CN212450666U - Preparation system of high solubility ammonium metatungstate - Google Patents
Preparation system of high solubility ammonium metatungstate Download PDFInfo
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- CN212450666U CN212450666U CN202022130982.XU CN202022130982U CN212450666U CN 212450666 U CN212450666 U CN 212450666U CN 202022130982 U CN202022130982 U CN 202022130982U CN 212450666 U CN212450666 U CN 212450666U
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Abstract
The utility model discloses a preparation system of high solubility ammonium metatungstate belongs to the metallurgical field, and the preparation side includes including following step: activating the raw material ammonium paratungstate at the temperature of 240-400 ℃ to obtain an activated product; mixing and dissolving the activated product and pure water, simultaneously heating to boil to obtain a mixed solution, and adjusting the pH value of the mixed solution to obtain a dilute ammonium metatungstate solution; aging, filtering, heating and concentrating the dilute ammonium metatungstate solution obtained in the step two to obtain a concentrated ammonium metatungstate solution; and (4) drying the concentrated ammonium metatungstate solution in the third step to obtain an ammonium metatungstate product. The method converts the ammonium paratungstate raw material into the ammonium metatungstate which is easy to dissolve in water through the activation step. The solubility of the ammonium metatungstate product prepared by the method is higher than 3000g/L, the solubility and the purity of the ammonium metatungstate product in the prior art are improved, and the requirements of high-end customers are met.
Description
Technical Field
The utility model relates to a metallurgical field, concretely relates to preparation method and system of high solubility ammonium metatungstate.
Background
Ammonium metatungstate is an important tungsten-containing compound, is mainly used for manufacturing various petrochemical catalysts and other tungsten compounds, and is a main raw material of a tungsten-based catalyst in an oil refinery. With the development of industries such as petroleum refining and petrochemical industry, the use amount of ammonium metatungstate is increased.
The production method of ammonium metatungstate can be roughly divided into two major types, namely a solid phase conversion method and a liquid phase conversion method.
The typical process of the solid phase conversion method is a thermal degradation method using APT as a raw material, which is mainly characterized in that APT is pyrolyzed to generate a large-water-soluble amorphous ammonium metatungstate substance by controlling the pyrolysis temperature of APT and the partial pressure of ammonia and water vapor, then the amorphous ammonium metatungstate substance is hydrated to prepare an ammonium metatungstate solution, and the solution is concentrated, cooled and crystallized to obtain the AMT solid.
The liquid phase conversion method, such as ion exchange method, neutralization method, nanofiltration method, etc., uses APT or sodium tungstate as raw material, and converts the raw material solution into ammonium metatungstate solution by adjusting the pH of the raw material solution, and then filters to remove insoluble impurities, and then prepares ammonium metatungstate by crystallization or spray drying.
However, both methods have their own and also their own disadvantages.
In the solid phase conversion method, the investment of the thermal cracking equipment is relatively high, but the most remarkable advantages are that the produced ammonium metatungstate product has high purity, good solubility and short production flow. However, the greatest disadvantage is the control of the thermal cracking temperature. The temperature is not well controlled, the phenomenon of over-burning or under-burning is easy to occur, the thermal degradation endpoint is difficult to judge, and the conversion rate is not stable. When the temperature is too high, APT is thermally cracked into insoluble tungsten trioxide; the temperature is too low, APT thermal cracking is insufficient, and the conversion rate is low. In developed countries, the mainstream production process is solid phase inversion.
The liquid phase conversion method mostly uses APT or ammonium tungstate as raw materials, and adopts different methods to reduce the pH value of the solution to a proper range to convert the solution into the ammonium metatungstate solution. At present, the domestic mainstream production process is still a liquid phase transformation method.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to solve one of the technical problem that exists among the prior art at least, provide a preparation method and system of high solubility ammonium metatungstate.
