CN109179504A - A method of preparing big granularity ammonium metavanadate - Google Patents
A method of preparing big granularity ammonium metavanadate Download PDFInfo
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- CN109179504A CN109179504A CN201811222095.6A CN201811222095A CN109179504A CN 109179504 A CN109179504 A CN 109179504A CN 201811222095 A CN201811222095 A CN 201811222095A CN 109179504 A CN109179504 A CN 109179504A
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- C01—INORGANIC CHEMISTRY
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- C01G31/00—Compounds of vanadium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The present invention relates to a kind of method for preparing big granularity ammonium metavanadate, the methods are as follows: ammonium metavanadate solution is added in crystallizer, control rate of temperature fall is 0.1-2 DEG C/h, until solution temperature is down to 25-35 DEG C in crystallizer；After solution temperature reaches 25-35 DEG C, continue that ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 3-5 DEG C/h, makes solution temperature in crystallizer be maintained at 25-35 DEG C, crystallization obtains 200 μm of granularity or more of spherical ammonium metavanadate.The present invention passes through the control to ammonium metavanadate solution crystallisation by cooling process conditional and parameter, 200 μm of granularity or more of spherical ammonium metavanadate product has been prepared, products obtained therefrom size uniformity, sphericity is high, granule strength is high, can satisfy the requirement of vanadium alloy and V electrolyte field to vanadic anhydride product granularity.Automation degree of equipment is high simultaneously, and technological operation is simple, is conducive to industrialized production, has a good application prospect.
Description
Technical field
The present invention relates to vanadium chemical fields, and in particular to a method of prepare big granularity ammonium metavanadate.
Background technique
Vanadium has the physicochemical property and mechanical property of many preciousnesses, thus is widely used in modernization industrial technology
In, it is important strategic materials.The vanadium of 80-85% is mainly used for adding agent in ferrous metals industry, makees alloying element, with system
Standby special steel.Vanadium has become China and develops the indispensable alloying element of new steel grade institute, is widely used in engineering machinery, vapour
Vehicle, Aeronautics and Astronautics, railway, steamer, skyscraper, bridge, oil transportation (gas) pipeline etc. manufacture multiple fields, referred to as " modern work
The monosodium glutamate of industry ".
Ammonium metavanadate is the crystalline powder of white, is slightly soluble in cold water, is dissolved in hot water and weak aqua ammonia.In air when calcination
Become vanadic anhydride.It is mainly used as chemical reagent, catalyst, battery material etc., it can also be used to produce vanadic anhydride.In height
In warm vanadium alloy smelting process, bulky grain size ammonium metavanadate can ensure that alloy formula is accurate, and ammonium metavanadate particle size is too small,
Vfanadium compound volatilization is serious, causes alloy compositions actual ratio to deviate formula, affects alloy property.
CN106241872B discloses a kind of preparation method of bulky grain ammonium metavanadate, dense by regulation sodium metavanadate solution
Degree, ammonium salt solution concentration, the adding manner of two kinds of solution and reaction time etc. influence the factor of crystallite dimension, use and feed it is heavy
Shallow lake law technology prepares that mean particle size is big, ammonium metavanadate product of narrow particle size distribution.
CN107434260A discloses a kind of preparation method of big granularity vanadic anhydride, includes the following steps: 1) to cold
But ammonium metavanadate mother liquor is passed through in crystallizer, keeping temperature is 85~100 DEG C, opens stirring；2) it is added into cooler crystallizer
Ammonium metavanadate crystal seed, segmented cooling obtain ammonium metavanadate crystal；3) the ammonium metavanadate crystal differential suspension for obtaining step 2) in
Inside cooler crystallizer, upper layer fine grain is taken out and is filtered；Lower layer's ammonium metavanadate crystal is taken out by bottom, is filtered, washed, done
Dry, calcining, obtains big granularity vanadic anhydride.
Although the ammonium metavanadate product of big granularity has been prepared in the above method, various in the prevalence of step,
It is complicated for operation, the problems such as state modulator is not flexible, it is unfavorable for the large-scale promotion in vanadium chemical field.Therefore, it is badly in need of exploitation one
The new method for preparing big granularity ammonium metavanadate product of kind, obtains the product haveing excellent performance, to meet vanadium alloy and V electrolyte
Requirement of the field to ammonium metavanadate granularity.
