CN109179504B - Method for preparing large-particle-size ammonium metavanadate - Google Patents
Method for preparing large-particle-size ammonium metavanadate Download PDFInfo
- Publication number
- CN109179504B CN109179504B CN201811222095.6A CN201811222095A CN109179504B CN 109179504 B CN109179504 B CN 109179504B CN 201811222095 A CN201811222095 A CN 201811222095A CN 109179504 B CN109179504 B CN 109179504B
- Authority
- CN
- China
- Prior art keywords
- crystallizer
- solution
- ammonium metavanadate
- controlling
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention relates to a method for preparing large-particle-size ammonium metavanadate, which comprises the following steps: adding an ammonium metavanadate solution into a crystallizer, and controlling the cooling rate to be 0.1-2 ℃/h until the temperature of the solution in the crystallizer is reduced to 25-35 ℃; and after the temperature of the solution reaches 25-35 ℃, continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3-5 ℃/h, keeping the temperature of the solution in the crystallizer at 25-35 ℃, and crystallizing to obtain spherical ammonium metavanadate with the particle size of more than 200 mu m. According to the invention, spherical ammonium metavanadate products with the granularity of more than 200 mu m are prepared by controlling conditions and parameters in the cooling crystallization process of the ammonium metavanadate solution, and the obtained products have uniform size, high sphericity and high particle strength, and can meet the requirements of the vanadium pentoxide product granularity in the fields of vanadium alloys and vanadium electrolytes. Meanwhile, the equipment has high automation degree, the process operation is simple, the industrial production is facilitated, and the method has a good application prospect.
Description
Technical Field
The invention relates to the field of vanadium chemical industry, in particular to a method for preparing large-particle-size ammonium metavanadate.
Background
Vanadium has many valuable physicochemical and mechanical properties, and thus is widely used in modern industrial technology and is an important strategic material. 80-85% of vanadium is mainly used as additive agent and alloy element in ferrous metallurgy industry to prepare special steel. Vanadium has become an indispensable alloy element for developing new steel grades in China, is widely applied to a plurality of fields of manufacturing engineering machinery, automobiles, aviation, aerospace, railways, ships, high-rise buildings, bridges, oil (gas) pipelines and the like, and is called as monosodium glutamate in modern industry.
Ammonium metavanadate is a white crystalline powder, slightly soluble in cold water, soluble in hot water and dilute ammonia. When burned in air, becomes vanadium pentoxide. It is mainly used as chemical reagent, catalyst, battery material, etc. and can also be used for preparing vanadium pentoxide. In the smelting process of the high-temperature vanadium alloy, the large-particle-size ammonium metavanadate can ensure the accuracy of the alloy formula, the particle size of the ammonium metavanadate is too small, and vanadium compounds are seriously volatilized, so that the actual proportion of alloy components deviates from the formula, and the alloy performance is influenced.
CN106241872B discloses a method for preparing large-particle ammonium metavanadate, which is characterized in that a mixed-feeding precipitation method technology is adopted to prepare an ammonium metavanadate product with large average particle size and narrow particle size distribution by regulating and controlling factors influencing the grain size such as sodium metavanadate solution concentration, ammonium salt solution concentration, adding modes and reaction time of two solutions.
CN107434260A discloses a preparation method of large-particle-size vanadium pentoxide, which comprises the following steps: 1) introducing ammonium metavanadate mother liquor into a cooling crystallizer, keeping the temperature at 85-100 ℃, and starting stirring; 2) adding ammonium metavanadate crystal seeds into the cooling crystallizer, and cooling in sections to obtain ammonium metavanadate crystals; 3) suspending the ammonium metavanadate crystals obtained in the step 2) in a cooling crystallizer in layers, and taking out and filtering the upper fine crystals; and taking out the lower ammonium metavanadate crystal from the bottom, and filtering, washing, drying and calcining to obtain the large-granularity vanadium pentoxide.