The technical solution of the utility model is as follows:
a preparation method of high-solubility ammonium metatungstate comprises the following steps:
the method comprises the following steps: activating the raw material ammonium paratungstate at the temperature of 240-400 ℃ to obtain an activated product;
step two: mixing and dissolving the activated product in the step one with pure water, simultaneously heating to boil to obtain a mixed solution, and adjusting the pH value of the mixed solution to obtain a dilute ammonium metatungstate solution;
step three: aging, filtering, heating and concentrating the dilute ammonium metatungstate solution obtained in the step two to obtain a concentrated ammonium metatungstate solution;
step four: and (4) drying the concentrated ammonium metatungstate solution in the third step to obtain an ammonium metatungstate product.
Preferably, in the first step, the number of activation times is at least 2, and the first activation temperature is: at the temperature of 250 ℃ and 350 ℃, the activation time is 20-70min, and the second activation temperature is as follows: 250 ℃ and 400 ℃, and the activation time is 20-70 min.
Preferably, in the second step, the conductivity of the pure water is less than 10 us/cm.
Preferably, in the second step, the pH of the mixed solution is adjusted to 3-5 when the mixed solution WO is used3When the content reaches 200-250g/L, boiling and stirring for more than 30 minutes, and aging for 1-3 hours.
Preferably, the third step is specifically to stand and age the dilute ammonium metatungstate solution in the second step for 4 to 8 hours, and filter to obtain a first filtrate; heating and concentrating the first filtrate, controlling the pH value of the solution to be 2.5-4 and the specific gravity of the solution to be 1.8-2.0, cooling, standing, aging for 4-8 hours, and filtering to obtain a second filtrate; heating and concentrating the second filtrate, controlling the pH value of the solution to be 2.5-3.5 and the specific gravity of the solution to be 2.2-2.4, cooling, standing, aging for 4-8 hours, and filtering to obtain a concentrated ammonium metatungstate solution.
Preferably, in the third step, the concentration of the concentrated ammonium metatungstate solution is more than 3000 g/L.
The utility model also discloses a preparation system of high solubility ammonium metatungstate is provided with according to the preface along the direction of feed:
the rotary furnace is used for activating the raw material ammonium paratungstate;
the stirring tank is used for preparing a dilute ammonium metatungstate solution;
the aging tank is used for aging the dilute ammonium metatungstate solution;
the filtering equipment is used for filtering the aged dilute ammonium metatungstate solution;
the reaction kettle is internally provided with a heating device and used for heating and concentrating the filtered dilute ammonium metatungstate solution to prepare a concentrated ammonium metatungstate solution;
and the spray drying equipment is used for drying the concentrated ammonium metatungstate solution.
Preferably, filtration equipment includes first coarse filtration equipment, second coarse filtration equipment and nanofiltration equipment, be provided with the two-stage filter cloth in the first coarse filtration equipment, be provided with the level four filter cloth in the second coarse filtration equipment, be provided with the macromolecule and receive the filter membrane in the nanofiltration equipment.
Preferably, the stirring tank comprises a tank body, a stirring device is arranged in the tank body, the wall part of the tank body is of a double-shell structure and comprises an outer shell and an inner shell, and a heating cavity is formed between the outer shell and the inner shell.
Preferably, the stirring device comprises a stirring shaft and a driving device for driving the stirring shaft to rotate, wherein a plurality of layers of stirring blades are arranged on the stirring shaft, and turbulent flow holes are formed in the stirring blades.
The utility model discloses one of following beneficial effect has at least:
1. the utility model discloses an activation step turns into ammonium paratungstate raw materials into the ammonium metatungstate of soluble in water, has avoided the shortcoming that pyrolysis temperature is difficult to control, the difficult judgement of thermal degradation terminal point in traditional solid phase transformation method, has improved ammonium metatungstate's conversion rate and solubility, makes the product through dissolving, concentration, drying process again, and the production flow who is shorter than traditional liquid phase transformation method, and the solubility is high, and product purity is high.
2. The utility model discloses an at least twice activation step for ammonium paratungstate can obtain the activation energy, takes off partial crystallization water and takes off partial ammonia more easily, and the reaction goes on to the positive direction, thereby makes its conversion obtain improving.