Summary of the invention
In view of problems of the prior art, big granularity ammonium metavanadate is prepared the purpose of the present invention is to provide a kind of
Method has been prepared 200 μm of granularity or more by the control to ammonium metavanadate solution crystallisation by cooling process conditional and parameter
Spherical ammonium metavanadate product.Products obtained therefrom size uniformity, sphericity is high, and granule strength is high, can satisfy vanadium alloy and vanadium electricity
Requirement of the liquid field to ammonium metavanadate granularity is solved, is had a good application prospect.
To achieve this purpose, the present invention adopts the following technical scheme:
The present invention provides a kind of methods for preparing big granularity ammonium metavanadate, the described method comprises the following steps:
(1) ammonium metavanadate solution is added in crystallizer, control rate of temperature fall is 0.1-2 DEG C/h, until solution in crystallizer
Temperature is down to 25-35 DEG C；
(2) after solution temperature reaches 25-35 DEG C in device to be crystallized, continue that ammonium metavanadate solution is added into crystallizer, control
Rate of temperature fall processed is 3-5 DEG C/h, so that solution temperature in crystallizer is maintained at 25-35 DEG C, crystallization obtains 200 μm of granularity or more of ball
Shape ammonium metavanadate.
The present invention is realized by the control for above-mentioned crystallization process parameter to the spherical ammonium metavanadate of big granularity (> 200
μm) preparation.Wherein, the present invention first cools down to ammonium metavanadate solution at 0.1-2 DEG C/h, under this rate, crystallization
Ammonium metavanadate in device forms biggish nucleus, when the nucleus in crystallize reaches certain amount, is continuously added into metavanadic acid
Ammonium salt solution, and controlling rate of temperature fall is 3-5 DEG C/h, under this rate, what ammonium metavanadate was formed before capable of being quickly aggregated in
Around nucleus, and then spherical ammonium metavanadate of the granularity at 200 μm or more is obtained.
According to the present invention, step (1) rate of temperature fall be 0.1-2 DEG C/h, such as can be 0.1 DEG C/h, 0.3 DEG C/h,
It is specific between 0.5 DEG C/h, 0.8 DEG C/h, 1.0 DEG C/h, 1.3 DEG C/h, 1.5 DEG C/h, 1.8 DEG C/h or 2 DEG C/h and above-mentioned numerical value
Point value, as space is limited and for concise consideration, the present invention no longer exclusive list.
As the rate of temperature fall of crystallizer in step (1) excessively slow (0.1 DEG C/h of <), crystallization time is too long, the nucleus of generation
It has been be precipitated that, while reducing production efficiency；As rate of temperature fall too fast (2 DEG C/h of >), the ammonium metavanadate quantity of big nucleus subtracts
It is few, it is unfavorable for preparing the ammonium metavanadate of big granularity.
According to the present invention, step (2) rate of temperature fall is 3-5 DEG C/h, such as can be 3 DEG C/h, 3.3 DEG C/h, 3.5
DEG C/h, 3.8 DEG C/h, 4 DEG C/h, 4.3 DEG C/h, 4.5 DEG C/h, the specific point value between 4.8 DEG C/h or 5 DEG C/h and above-mentioned numerical value,
As space is limited and for concise consideration, the present invention no longer exclusive list.
As the rate of temperature fall of crystallizer in step (2) excessively slow (3 DEG C/h of <), ammonium metavanadate reunion rate is slack-off, unfavorable
In the ammonium metavanadate for preparing big granularity；As rate of temperature fall too fast (5 DEG C/h of >), the too fast ammonium poly-vanadate caused that cools down is produced
Product are in irregular shape, are unfavorable for subsequent applications.
According to the present invention, the concentration of step (1) described ammonium metavanadate solution is 5-30g/L, such as can be 5g/L, 10g/
L, the specific point value between 15g/L, 20g/L, 25g/L or 30g/L and above-mentioned numerical value is examined as space is limited and for concise
Consider, the present invention no longer exclusive list.
According to the present invention, step (1) crystallizer is OSLO cooler crystallizer or DTB cooler crystallizer.