Although the ammonium metavanadate products with large particle sizes are prepared by the methods, the problems of various steps, complex operation, inflexible parameter control and the like generally exist, and the methods are not beneficial to large-scale popularization in the field of vanadium chemical industry. Therefore, it is urgently needed to develop a new method for preparing large-particle-size ammonium metavanadate products to obtain products with excellent performance so as to meet the requirements of the vanadium alloy and vanadium electrolyte field on the particle size of the ammonium metavanadate.
Disclosure of Invention
In view of the problems in the prior art, the present invention aims to provide a method for preparing ammonium metavanadate with large particle size, wherein spherical ammonium metavanadate products with particle size of more than 200 μm are prepared by controlling conditions and parameters in the process of cooling and crystallizing ammonium metavanadate solution. The obtained product has uniform size, high sphericity and high particle strength, can meet the requirement of the field of vanadium alloy and vanadium electrolyte on the granularity of ammonium metavanadate, and has good application prospect.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a method for preparing large-particle-size ammonium metavanadate, which comprises the following steps of:
(1) adding an ammonium metavanadate solution into a crystallizer, and controlling the cooling rate to be 0.1-2 ℃/h until the temperature of the solution in the crystallizer is reduced to 25-35 ℃;
(2) and after the temperature of the solution in the crystallizer reaches 25-35 ℃, continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3-5 ℃/h, keeping the temperature of the solution in the crystallizer at 25-35 ℃, and crystallizing to obtain spherical ammonium metavanadate with the particle size of more than 200 mu m.
The invention realizes the preparation of large-particle-size spherical ammonium metavanadate (larger than 200 mu m) by controlling the parameters of the crystallization process. The method comprises the steps of firstly cooling an ammonium metavanadate solution at the speed of 0.1-2 ℃/h, wherein the ammonium metavanadate in a crystallizer forms larger crystal nuclei at the speed, when the crystal nuclei in the crystallizer reach a certain amount, the ammonium metavanadate solution is continuously added, the cooling speed is controlled to be 3-5 ℃/h, and at the speed, the ammonium metavanadate can be rapidly polymerized around the previously formed crystal nuclei, so that spherical ammonium metavanadate with the particle size of more than 200 mu m is obtained.
According to the invention, the cooling rate in step (1) is 0.1-2 ℃/h, for example 0.1 ℃/h, 0.3 ℃/h, 0.5 ℃/h, 0.8 ℃/h, 1.0 ℃/h, 1.3 ℃/h, 1.5 ℃/h, 1.8 ℃/h or 2 ℃/h, and the specific values therebetween are not exhaustive for reasons of space and simplicity.
When the cooling rate of the crystallizer in the step (1) is too slow (less than 0.1 ℃/h), the crystallization time is too long, the generated crystal nucleus is separated out, and the production efficiency is reduced; when the temperature reduction rate is too fast (more than 2 ℃/h), the quantity of the ammonium metavanadate with large crystal nucleus is reduced, which is not beneficial to preparing the ammonium metavanadate with large particle size.
According to the invention, the cooling rate in step (2) is 3-5 ℃/h, and can be, for example, 3 ℃/h, 3.3 ℃/h, 3.5 ℃/h, 3.8 ℃/h, 4 ℃/h, 4.3 ℃/h, 4.5 ℃/h, 4.8 ℃/h or 5 ℃/h, and specific values therebetween, and the invention is not exhaustive for reasons of space and simplicity.
When the cooling rate of the crystallizer in the step (2) is too low (less than 3 ℃/h), the agglomeration rate of the ammonium metavanadate is reduced, which is not beneficial to preparing the ammonium metavanadate with large granularity; when the cooling rate is too fast (more than 5 ℃/h), the obtained ammonium polyvanadate product is irregular in shape due to the too fast cooling, and the subsequent application is not facilitated.
According to the invention, the concentration of the ammonium metavanadate solution in the step (1) is 5-30g/L, for example, 5g/L, 10g/L, 15g/L, 20g/L, 25g/L or 30g/L, and the specific values therebetween are limited by space and for the sake of brevity, and the invention is not exhaustive.