3. The utility model discloses a multiple ageing, filtration, intensification are concentrated, make concentrated ammonium metatungstate solution, make things convenient for subsequent processing with the concentration of rare ammonium metatungstate.
4. The utility model prepares a first filtrate by standing and aging the obtained dilute ammonium metatungstate solution for 4 to 8 hours and filtering; heating and concentrating the first filtrate, and controlling the pH value of the solution to be 2.5-4, wherein when the specific gravity of the solution reaches 1.8-2.0; cooling, standing and aging for 4-8 hours, and filtering by using a high-molecular nanofiltration membrane to obtain a second filtrate; heating and concentrating the second filtrate, controlling the pH value of the solution to be 2.5-3.5, cooling, standing and aging for 4-8 hours when the specific gravity of the solution reaches 2.2-2.4, and filtering to obtain the high-purity concentrated ammonium metatungstate solution. By the process operation, the concentration efficiency is high, the product loss is less, and the conversion rate is high.
5. The utility model discloses a preparation system adopts spray drying equipment to carry out the drying, and the product purity that makes is high, carries out multistage filtration simultaneously, and product purity is high for it is high in follow-up technology solubility, sets up the vortex hole on the stirring leaf of agitator tank, and the stirring is more even, makes its reaction efficiency higher.
Drawings
FIG. 1 is a schematic flow chart of a first embodiment of the method of the present invention;
FIG. 2 is a first schematic structural view of a preparation system according to a second embodiment of the present invention;
FIG. 3 is a schematic structural view of a second embodiment of the manufacturing system of the present invention;
FIG. 4 is a schematic structural view of a stirring tank according to a second embodiment of the present invention;
in the figure, 100-rotary kiln, 200-stirring tank, 201-outer shell, 202-inner shell, 203-stirring blade, 204-burbling hole, 205-driving device, 300-aging tank, 400-filtering device, 401-first coarse filtering device, 402-second coarse filtering device, 403-nanofiltration device, 500-reaction kettle, 600-spray drying device.
Detailed Description
This section will describe in detail the embodiments of the present invention, preferred embodiments of the present invention are shown in the attached drawings, which are used to supplement the description of the text part of the specification with figures, so that one can intuitively and vividly understand each technical feature and the whole technical solution of the present invention, but they cannot be understood as the limitation of the protection scope of the present invention.
In the description of the present invention, it should be understood that the orientation or positional relationship indicated with respect to the orientation description, such as up, down, front, rear, left, right, etc., is based on the orientation or positional relationship shown in the drawings, and is only for convenience of description and simplification of description, and does not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention.
In the description of the present invention, a plurality of means are one or more, a plurality of means are two or more, and the terms greater than, less than, exceeding, etc. are understood as not including the number, and the terms greater than, less than, within, etc. are understood as including the number. If the first and second are described for the purpose of distinguishing technical features, they are not to be understood as indicating or implying relative importance or implicitly indicating the number of technical features indicated or implicitly indicating the precedence of the technical features indicated.
In the description of the present invention, unless there is an explicit limitation, the words such as setting, installation, connection, etc. should be understood in a broad sense, and those skilled in the art can reasonably determine the specific meanings of the above words in combination with the specific contents of the technical solution.
Reference is made to fig. 1-4; the utility model discloses a first embodiment:
a preparation method of high-solubility ammonium metatungstate comprises the following steps:
the method comprises the following steps: activating the raw material ammonium paratungstate at the temperature of 240-400 ℃ to obtain an activated product;
the chemical reaction formula is as follows: 5 (NH)4)2O·12WO3·H2O＝4NH3+(NH4)6[H2W12O40]·2H2O
The activation step can make the ammonium paratungstate lose crystal water and remove part of ammonia to activate the ammonium paratungstate dissolved in water;
step two: mixing and dissolving the activated product in the step one with pure water, simultaneously heating to boil to obtain a mixed solution, and adjusting the pH value of the mixed solution to obtain a dilute ammonium metatungstate solution;
step three: aging, filtering, heating and concentrating the dilute ammonium metatungstate solution obtained in the step two to obtain a concentrated ammonium metatungstate solution; recycling the filtered filter residue;
step four: and (4) drying the concentrated ammonium metatungstate solution in the third step to obtain an ammonium metatungstate product.