According to the present invention, the temperature difference≤5 of solution in crystallizer cooling water return water and crystallizer are controlled during entire crystallization
DEG C, it is therefore an objective to prevent heat exchange interface excessive temperature differentials from causing to break out nucleation in heat exchange interface, crystal, which is attached on tube wall, blocks pipeline.
According to the present invention, liquid level reaches overflow port in control crystallizer in step (1).
According to the present invention, liquid level is higher than overflow port in control crystallizer in step (2).
According to the present invention, the charging pump discharge for controlling crystallizer in crystallization process is 0.1-10m3/ h, such as can be
0.1m3/h、1m3/h、2m3/h、3m3/h、4m3/h、5m3/h、6m3/h、7m3/h、8m3/h、9m3/ h or 10m3/ h and above-mentioned number
Specific point value between value, as space is limited and for concise consideration, the present invention no longer exclusive list.
According to the present invention, the spherical ammonium metavanadate obtained to step (2) crystallization is successively filtered, and is washed, dry.
As a preferred technical solution, the method for the present invention for preparing big granularity ammonium metavanadate the following steps are included:
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 5-30g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 0.1-2 DEG C/h, until solution temperature is down to 25-35 DEG C in crystallizer, control crystallizer cooling water return water with it is molten in crystallizer
The temperature difference≤5 DEG C of liquid；
(3) after solution temperature reaches 25-35 DEG C in device to be crystallized, control charging pump discharge is 0.1-10m3/ h, continue to
Ammonium metavanadate solution is added in crystallizer, control rate of temperature fall is 3-5 DEG C/h, and solution temperature in crystallizer is made to be maintained at 25-35
DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallizer in crystallization process
The temperature difference≤5 DEG C of solution in cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Compared with prior art, the present invention is at least had the advantages that
(1) present invention is prepared by the control to ammonium metavanadate solution crystallisation by cooling process conditional and parameter
200 μm of granularity or more of spherical ammonium metavanadate product, products obtained therefrom size uniformity, sphericity is high, and granule strength is high, can satisfy
The requirement of vanadium alloy and V electrolyte field to vanadic anhydride product granularity.
(2) present device high degree of automation, technological operation is simple, is conducive to industrialized production, has good answer
Use prospect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram for the crystallizer that a kind of specific embodiment of the present invention provides.
The present invention is described in more detail below.But following examples is only simple example of the invention, not generation
Table or limitation the scope of the present invention, protection scope of the present invention are subject to claims.
Specific embodiment
To further illustrate the technical scheme of the present invention below with reference to the accompanying drawings and specific embodiments.
The method for preparing big granularity ammonium metavanadate that a kind of specific embodiment of the present invention provides can be used and be provided in Fig. 1
Crystallizer carry out.In preparation process, the solution in ammonium metavanadate solution surge tank is added to by crystallization by feed pump first
In device, until liquid level reaches overflow port；It is then turned on cooling water pump and circulating pump, by adjusting cooling water flow and circulation pump frequency
Control crystallizer rate of temperature fall；After the temperature of ammonium metavanadate solution reaches predetermined value in device to be crystallized, open feed pump continue to
Ammonium metavanadate solution is added in crystallizer, controls the rate of temperature fall and temperature of solution in crystallizer, and opens discharging pump discharging, knot
Liquid level is higher than the temperature difference≤5 of solution in overflow port and crystallizer cooling water return water and crystallizer in brilliant process control crystallizer
℃；After discharging pump discharging, by filtering, washing obtains 200 μm of granularity or more of spherical ammonium metavanadate after dry.
In order to better illustrate the present invention, it is easy to understand technical solution of the present invention, of the invention is typical but non-limiting
Embodiment is as follows:
Embodiment 1
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 20.12g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 0.5 DEG C/h, until solution temperature is down to 30 DEG C in crystallizer, the temperature of solution in control crystallizer cooling water return water and crystallizer
Difference≤1 DEG C；
(3) after solution temperature reaches 30 DEG C in device to be crystallized, feed pump continuous feed, feed rate 6m are opened3/ h, holds
Continue and ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 4 DEG C/h, and solution temperature in crystallizer is made to be maintained at 30
DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallizer in crystallization process
The temperature difference≤1 DEG C of solution in cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Through detecting: 200 μm of partial size > and 300 μm of < of content are 62% in obtained ammonium metavanadate product, partial size >=300
μm content be 38%.