According to the invention, the crystallizer of step (1) is an OSLO cooled crystallizer or a DTB cooled crystallizer.
According to the invention, the temperature difference between the cooling water return water of the crystallizer and the solution in the crystallizer is controlled to be less than or equal to 5 ℃ in the whole crystallization process, so that the problem that the temperature difference of a heat exchange interface is too large to cause the explosion nucleation on the heat exchange interface is solved, and crystals are attached to the pipe wall to block the pipeline.
According to the invention, in the step (1), the liquid level in the crystallizer is controlled to reach the overflow port.
According to the invention, in the step (2), the liquid level in the crystallizer is controlled to be higher than the overflow port.
According to the invention, the flow of the feed pump of the crystallizer during the crystallization process is controlled to be 0.1-10m3H, for example, may be 0.1m3/h、1m3/h、2m3/h、3m3/h、4m3/h、5m3/h、6m3/h、7m3/h、8m3/h、9m3H or 10m3The values of/h, and the specific points between the above values, are not exhaustive for the invention, being limited to space and for the sake of brevity.
According to the invention, the spherical ammonium metavanadate crystallized in the step (2) is sequentially filtered, washed and dried.
As a preferred technical scheme, the method for preparing large-particle-size ammonium metavanadate comprises the following steps:
(1) starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 5-30g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 0.1-2 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 25-35 ℃, and controlling the temperature difference between the backwater of the cooling water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃;
(3) controlling the flow of the feeding pump to be 0.1-10m after the temperature of the solution in the crystallizer reaches 25-35 DEG C3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3-5 ℃/h, keeping the temperature of the solution in the crystallizer at 25-35 ℃, simultaneously starting a discharging pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Compared with the prior art, the invention at least has the following beneficial effects:
(1) according to the invention, spherical ammonium metavanadate products with the granularity of more than 200 mu m are prepared by controlling conditions and parameters in the cooling crystallization process of the ammonium metavanadate solution, and the obtained products have uniform size, high sphericity and high particle strength, and can meet the requirements of the vanadium pentoxide product granularity in the fields of vanadium alloys and vanadium electrolytes.
(2) The invention has high automation degree of equipment and simple process operation, is beneficial to industrial production and has good application prospect.
Drawings
Fig. 1 is a schematic structural diagram of a crystallizer according to an embodiment of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
The technical scheme of the invention is further explained by the specific implementation mode in combination with the attached drawings.
The method for preparing ammonium metavanadate with large particle size provided by a specific embodiment of the invention can be carried out by adopting the crystallizer provided in FIG. 1. In the preparation process, firstly, adding the solution in an ammonium metavanadate solution buffer tank into a crystallizer through a feed pump until the liquid level reaches an overflow port; then starting a cooling water pump and a circulating pump, and controlling the cooling rate of the crystallizer by adjusting the flow rate of cooling water and the frequency of the circulating pump; after the temperature of the ammonium metavanadate solution in the crystallizer reaches a preset value, starting a feed pump to continuously add the ammonium metavanadate solution into the crystallizer, controlling the cooling rate and the temperature of the solution in the crystallizer, starting a discharge pump to discharge, and controlling the liquid level in the crystallizer to be higher than an overflow port and the temperature difference between the cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃ in the crystallization process; after the material is discharged by a discharge pump, spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained after filtering, washing and drying.
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
(1) Starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 20.12g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 0.5 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 30 ℃, and controlling the temperature difference between the cooling water backwater of the crystallizer and the solution in the crystallizer to be less than or equal to 1 ℃;
(3) after the temperature of the solution in the crystallizer reaches 30 ℃, starting a feeding pump to continuously feed, wherein the feeding flow is 6m3Continuously adding ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 4 ℃/h, keeping the temperature of the solution in the crystallizer at 30 ℃, simultaneously starting a discharge pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the cooling of the crystallizer during the crystallization processThe temperature difference between the backwater of cooling water and the solution in the crystallizer is less than or equal to 1 ℃;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Through detection: the obtained ammonium metavanadate product contains 62% of ammonium metavanadate with the particle size larger than 200 mu m and smaller than 300 mu m, and 38% of ammonium metavanadate with the particle size larger than or equal to 300 mu m.