In the first step, the activation times are at least 2 times, and the first activation temperature is as follows: at the temperature of 250 ℃ and 350 ℃, the activation time is 20-70min, and the second activation temperature is as follows: 250 ℃ and 400 ℃, and the activation time is 20-70 min.
In the second step, the conductivity of the pure water is less than 10us/cm, the smaller the conductivity of the pure water is, the higher the purity of the pure water is, namely, the content of other ionic impurities is low, and the influence on the reaction is reduced.
In the second step, the pH value of the mixed solution is adjusted to 3-5 when the solution WO is used3When the content reaches 200-250g/L, boiling and stirring for more than 30 minutes, and aging for 1-3 hours.
The third step is specifically that the dilute ammonium metatungstate solution in the second step is stood and aged for 4-8 hours, and is filtered to prepare a first filtrate; heating and concentrating the first filtrate, controlling the pH value of the solution to be 2.5-4 and the specific gravity of the solution to be 1.8-2.0, cooling, standing, aging for 4-8 hours, and filtering to obtain a second filtrate; heating and concentrating the second filtrate, controlling the pH value of the solution to be 2.5-3.5 and the specific gravity of the solution to be 2.2-2.4, cooling, standing, aging for 4-8 hours, and filtering to obtain a concentrated ammonium metatungstate solution.
In the third step, the concentration of the concentrated ammonium metatungstate solution is more than 3000 g/L.
The following specific examples are used to further illustrate the technical solutions of the first embodiment.
The specific gravity of a solution referred to in this application is the mass of the solution per volume of the solution.
Example 1
Activating the raw material ammonium paratungstate in a rotary furnace 100 at the temperature of 240 ℃ for 75min to obtain an activated product; mixing the activated product with pure water in a stirring tank 200, wherein the conductivity of the pure water is 9us/cm, stirring, simultaneously heating to boil, and controlling the pH value of the solution to be 3. When the solution is WO3When the content reaches 200g/L, boiling and stirring for 30 minutes, and aging for 2 hours. Filtering to obtain a dilute ammonium metatungstate solution;
standing and aging the obtained dilute ammonium metatungstate solution in an aging tank 300 for 4 hours, and performing two-stage filtration in a first coarse filtration device 401 to obtain a first filtrate; pumping the first filtrate into a reaction kettle, heating to 500 deg.C for concentration, controlling the pH value of the solution at 2.5, stopping pumping the first filtrate when the specific gravity of the solution reaches 1.8, cooling, standing and aging in an aging tank 300 for 4 hours, and filtering with a nanofiltration device 403 to obtain a second filtrate; pumping the second filtrate into a reaction kettle 500, heating and concentrating, controlling the pH value of the solution to be 2.5, stopping pumping the second filtrate when the specific gravity of the solution reaches 2.2, cooling, standing and aging in an aging tank 300 for 4 hours, and performing four-stage filtration in a second rough filtration device 402 to obtain the high-purity concentrated ammonium metatungstate solution.
Spray drying of the concentrated high-purity ammonium metatungstate solution: and drying the obtained high-purity ammonium metatungstate solution by adopting spray drying equipment, and specifically preparing a high-purity and high-solubility ammonium metatungstate product by adopting domestic advanced high-speed centrifugal spray drying equipment.