Embodiment 2
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 25.68g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 1 DEG C/h, until solution temperature is down to 35 DEG C in crystallizer, the temperature difference of solution in control crystallizer cooling water return water and crystallizer
≤2℃；
(3) after solution temperature reaches 35 DEG C in device to be crystallized, feed pump continuous feed, feed rate 8m are opened3/ h, holds
Continue and ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 3.5 DEG C/h, and solution temperature in crystallizer is made to be maintained at 35
DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallizer in crystallization process
The temperature difference≤5 DEG C of solution in cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Through detecting: 200 μm of partial size > and 300 μm of < of content are 58% in obtained ammonium metavanadate product, partial size >=300
μm content be 42%.
Embodiment 3
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 16.73g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 2 DEG C/h, until solution temperature is down to 25 DEG C in crystallizer, the temperature difference of solution in control crystallizer cooling water return water and crystallizer
≤4℃；
(3) after solution temperature reaches 25 DEG C in device to be crystallized, feed pump continuous feed, feed rate 3m are opened3/ h, holds
Continue and ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 3 DEG C/h, and solution temperature in crystallizer is made to be maintained at 25
DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallizer in crystallization process
The temperature difference≤3 DEG C of solution in cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Through detecting: 200 μm of partial size > and 300 μm of < of content are 71% in obtained ammonium metavanadate product, partial size >=300
μm content be 29%.
Embodiment 4
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 9.86g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 0.1 DEG C/h, until solution temperature is down to 28 DEG C in crystallizer, the temperature of solution in control crystallizer cooling water return water and crystallizer
Difference≤5 DEG C；
(3) after solution temperature reaches 28 DEG C in device to be crystallized, feed pump continuous feed, feed rate 7m are opened3/ h, holds
Continue and ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 5 DEG C/h, and solution temperature in crystallizer is made to be maintained at 30
DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallizer in crystallization process
The temperature difference≤5 DEG C of solution in cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Through detecting: 200 μm of partial size > and 300 μm of < of content are 55% in obtained ammonium metavanadate product, partial size >=300
μm content be 45%.
Embodiment 5
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 5.03g/L is added in crystallizer, until liquid level reaches
Overflow port stops charging；
(2) cooling water and circulating pump are opened, by adjusting cooling water flow and circulation pump frequency control crystallizer cooling speed
Rate is 1.5 DEG C/h, until solution temperature is down to 33 DEG C in crystallizer, the temperature of solution in control crystallizer cooling water return water and crystallizer
Difference≤3 DEG C；
(3) after solution temperature reaches 33 DEG C in device to be crystallized, feed pump continuous feed, feed rate 10m are opened3/ h,
Continue that ammonium metavanadate solution is added into crystallizer, control rate of temperature fall is 4.5 DEG C/h, is maintained at solution temperature in crystallizer
30 DEG C, while discharging pump continuous discharge is opened, guarantee that mould liquid level is maintained at overflow port or more, controls crystallization in crystallization process
The temperature difference≤1 DEG C of solution in device cooling water return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
Through detecting: 200 μm of partial size > and 300 μm of < of content are 73% in obtained ammonium metavanadate product, partial size >=300
μm content be 27%.
Comparative example 1
Compared with Example 1, other than the rate of temperature fall of crystallizer in step (2) is adjusted to 0.05 DEG C/h, other steps
Rapid and condition is identical with embodiment 1.
The results show that crystallization time is too long, the nucleus of generation has been precipitated, partial size in subsequent obtained ammonium metavanadate product
Generally it is less than≤200 μm.
Comparative example 2
Compared with Example 1, other than the rate of temperature fall of crystallizer in step (2) is adjusted to 4 DEG C/h, other steps and
Condition is identical with embodiment 1.
Through detecting: the content of partial size≤200 μm is 35% in obtained ammonium metavanadate product, 200 μm of partial size > and < 300
μm content be 56%, the contents of partial size > 300 μm is 19%.
Comparative example 3
Compared with Example 1, other than the rate of temperature fall of crystallizer in step (3) is adjusted to 2 DEG C/h, other steps and
Condition is identical with embodiment 1.