Example 2
(1) Starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 25.68g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 1 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 35 ℃, and controlling the temperature difference between the backwater of the cooling water of the crystallizer and the solution in the crystallizer to be less than or equal to 2 ℃;
(3) after the temperature of the solution in the crystallizer reaches 35 ℃, starting a feeding pump to continuously feed, wherein the feeding flow is 8m3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3.5 ℃/h, keeping the temperature of the solution in the crystallizer at 35 ℃, simultaneously starting a discharging pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Through detection: the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 58 percent, and the content of the ammonium metavanadate product with the particle size of more than or equal to 300 mu m is 42 percent.
Example 3
(1) Starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 16.73g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 2 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 25 ℃, and controlling the temperature difference between the backwater of the cooling water of the crystallizer and the solution in the crystallizer to be less than or equal to 4 ℃;
(3) after the temperature of the solution in the crystallizer reaches 25 ℃, starting a feeding pump to continuously feed, wherein the feeding flow is 3m3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3 ℃/h, keeping the temperature of the solution in the crystallizer at 25 ℃, simultaneously starting a discharging pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 3 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Through detection: the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 71 percent, and the content of the ammonium metavanadate product with the particle size of more than or equal to 300 mu m is 29 percent.
Example 4
(1) Starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 9.86g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 0.1 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 28 ℃, and controlling the temperature difference between the backwater of the cooling water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃;
(3) after the temperature of the solution in the crystallizer reaches 28 ℃, starting a feeding pump to continuously feed, wherein the feeding flow is 7m3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 5 ℃/h, keeping the temperature of the solution in the crystallizer at 30 ℃, simultaneously starting a discharge pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Through detection: the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 55 percent, and the content of the ammonium metavanadate product with the particle size of more than or equal to 300 mu m is 45 percent.
Example 5
(1) Starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 5.03g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 1.5 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 33 ℃, and controlling the temperature difference between the cooling water backwater of the crystallizer and the solution in the crystallizer to be less than or equal to 3 ℃;
(3) after the temperature of the solution in the crystallizer reaches 33 ℃, starting a feeding pump to continuously feed, wherein the feeding flow is 10m3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 4.5 ℃/h, keeping the temperature of the solution in the crystallizer at 30 ℃, simultaneously starting a discharging pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 1 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Through detection: the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 73 percent, and the content of the ammonium metavanadate product with the particle size of more than or equal to 300 mu m is 27 percent.
Comparative example 1
The procedure and conditions were exactly the same as those in example 1 except that the temperature lowering rate of the crystallizer in step (2) was adjusted to 0.05 ℃/h as compared with example 1.
The result shows that the crystallization time is too long, the generated crystal nucleus is separated out, and the particle size of the ammonium metavanadate product obtained subsequently is generally less than or equal to 200 mu m.
Comparative example 2
The procedure and conditions were exactly the same as those in example 1 except that the temperature lowering rate of the crystallizer in step (2) was adjusted to 4 ℃/h as compared with example 1.
Through detection: the content of the ammonium metavanadate product with the particle size of less than or equal to 200 mu m is 35 percent, the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 56 percent, and the content of the ammonium metavanadate product with the particle size of more than 300 mu m is 19 percent.
Comparative example 3
The procedure and conditions were exactly the same as those in example 1 except that the temperature lowering rate of the crystallizer in step (3) was adjusted to 2 ℃/h as compared with example 1.
Through detection: the content of the ammonium metavanadate product with the particle size of less than or equal to 200 mu m is 27 percent, the content of the ammonium metavanadate product with the particle size of more than 200 mu m and less than 300 mu m is 58 percent, and the content of the ammonium metavanadate product with the particle size of more than 300 mu m is 15 percent.