Example 2
Activating the raw material ammonium paratungstate in a rotary furnace 100 at 290 ℃ for 45min to obtain an activated product; mixing the activated product with pure water in a stirring tank 200, wherein the conductivity of the pure water is 8us/cm, stirring, simultaneously heating to boil, and controlling the pH value of the solution to be 3. When the solution is WO3When the content reaches 200g/L, boiling and stirring for 30 minutes, and aging for 2 hours. Filtering to obtain a dilute ammonium metatungstate solution;
standing and aging the obtained dilute ammonium metatungstate solution in an aging tank 300 for 4 hours, and performing two-stage filtration in a first coarse filtration device 401 to obtain a first filtrate; pumping the first filtrate into a reaction kettle, heating to 500 deg.C for concentration, controlling the pH value of the solution at 2.5, stopping pumping the first filtrate when the specific gravity of the solution reaches 1.8, cooling, standing and aging in an aging tank 300 for 4 hours, and filtering with a nanofiltration device 403 to obtain a second filtrate; pumping the second filtrate into a reaction kettle 500, heating and concentrating, controlling the pH value of the solution to be 2.5, stopping pumping the second filtrate when the specific gravity of the solution reaches 2.2, cooling, standing and aging in an aging tank 300 for 4 hours, and performing four-stage filtration in a second rough filtration device 402 to obtain the high-purity concentrated ammonium metatungstate solution.
Spray drying of the concentrated high-purity ammonium metatungstate solution: and drying the obtained high-purity ammonium metatungstate solution by adopting spray drying equipment, and specifically preparing a high-purity and high-solubility ammonium metatungstate product by adopting domestic advanced high-speed centrifugal spray drying equipment.
Example 3
Activating the raw material ammonium paratungstate in a rotary furnace 100 at the temperature of 260 ℃ for 65min to obtain an activated product; mixing the activated product with pure water in a stirring tank 200, wherein the conductivity of the pure water is 8us/cm, stirring, simultaneously heating to boil, and controlling the pH value of the solution at 4. When the solution is WO3When the content reaches 200g/L, the mixture is boiled and stirred for 35 minutes and aged for 2 hours. Filtering to obtain a dilute ammonium metatungstate solution;
standing and aging the obtained dilute ammonium metatungstate solution in an aging tank 300 for 6 hours, and performing two-stage filtration in a first coarse filtration device 401 to obtain a first filtrate; pumping the first filtrate into a reaction kettle, heating to 500 ℃ for concentration, controlling the pH value of the solution to be 3, stopping pumping the first filtrate when the specific gravity of the solution reaches 2.0, cooling, standing and aging in an aging tank 300 for 6 hours, and filtering with a nanofiltration device 403 to obtain a second filtrate; pumping the second filtrate into a reaction kettle 500, heating and concentrating, controlling the pH value of the solution to be 2.5, stopping pumping the second filtrate when the specific gravity of the solution reaches 2.2, cooling, standing and aging in an aging tank 300 for 6 hours, and performing four-stage filtration in a second rough filtration device 402 to obtain the high-purity concentrated ammonium metatungstate solution.
Spray drying of the concentrated high-purity ammonium metatungstate solution: and drying the obtained high-purity ammonium metatungstate solution by adopting spray drying equipment, and specifically preparing a high-purity and high-solubility ammonium metatungstate product by adopting domestic advanced high-speed centrifugal spray drying equipment.
Example 4
This example is a modification of example 2, specifically, 2 times of activation, the first activation: temperature 260 ℃, time 50min, second activation: the temperature is 350 deg.C and the time is 45 min.
Example 5
This example is a modification of example 2, specifically, 3 times of activation, the first activation: holding at 270 deg.C for 45min, second activation: keeping at 400 deg.C for 55min, activating for the third time: the temperature was maintained at 290 ℃ for 65 min.
Example 6
This example is a modification of example 2, specifically, 3 times of activation, the first activation: keeping at 280 deg.C for 50min, at 295 deg.C for 60min, and at 280 deg.C for 70 min.
Comparative example 1
Mixing raw materials of ammonium paratungstate and pure water in a stirring tank 200, wherein the conductivity of the pure water is 9us/cm, stirring, simultaneously heating to boil, and controlling the pH value of the solution to be 3. When the solution is WO3When the content reaches 200g/L, boiling and stirring for 30 minutes, and aging for 2 hours. Filtering to obtain a dilute ammonium metatungstate solution;
standing and aging the obtained dilute ammonium metatungstate solution in an aging tank 300 for 4 hours, and performing two-stage filtration in a first coarse filtration device 401 to obtain a first filtrate; pumping the first filtrate into a reaction kettle, heating to 500 deg.C for concentration, controlling the pH value of the solution at 2.5, stopping pumping the first filtrate when the specific gravity of the solution reaches 1.8, cooling, standing and aging in an aging tank 300 for 4 hours, and filtering with a nanofiltration device 403 to obtain a second filtrate; pumping the second filtrate into a reaction kettle 500, heating and concentrating, controlling the pH value of the solution to be 2.5, stopping pumping the second filtrate when the specific gravity of the solution reaches 2.2, cooling, standing and aging in an aging tank 300 for 4 hours, and performing four-stage filtration in a second rough filtration device 402 to obtain the high-purity concentrated ammonium metatungstate solution.