Through detecting: the content of partial size≤200 μm is 27% in obtained ammonium metavanadate product, 200 μm of partial size > and < 300
μm content be 58%, the contents of partial size > 300 μm is 15%.
Comparative example 4
Compared with Example 1, other than the rate of temperature fall of crystallizer in step (2) is adjusted to 6 DEG C/h, other steps and
Condition is identical with embodiment 1.
Through detecting: obtained ammonium metavanadate product form is irregular, and size is different, affects the application performance of product.
Comparative example 5
Compared with Example 1, in addition to controlling solution in crystallizer cooling water return water and crystallizer in step (3) crystallization process
The temperature difference be 5.5 DEG C outer, other steps and condition are identical with embodiment 1.
The results show that crystal, which is attached on tube wall, blocks pipeline, the process of crystallization is affected.
The preferred embodiment of the present invention has been described above in detail, still, during present invention is not limited to the embodiments described above
Detail within the scope of the technical concept of the present invention can be with various simple variants of the technical solution of the present invention are made, this
A little simple variants all belong to the scope of protection of the present invention.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case where shield, can be combined in any appropriate way, in order to avoid unnecessary repetition, the present invention to it is various can
No further explanation will be given for the combination of energy.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (9)
1. a kind of method for preparing big granularity ammonium metavanadate, which is characterized in that the described method comprises the following steps:
(1) ammonium metavanadate solution is added in crystallizer, control rate of temperature fall is 0.1-2 DEG C/h, until solution temperature in crystallizer
It is down to 25-35 DEG C；
(2) after solution temperature reaches 25-35 DEG C in device to be crystallized, continue that ammonium metavanadate solution is added into crystallizer, control drop
Warm rate is 3-5 DEG C/h, and solution temperature is made in crystallizer to be maintained at 25-35 DEG C, crystallization obtain 200 μm of granularity or more it is spherical partially
Ammonium vanadate.
2. the method as described in claim 1, which is characterized in that the concentration of step (1) described ammonium metavanadate solution is 5-30g/
L。
3. method according to claim 1 or 2, which is characterized in that step (1) crystallizer be OSLO cooler crystallizer or
DTB cooler crystallizer.
4. the method according to claim 1, which is characterized in that control crystallizer cooling water during entire crystallization
The temperature difference≤5 DEG C of solution in return water and crystallizer.
5. method according to any of claims 1-4, which is characterized in that liquid level reaches in control crystallizer in step (1)
Overflow port.
6. the method according to claim 1 to 5, which is characterized in that liquid level is higher than in control crystallizer in step (2)
Overflow port.
7. as the method according to claim 1 to 6, which is characterized in that feed pump in control crystallization process in step (2)
Flow is 0.1-10m3/h。
8. the method according to claim 1 to 7, which is characterized in that step (2) are crystallized with obtained spherical metavanadic acid
Ammonium is successively filtered, and is washed, dry.
9. the method according to claim 1, which is characterized in that the described method comprises the following steps:
(1) feed pump is opened, the ammonium metavanadate solution that concentration is 5-30g/L is added in crystallizer, until liquid level reaches overflow
Mouthful, stop charging；
(2) cooling water and circulating pump are opened, is by adjusting cooling water flow and circulation pump frequency control crystallizer rate of temperature fall
0.1-2 DEG C/h, until solution temperature is down to 25-35 DEG C in crystallizer, solution in control crystallizer cooling water return water and crystallizer
The temperature difference≤5 DEG C；
(3) after solution temperature reaches 25-35 DEG C in device to be crystallized, control charging pump discharge is 0.1-10m3/ h continues to crystallizer
Middle addition ammonium metavanadate solution, control rate of temperature fall are 3-5 DEG C/h, so that solution temperature in crystallizer is maintained at 25-35 DEG C, simultaneously
Discharging pump continuous discharge is opened, guarantees that mould liquid level is maintained at overflow port or more, controls crystallizer cooling water in crystallization process
The temperature difference≤5 DEG C of solution in return water and crystallizer；
(4) it after discharging pump discharging, is successively filtered, washed, dried, obtain 200 μm of granularity or more of spherical ammonium metavanadate.
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