Comparative example 4
The procedure and conditions were exactly the same as those in example 1 except that the temperature lowering rate of the crystallizer in step (2) was adjusted to 6 ℃/h as compared with example 1.
Through detection: the obtained ammonium metavanadate product has irregular shape and different size, and the application performance of the product is influenced.
Comparative example 5
Compared with the embodiment 1, the method has the same steps and conditions as the embodiment 1 except that the temperature difference between the cooling water return water of the crystallizer and the solution in the crystallizer is controlled to be 5.5 ℃ in the crystallization process of the step (3).
The results show that crystals adhere to the tube wall and block the tube, affecting the progress of crystallization.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.
Claims (7)
1. A method for preparing large-particle size ammonium metavanadate, comprising the steps of:
(1) adding an ammonium metavanadate solution into a crystallizer, and controlling the cooling rate to be 0.1-2 ℃/h until the temperature of the solution in the crystallizer is reduced to 25-35 ℃;
(2) continuously adding an ammonium metavanadate solution into the crystallizer after the temperature of the solution in the crystallizer reaches 25-35 ℃, controlling the cooling rate to be 3-5 ℃/h, keeping the temperature of the solution in the crystallizer at 25-35 ℃, and crystallizing to obtain spherical ammonium metavanadate with the particle size of more than 200 mu m;
the temperature difference between the cooling water return water of the crystallizer and the solution in the crystallizer is controlled to be less than or equal to 5 ℃ in the whole crystallization process;
controlling the flow of a feed pump to be 0.1-10m in the crystallization process in the step (2)3/h。
2. The method of claim 1, wherein the ammonium metavanadate solution of step (1) has a concentration of 5 to 30 g/L.
3. The method of claim 1 or 2, wherein the crystallizer of step (1) is an OSLO cooled crystallizer or a DTB cooled crystallizer.
4. The method of claim 1 or 2, wherein the liquid level in the crystallizer is controlled to reach the overflow port in step (1).
5. The method of claim 4, wherein the liquid level in the crystallizer is controlled to be higher than the overflow port in the step (2).
6. The method according to claim 1 or 2, wherein the spherical ammonium metavanadate crystallized in the step (2) is sequentially filtered, washed and dried.
7. The method of claim 1, wherein the method comprises the steps of:
(1) starting a feeding pump, adding an ammonium metavanadate solution with the concentration of 5-30g/L into the crystallizer until the liquid level reaches an overflow port, and stopping feeding;
(2) starting cooling water and a circulating pump, controlling the cooling rate of the crystallizer to be 0.1-2 ℃/h by adjusting the flow rate of the cooling water and the frequency of the circulating pump until the temperature of the solution in the crystallizer is reduced to 25-35 ℃, and controlling the temperature difference between the backwater of the cooling water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃;
(3) controlling the flow of the feeding pump to be 0.1-10m after the temperature of the solution in the crystallizer reaches 25-35 DEG C3Continuously adding an ammonium metavanadate solution into the crystallizer, controlling the cooling rate to be 3-5 ℃/h, keeping the temperature of the solution in the crystallizer at 25-35 ℃, simultaneously starting a discharging pump to continuously discharge, ensuring that the liquid level of the crystallizer is kept above an overflow port, and controlling the temperature difference between cooling water return water of the crystallizer and the solution in the crystallizer to be less than or equal to 5 ℃ in the crystallization process;
(4) after the material is discharged by a discharge pump, the spherical ammonium metavanadate with the granularity of more than 200 mu m is obtained by filtering, washing and drying in sequence.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811222095.6A CN109179504B (en) | 2018-10-19 | 2018-10-19 | Method for preparing large-particle-size ammonium metavanadate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811222095.6A CN109179504B (en) | 2018-10-19 | 2018-10-19 | Method for preparing large-particle-size ammonium metavanadate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109179504A CN109179504A (en) | 2019-01-11 |