Spray drying of the concentrated high-purity ammonium metatungstate solution: and drying the obtained high-purity ammonium metatungstate solution by adopting spray drying equipment, and specifically preparing a high-purity and high-solubility ammonium metatungstate product by adopting domestic advanced high-speed centrifugal spray drying equipment.
Comparative example 2
Activating the raw material ammonium paratungstate in a rotary furnace 100 at 290 ℃ for 45min to obtain an activated product; mixing the activated product with pure water in a stirring tank 200, wherein the conductivity of the pure water is less than 10us/cm, stirring, simultaneously heating to boil, and controlling the pH value of the solution to be 3. When the solution is WO3When the content reaches 200g/L, boiling and stirring for 30 minutes, and aging for 2 hours. Filtering to obtain a dilute ammonium metatungstate solution;
standing and aging the obtained dilute ammonium metatungstate solution in an aging tank 300 for 4 hours, and performing two-stage filtration in a first coarse filtration device 401 to obtain a filtrate; pumping the filtrate into a reaction kettle, heating to 500 ℃ and concentrating to obtain high-purity concentrated ammonium metatungstate solution.
Solubility tests (solubility in water at 30 ℃ C.) were carried out for the examples and comparative examples, and the test values are shown in Table 1.
The chemical reaction formula is as follows: 5 (NH)4)2O·12WO3·H2O＝4NH3+(NH4)6[H2W12O40]·2H2O
Simultaneously, the tungsten content of the activated product is tested by adopting an absorptiometry method, in particular to WO in the activated product3In mass ratio of (a).
TABLE 1 Performance test values of examples and comparative examples
| Test specimen | The tungsten content of the activated product is (wt%) | Solubility (g/L) of ammonium metatungstate |
| Example 1 | 93 | 3010 |
| Example 2 | 94 | 3020 |
| Example 3 | 92 | 3020 |
| Example 4 | 94 | 3050 |
| Example 5 | 95 | 3070 |
| Example 6 | 94.5 | 3040 |
| Comparative example 1 | 88 | 2010 |
| Comparative example 2 | 93 | 2090 |
As can be seen from the above table, the activated product in the example has a higher tungsten content than the comparative example, and the ammonium metatungstate product in the example has a higher solubility than the comparative example, wherein the activated product in the example 5 has a tungsten content of 95 wt%, the ammonium metatungstate product has a solubility as high as 3070g/L, while the activated product in the comparative example 1 has a tungsten content of 90 wt% and a solubility of only 1050g/L, and as can be seen from the comparative analysis of the comparative example 1, the activation step in the example can activate the ammonium paratungstate with lost crystal water and part of ammonia removed to water-soluble ammonium metatungstate, and at a certain temperature, the conversion rate of ammonium metatungstate is increased, so that the tungsten content of the activated product is increased, the purity of the subsequent product is high, and the solubility is also greatly increased; in comparative example 2, only one filtration is adopted, the filtration precision is low, and impurities are easy to exist in the product, so that the solubility of the product is low. Examples 4 to 6 are superior to examples 1 to 3 mainly due to the influence of the number of activation times, and examples 4 to 6 adopt multiple activation, so that the conversion rate of ammonium paratungstate to ammonium metatungstate is improved, and ammonium metatungstate is easily soluble in water, so that the solubility of ammonium metatungstate is improved.
The utility model discloses the second embodiment is still provided:
a system for preparing high-solubility ammonium metatungstate, which is applied to the first embodiment; specifically, there are provided in order along the direction of feed:
a rotary kiln 100 for activating the raw material ammonium paratungstate;
an agitator tank 200 for preparing a dilute ammonium metatungstate solution;
an aging tank 300 for aging the dilute ammonium metatungstate solution;
a filtering device 400 for filtering the aged dilute ammonium metatungstate solution;
the reaction kettle 500 is internally provided with a heating device and is used for heating and concentrating the filtered dilute ammonium metatungstate solution to prepare a concentrated ammonium metatungstate solution;
and a spray drying apparatus 600 for drying the concentrated ammonium metatungstate solution.
As a preferred embodiment of the present invention, it may also have the following additional technical features:
The stirring tank 200 comprises a tank body, a stirring device is arranged in the tank body, the wall part of the tank body is of a double-shell structure and comprises an outer shell 201 and an inner shell 202, a heating cavity is formed between the outer shell 201 and the inner shell 202, specifically, the heating cavity can be heated by injecting steam, and heating elements can be additionally arranged in the heating cavity for heating.
The stirring device comprises a stirring shaft and a driving device 205 used for driving the stirring shaft to rotate, wherein a plurality of layers of stirring blades 203 are arranged on the stirring shaft, a flow disturbing hole 204 is arranged on each stirring blade 203, and the flow disturbing hole 204 can be one or more combinations of a circle, a triangle and a rectangle.
The preparation system of this embodiment adopts spray drying equipment to dry, and the product purity of making is high, carries out multistage filtration simultaneously, and product purity is high for it is high in subsequent technology solubility, sets up on agitator tank 200's stirring leaf 203 and disturbs the orifice 204, and the stirring is more even, makes its reaction efficiency higher.
The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.
In the description of the embodiments of the present invention, it should be understood that "-" and "-" indicate the same range of two numerical values, and the range includes the end points. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing the associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter related objects are in an "or" relationship.
The above is only the preferred embodiment of the present invention, as long as the technical solution of the purpose of the present invention is realized by the substantially same means, all belong to the protection scope of the present invention.
Claims (4)
1. The utility model provides a preparation system of high solubility ammonium metatungstate which characterized in that is provided with according to the preface along the direction of feed:
a rotary kiln (100) for activating the ammonium paratungstate as a raw material;
an agitator tank (200) for preparing a dilute ammonium metatungstate solution;
an aging tank (300) for aging the dilute ammonium metatungstate solution;
the filtering device (400) is used for filtering the aged dilute ammonium metatungstate solution;
the reaction kettle (500) is internally provided with a heating device and is used for heating and concentrating the filtered dilute ammonium metatungstate solution to prepare a concentrated ammonium metatungstate solution;
and the spray drying equipment (600) is used for drying the concentrated ammonium metatungstate solution.
2. The system for preparing ammonium metatungstate with high solubility according to claim 1, wherein the filtering device (400) comprises a first coarse filtering device (401), a second coarse filtering device (402) and a nanofiltration device (403), two stages of filter cloth are arranged in the first coarse filtering device (401), four stages of filter cloth are arranged in the second coarse filtering device (402), and a high molecular nanofiltration membrane is arranged in the nanofiltration device (403).
3. The system for preparing the high-solubility ammonium metatungstate according to claim 1, wherein the stirring tank (200) comprises a tank body, a stirring device is arranged in the tank body, the wall part of the tank body is of a double-shell structure and comprises an outer shell (201) and an inner shell (202), and a heating cavity is formed between the outer shell (201) and the inner shell (202).
4. The system for preparing high-solubility ammonium metatungstate according to claim 3, wherein the stirring device comprises a stirring shaft and a driving device (205) for driving the stirring shaft to rotate, the stirring shaft is provided with a plurality of layers of stirring blades (203), and the stirring blades (203) are provided with turbulent flow holes (204).
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| CN112079388A (en) * | 2020-09-23 | 2020-12-15 | 江西铜鼓有色冶金化工有限责任公司 | Preparation method and system of high-solubility ammonium metatungstate |
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