μm of granularity ＞
Change the blending of two vanadium powders, using microwave with the heating rate of 20~100 DEG C/min be warming up at 500~550 DEG C calcining 5~
30min obtains the vanadic anhydride that purity is 98.5wt%, and a kind of ammonium metavanadate calcining and decomposing is disclosed in CN102502829A
The production technology for preparing high purity vanadic anhydride, by the way that the ammonium metavanadate powder of high-purity is placed in rustless steel container,
Dehydration deamination is carried out under rough vacuum in the reacting furnace of oxidizing atmosphere and is calcined oxidation reaction obtaining the vanadic anhydride of high-purity,
Tetravalence content of vanadium is less than 0.20wt% in its vanadic anhydride prepared, and the content of vanadic anhydride is up to 99.5%.
On the basis of existing technology, those skilled in the art requires further improvement the calcine technology of ammonium metavanadate,
To prepare the less high-purity vanadium pentoxide of a kind of purity higher, tetravalence content of vanadium, moreover, the calcine technology should be simple
Easy-to-use, low for equipment requirements, easy to operate, wide adaptation range, it is at low cost and have preferable Social benefit and economic benefit.
Invention content
For the deficiencies in the prior art, one of the objects of the present invention is to provide a kind of tetravalence content of vanadium to be less than
The preparation method of the vanadic anhydride of 0.005wt%, to obtain a kind of purity higher, the less vanadic anhydride of tetravalence content of vanadium
Product.
To reach this purpose, the preparation method includes the following steps：
By ammonium metavanadate, constant temperature pre-processes at 150~280 DEG C in oxidizing atmosphere, heats up, is forged later
Burning processing obtains the vanadic anhydride that the tetravalence content of vanadium is less than 0.005wt%.
Wherein, constant temperature carry out pretreated temperature can be 160 DEG C, 170 DEG C, 180 DEG C, 190 DEG C, 200 DEG C, 210 DEG C,
220 DEG C, 230 DEG C, 240 DEG C, 250 DEG C, 260 DEG C or 270 DEG C etc..
The present invention is located in advance by being introduced into the constant temperature in oxidizing atmosphere in the calcine technology that tradition prepares vanadic anhydride
The step of reason so that ammonium metavanadate can be decomposed generation by ammonium metavanadate pre-oxidation stable in advance at 150~280 DEG C
The reducing substances such as ammonia exclude, and effectively prevent ammonium metavanadate and decompose the reducibility gas such as the ammonia generated in higher temperature
For the reduction effect of pentavalent vanadium, and then the content of tetravalence vanadium in product is reduced,
Pretreated temperature is excessively high can be so that the speed that pentavalent vanadium is reduced be accelerated, and temperature is too low, can not play and aoxidize it
The effect of middle reducing substances, it is preferable that the pretreated temperature is 180~260 DEG C.
For the oxidation effectiveness being optimal, the pretreated time is more reasonable, in time longer easy raising product
The content of fixedness impurity reduces the purity of vanadic anhydride product, and the time is shorter easy so that aoxidizing insufficient, raising five
The content of tetravalence vanadium in V 2 O product, it is preferable that the pretreated time be 30~180min, for example, 40min,
50min、60min、70min、80min、90min、100min、110min、120min、130min、140min、150min、
160min or 170min etc., further preferably 60~150min.
Preferably, the calcination processing is calcining at constant temperature, and the temperature of calcination processing is 450~590 DEG C, for example, 460 DEG C,
470 DEG C, 480 DEG C, 490 DEG C, 500 DEG C, 510 DEG C, 520 DEG C, 530 DEG C, 540 DEG C, 550 DEG C, 560 DEG C, 570 DEG C or 580 DEG C etc., into
One step is preferably 480~550 DEG C.
Preferably, the heating is at the uniform velocity heats up, and the heating rate at the uniform velocity to heat up is 1~20 DEG C/min, for example, 2 DEG C/
min、3℃/min、4℃/min、5℃/min、6℃/min、7℃/min、9℃/min、11℃/min、13℃/min、15℃/
Min, 17 DEG C/min or 19 DEG C/min etc., further preferably 4~16 DEG C/min.
Preferably, the time of the calcination processing be 40~200min, for example, 60min, 80min, 100min,
120min, 140min, 160min, 180min or 190min etc., further preferably 60~120min.
Preferably, the ammonium metavanadate is ammonium metavanadate powder.
Compared to the smaller ammonium metavanadate powder of grain size, the present invention is more suitable for making with the larger ammonium metavanadate powder of grain size
For raw material, it is preferable that the grain size of the ammonium metavanadate powder is 20~100 μm, for example, 25 μm, 35 μm, 45 μm, 55 μm, 65 μ
M, 75 μm, 85 μm, 90 μm or 95 μm etc..
Preferably, the pretreatment and calcination processing carry out in tube furnace.
Preferably, the oxidizing atmosphere is obtained by being passed through oxygen and/or air in tube furnace.
Preferably, flow≤1000mL/min of the oxygen and/or air, for example, 50mL/min, 100mL/min,
200mL/min、300mL/min、400mL/min、500mL/min、600mL/min、700mL/min、800mL/min、900mL/
Min or 950mL/min etc., further preferably 200~800mL/min.
Preferably, the preparation method includes the following steps：
The ammonium metavanadate powder that grain size is 20~100 μm is placed in tube furnace, oxygen and/or sky are passed through in tube furnace
The flow of gas, oxygen and/or air is 200~800mL/min, is at the uniform velocity heated up with the heating rate of 1~20 DEG C/min later,
Constant temperature carries out 30~180min of pretreatment at 150~280 DEG C, continues at the uniform velocity to heat up with the heating rate of 1~20 DEG C/min later,
40~200min of calcining at constant temperature carries out calcination processing at 450~590 DEG C, obtains the tetravalence content of vanadium and is less than 0.005wt%
Vanadic anhydride.
The second object of the present invention is to provide a kind of vanadic anhydride prepared by the preparation method, by this hair
The content ＜ 0.005wt% of tetravalence vanadium in the vanadic anhydride that preparation method described in bright is prepared, much smaller than passing through it
The vanadic anhydride of his prior art preparation.
Compared with prior art, the invention has the advantages that：
(1) present invention by introducing pretreated step before conventional calcination technique, by select 150~280 DEG C this
One pretreated temperature range so that the vanadic anhydride product purity being prepared has compared to conventional preparation techniques into one
The raising of step can apply the present invention by adjusting calcination process, be set without separately purchasing other in the industrial production
It is standby, therefore the present invention also has many advantages, such as that practicability is good, economical and practical, is suitble to large-scale promotion in production；
(2) method of the present invention can obtain the content ＜ 0.005wt%'s of purity >=99.95wt% and tetravalence vanadium
Vanadic anhydride product, disclosure satisfy that aerospace industry, nuclear industry, solar energy, wind power plant, coating, catalyst and
To the demand of the vanadic anhydride product of the low tetravalence content of vanadium of high-purity in the fields such as luminescent material.
Specific implementation mode
The technical solution further illustrated the present invention below by specific implementation mode.
Those skilled in the art understand the present invention it will be clearly understood that the embodiment is only to aid in, and are not construed as to this hair
Bright concrete restriction.
In the following example and reference examples, used ammonium metavanadate is purchased from Shanghai Aladdin Co., Ltd, purity
And the content of which part impurity is as shown in table 1：
Table 1
| Ingredient | NH4VO3 | Si | Na | Al | Ti | Fe | Cl | Ca |
| Content (wt%) | 99.9 | 0.002 | 0.001 | 0.002 | 0.001 | 0.002 | 0.001 | 0.001 |
In the following example and reference examples, used tube furnace is the production of Hefei Ke Jing Materials Technology Ltd.
GSL-4Z type tube furnaces.
Embodiment 1
It is prepared via a method which vanadic anhydride product 1：
The ammonium metavanadate powder that 20g grain sizes are 28 μm is placed in tube furnace, pure oxygen, the stream of pure oxygen are passed through in tube furnace
Amount is 200mL/min, is at the uniform velocity heated up with the heating rate of 1 DEG C/min later, is warming up to constant temperature at 210 DEG C and is pre-processed
60min continues at the uniform velocity to heat up with the heating rate of 4 DEG C/min later, and calcining at constant temperature 120min is carried out at calcining at 530 DEG C
Reason, obtains vanadic anhydride product 1.
Embodiment 2
It is prepared via a method which vanadic anhydride product 2：
The ammonium metavanadate powder that 20g grain sizes are 28 μm is placed in tube furnace, pure oxygen, the stream of pure oxygen are passed through in tube furnace
Amount is 300mL/min, is at the uniform velocity heated up with the heating rate of 20 DEG C/min later, is warming up to constant temperature at 150 DEG C and is pre-processed
60min continues at the uniform velocity to heat up with the heating rate of 16 DEG C/min later, and calcining at constant temperature 60min is carried out at calcining at 550 DEG C
Reason, obtains vanadic anhydride product 2.
Embodiment 3
It is prepared via a method which vanadic anhydride product 3：
With differing only in for embodiment 1, it is 150 DEG C that constant temperature, which carries out pretreated temperature, time 150min.
Embodiment 3 obtains vanadic anhydride product 3.
Embodiment 4
It is prepared via a method which vanadic anhydride product 4：
With differing only in for embodiment 1, it is 280 DEG C that constant temperature, which carries out pretreated temperature, time 40min.
Embodiment 4 obtains vanadic anhydride product 4.
Embodiment 5
It is prepared via a method which vanadic anhydride product 5：
Temperature with differing only in for embodiment 1, calcination processing is 460 DEG C, time 190min.
Embodiment 5 obtains vanadic anhydride product 5.
Embodiment 6
It is prepared via a method which vanadic anhydride product 6：
Temperature with differing only in for embodiment 1, calcination processing is 580 DEG C, time 40min.
Embodiment 6 obtains vanadic anhydride product 6.
Embodiment 7
It is prepared via a method which vanadic anhydride product 7：
With differing only in for embodiment 1, it is not passed through pure oxygen in tube furnace, but is passed through air, and the flow of air is
1000mL/min。
Embodiment 7 obtains vanadic anhydride product 7.
Embodiment 8
It is prepared via a method which vanadic anhydride product 8：
Grain size with differing only in for embodiment 1, ammonium metavanadate is 100 μm.
Embodiment 8 obtains vanadic anhydride product 8.
Embodiment 9
It is prepared via a method which vanadic anhydride product 9：
With differing only in for embodiment 1, constant temperature carries out the pretreated time as 20min.
Embodiment 9 obtains vanadic anhydride product 9.
Embodiment 10
It is prepared via a method which vanadic anhydride product 10：
With differing only in for embodiment 1, constant temperature carries out the pretreated time as 220min.
Embodiment 10 obtains vanadic anhydride product 10.
Reference examples 1
It is prepared via a method which vanadic anhydride product 11：
With differing only in for embodiment 1, it is 130 DEG C that constant temperature, which carries out pretreated temperature,.
Reference examples 1 obtain vanadic anhydride product 11.
Reference examples 2
It is prepared via a method which vanadic anhydride product 12：
With differing only in for embodiment 1, it is 305 DEG C that constant temperature, which carries out pretreated temperature,.
Reference examples 2 obtain vanadic anhydride product 12.
Reference examples 3
It is prepared via a method which vanadic anhydride product 13：
The ammonium metavanadate powder that 20g grain sizes are 50 μm is placed in tube furnace, pure oxygen, the stream of pure oxygen are passed through in tube furnace
Amount is 300mL/min, is warming up to 530 DEG C later with the heating rate of average 30 DEG C/min, calcining at constant temperature 60min is carried out at calcining
Reason, obtains vanadic anhydride product 13.
Reference examples 4
It is prepared via a method which vanadic anhydride product 14：
The ammonium metavanadate powder that 20g grain sizes are 50 μm is placed in tube furnace, pure oxygen, the stream of pure oxygen are passed through in tube furnace
Amount is 300mL/min, is warming up to 530 DEG C later with the heating rate of average 5 DEG C/min, calcining at constant temperature 60min is carried out at calcining
Reason, obtains vanadic anhydride product 14.
The purity for the vanadic anhydride product 1~14 that above-described embodiment and reference examples are obtained by following test method and
The content of wherein tetravalence vanadium is tested, and test result is listed in table 2：
(1) vanadic anhydride product purity is tested
According to provincial standard DB51/T 2044-2015《The assay method of high-purity vanadium pentoxide impurity content》
Described in method the purity of vanadic anhydride product 1~14 is measured, the purity of vanadic anhydride product is by by five
V 2 O product total weight subtracts the weight of wherein all other impurities elements in addition to vanadium, oxygen, then divided by vanadic anhydride
The total weight of product obtains.
(2) in vanadic anhydride product tetravalence content of vanadium measurement
YB/T 4248-2011 according to national standards《The measurement minusing of vanadic anhydride vanadium tetraoxide content》Middle institute
The method stated is measured the content of tetravalence vanadium in vanadic anhydride product 1~14.
The purity and tetravalence content of vanadium contrast table of 2 vanadic anhydride product 1~14 of table
| Vanadic anhydride product | Purity (wt%) | Tetravalence content of vanadium (wt%) |
| 1 | 99.98 | 0.0032 |
| 2 | 99.98 | 0.0038 |
| 3 | 99.98 | 0.0034 |
| 4 | 99.97 | 0.0039 |
| 5 | 99.97 | 0.0041 |
| 6 | 99.98 | 0.0035 |
| 7 | 99.98 | 0.0028 |
| 8 | 99.98 | 0.0037 |
| 9 | 99.97 | 0.0049 |
| 10 | 99.95 | 0.0048 |
| 11 | 99.91 | 0.0184 |
| 12 | 99.90 | 0.0243 |
| 13 | 98.89 | 0.4020 |
| 14 | 99.88 | 0.0425 |
From table 2 it can be seen that the present invention by introducing pretreated step before conventional calcination technique, can be carried effectively
The purity of vanadic anhydride product prepared by height and the content for reducing wherein tetravalence vanadium, by suitably being adjusted to pretreatment condition
It is whole, can further reduce the content of tetravalence vanadium in product, moreover, 150~280 DEG C of the selection of present invention specificity this
One pretreated temperature range can further realize the purity >=99.95wt% for the vanadic anhydride product being prepared, and
And make the content ＜ 0.005wt% of wherein tetravalence vanadium.
Applicant states that the present invention illustrates the process of the present invention, but the present invention not office by above-described embodiment
It is limited to above-mentioned processing step, that is, does not mean that the present invention has to rely on above-mentioned processing step and could implement.Technical field
Technical staff it will be clearly understood that any improvement in the present invention, equivalence replacement and auxiliary element to raw material selected by the present invention
Addition, the selection etc. of concrete mode, all fall within protection scope of the present invention and the open scope.
Claims (10)
1. a kind of preparation method of vanadic anhydride of tetravalence content of vanadium less than 0.005wt%, which is characterized in that the preparation side
Method includes the following steps：
By ammonium metavanadate, constant temperature pre-processes at 150~280 DEG C in oxidizing atmosphere, heats up, is carried out at calcining later
Reason obtains the vanadic anhydride that the tetravalence content of vanadium is less than 0.005wt%.
2. preparation method according to claim 1, which is characterized in that the pretreated temperature is 180~260 DEG C；
Preferably, the pretreated time is 30~180min, further preferably 60~150min.
3. preparation method according to claim 1 or 2, which is characterized in that the heating at the uniform velocity heats up at the uniform velocity to heat up
Heating rate is 1~20 DEG C/min, preferably 4~16 DEG C/min.
4. the preparation method according to one of claims 1 to 3, which is characterized in that the calcination processing is calcining at constant temperature, is forged
The temperature for burning processing is 450~590 DEG C, preferably 480~550 DEG C.
5. the preparation method according to one of Claims 1 to 4, which is characterized in that the time of the calcination processing be 40~
200min, preferably 60~120min.
6. the preparation method according to one of Claims 1 to 5, which is characterized in that the ammonium metavanadate is ammonium metavanadate powder
End；
Preferably, the grain size of the ammonium metavanadate powder is 20~100 μm.
7. the preparation method according to one of claim 1~6, which is characterized in that the pretreatment and calcination processing are in pipe
It is carried out in formula stove.
8. preparation method according to claim 7, which is characterized in that the oxidizing atmosphere in tube furnace by being passed through
Oxygen and/or air obtain；
Preferably, flow≤1000mL/min of the oxygen and/or air, further preferably 200~800mL/min.
9. the preparation method according to one of claim 1~8, which is characterized in that the preparation method includes the following steps：
The ammonium metavanadate powder that grain size is 20~100 μm is placed in tube furnace, oxygen and/or air are passed through in tube furnace,
The flow of oxygen and/or air is 200~800mL/min, is at the uniform velocity heated up with the heating rate of 1~20 DEG C/min later, 150
Constant temperature carries out 30~180min of pretreatment at~280 DEG C, continues at the uniform velocity to heat up with the heating rate of 1~20 DEG C/min later,
40~200min of calcining at constant temperature carries out calcination processing at 450~590 DEG C, obtains the tetravalence content of vanadium less than 0.005wt%'s
Vanadic anhydride.
10. vanadic anhydride prepared by a kind of preparation method as described in one of claim 1~9, which is characterized in that described five
The content ＜ 0.005wt% of tetravalence vanadium in V 2 O.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114684855A (en) * | 2022-05-20 | 2022-07-01 | 宿州学院 | Method for preparing vanadium pentoxide in different shapes by combining hydrothermal method with calcination method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289226A (en) * | 2008-03-07 | 2008-10-22 | 昆明理工大学 | Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate |
| CN102502829A (en) * | 2011-11-18 | 2012-06-20 | 吉首大学 | Production process for preparing high-purity vanadium pentoxide by means of calcining and decomposing metavanadic acid |
| CN106830077A (en) * | 2017-01-17 | 2017-06-13 | 中国科学院过程工程研究所 | A kind of method of vanadic anhydride purification |
| CN106946290A (en) * | 2016-01-07 | 2017-07-14 | 中国科学院过程工程研究所 | A kind of method of vanadic anhydride purification |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101289226A (en) * | 2008-03-07 | 2008-10-22 | 昆明理工大学 | Process for preparing vanadic anhydride by vacuum calcining ammonium poly-vanadate |
| CN102502829A (en) * | 2011-11-18 | 2012-06-20 | 吉首大学 | Production process for preparing high-purity vanadium pentoxide by means of calcining and decomposing metavanadic acid |
| CN106946290A (en) * | 2016-01-07 | 2017-07-14 | 中国科学院过程工程研究所 | A kind of method of vanadic anhydride purification |
| CN106830077A (en) * | 2017-01-17 | 2017-06-13 | 中国科学院过程工程研究所 | A kind of method of vanadic anhydride purification |
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| CN114684855A (en) * | 2022-05-20 | 2022-07-01 | 宿州学院 | Method for preparing vanadium pentoxide in different shapes by combining hydrothermal method with calcination method |
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