| CN109179504B true CN109179504B (en) | 2020-12-04 |
Family
ID=64946269
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811222095.6A Active CN109179504B (en) | 2018-10-19 | 2018-10-19 | Method for preparing large-particle-size ammonium metavanadate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109179504B (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003443A (en) * | 2014-06-13 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium metavanadate by adding seed crystals |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106430305A (en) * | 2016-08-31 | 2017-02-22 | 大连博融新材料股份有限公司 | Production method of high-density ammonium metavanadate |
| CN107434260A (en) * | 2017-09-04 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of preparation method of big granularity vanadic anhydride |
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
-
2018
- 2018-10-19 CN CN201811222095.6A patent/CN109179504B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104003443A (en) * | 2014-06-13 | 2014-08-27 | 攀钢集团攀枝花钢铁研究院有限公司 | Method for preparing ammonium metavanadate by adding seed crystals |
| CN106241872A (en) * | 2016-07-29 | 2016-12-21 | 中南大学 | A kind of preparation method of bulky grain ammonium metavanadate |
| CN106430305A (en) * | 2016-08-31 | 2017-02-22 | 大连博融新材料股份有限公司 | Production method of high-density ammonium metavanadate |
| CN107434260A (en) * | 2017-09-04 | 2017-12-05 | 河钢股份有限公司承德分公司 | A kind of preparation method of big granularity vanadic anhydride |
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
Non-Patent Citations (2)
| Title |
|---|
| Ammonium metavanadate: an effective catalyst for synthesis of α-hydroxyphosphonates;Swapnil S. Sonar et al.;《ARKIVOC》;20091231;第138-148页 * |
| 碳酸氢铵溶液中偏钒酸铵的冷却结晶;郭雪梅等;《化工进展》;20180331;第37卷(第3期);第853-860页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109179504A (en) | 2019-01-11 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111874958B (en) | Wet synthesis method of NCMA high-nickel quaternary precursor | |
| CN109081374B (en) | Method for preparing large-particle-size spherical ammonium polyvanadate | |
| CN105600809A (en) | Method and device for preparing lithium hexafluorophosphate through dynamic crystallization | |
| CN110451582B (en) | Method for continuously producing ferric trichloride | |
| CN106430305A (en) | Production method of high-density ammonium metavanadate | |
| Wang et al. | Advances in reactive co-precipitation technology for preparing high-performance cathodes | |
| CN102745662A (en) | Preparation method of amorphous iron phosphate | |
| CN113025833A (en) | Method for precipitating vanadium from high-concentration vanadium solution | |
| CN104944475B (en) | A kind of preparation method of super coarse granule high-purity cobalt carbonate | |
| CN105016373A (en) | Method for producing copper chloride through waste etching liquid containing copper | |
| CN109179504B (en) | Method for preparing large-particle-size ammonium metavanadate | |
| CN114210965A (en) | Metallic silver and preparation method and application thereof | |
| CN101269804B (en) | Method for producing high-purity phosphoric acid crystal | |
| CN102126756B (en) | Method for producing industrial grade ammonium paramolybdate | |
| WO2024139112A1 (en) | Process and system for preparing iron phosphate by using out-of-kettle circulating mixing and stirring | |
| CN114054767A (en) | Molybdenum powder and preparation process thereof | |
| CN102887870B (en) | Octogen for detonating tube | |
| CN110453091B (en) | Method for preparing high-purity cobalt solution from cobalt alloy waste | |
| CN111661856A (en) | Preparation method of large-particle spherical sodium sulfate crystal | |
| CN114572954B (en) | Method for preparing battery grade ferric phosphate by using pyrite cinder | |
| CN103708566B (en) | Method for improving filtering performance of ferrous sulfate | |
| CN106800303B (en) | Method for preparing potassium iodide by using microchannel reactor | |
| CN110433522B (en) | Production method for continuous crystallization of thiourea | |
| CN103803640B (en) | Method for preparing nanometer ITO (indium tin oxide) powder by virtue of coprecipitation method | |
| CN102921959A (en) | Method for preparing metal bismuth powder by using microwave hydrothermal method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |