Treatment method of ammonium paratungstate sieve head material

Abstract

The invention discloses a treatment method of an ammonium paratungstate sieve head material. The treatment method comprises the following steps: S1, preparing a solution; step S2, dissolving; s3, filtering and washing; step S4, drying and screening; according to the process disclosed by the invention, the ammonium paratungstate sieve head material is adjusted and treated, the consumption of auxiliary materials is reduced, the energy consumption is low, and the open crystal appearance of the original ammonium paratungstate crystal is kept; compared with the original undersize ammonium paratungstate product, the ammonium paratungstate product recovered and treated by the method has the advantages that the impurity element content is lower, the total impurity content is 20-30ppm lower than that before treatment, and the product quality is integrally improved.

Description

Technical Field

[0001] The present invention belongs to the technical field of tungsten smelting, and specifically relates to a method for treating ammonium paratungstate screen head material. Background Art

[0002] Ammonium paratungstate is an important intermediate product in the production of tungsten metal powder. Crystallizing ammonium paratungstate from ammonium tungstate solution is one of the important processes in the entire tungsten smelting. In the existing tungsten smelting process, more than 95% of the ammonium paratungstate products are prepared by evaporation crystallization. The wet ammonium paratungstate obtained by evaporation crystallization of ammonium tungstate solution needs to be dried and screened to obtain qualified ammonium paratungstate products. During the drying process, whether it is steam drying or microwave drying, factors such as excessive moisture in the wet ammonium paratungstate and uneven heating during the drying process can cause ammonium paratungstate to easily agglomerate during the drying process. After drying, the ammonium paratungstate is screened to obtain oversize materials (ammonium paratungstate screen head materials) and undersize materials (qualified ammonium paratungstate products).

[0003] Currently, most tungsten smelting and processing enterprises have two methods for treating screen head materials. One method is to grind the screen head materials by mechanical crushing and then mix them into qualified ammonium paratungstate products. Mechanical crushing destroys the crystal form and morphology of ammonium paratungstate, and may also introduce pollutants during the crushing process. At the same time, a large amount of dust is generated during the crushing process, resulting in the loss of ammonium paratungstate. Another method is to dissolve the screen head materials in concentrated ammonia water under elevated temperature and pressure to form ammonium tungstate solution, and then evaporate and crystallize the ammonium tungstate solution to prepare ammonium paratungstate products. This method requires pressure vessels, consumes ammonia water and steam, and at the same time, crystallization waste gas and crystallization mother liquor are generated during the crystallization process, increasing the treatment of waste water and waste steam. This method has a long process and high treatment cost.

[0004] Based on this, the present invention provides a method for treating ammonium paratungstate screen head material. Summary of the Invention

[0005] In view of the above situation, in order to overcome the defects of the prior art, the present invention provides a method for treating ammonium paratungstate screen head material, which effectively solves the problems raised in the background art.

[0006] To achieve the above object, the present invention provides the following technical solution: A method for treating ammonium paratungstate screen head material, comprising the following steps:

[0007] Step S1, solution preparation: Add pure water to the reaction kettle, and then supplement ammonium salt to prepare a dilute ammonium salt solution with a concentration of 0.2 - 0.8%.

[0008] Step S2, dissolution: Start the stirring of the reaction kettle, add ammonium paratungstate screen head material to the reaction kettle, and heat it by introducing jacket steam. Control the solution temperature within 50°C and stir for 1 - 2 hours.

[0009] Step S3, filtration and washing: Put the mixed material liquid in the reaction kettle in Step S2 into a suction filter tray, and vacuum filter it to obtain mother liquor and wet ammonium paratungstate 1. The wet ammonium paratungstate 1 is then washed 1-2 times with pure water having a conductivity less than 15 μS / cm, and the washing water is vacuumed off to obtain wet ammonium paratungstate 2; the mother liquor and the washing water are returned to Step S1;

[0010] Step S4, drying and screening: The wet ammonium paratungstate obtained in Step S3 is dried and screened to obtain a qualified ammonium paratungstate product

[0011] Preferably, in Step S1, pure water and ammonium salt are added to the reaction kettle, and the concentration of the ammonium salt solution is controlled to be 0.3-0.5%, wherein the ammonium salt is one of ammonium chloride or ammonium nitrate.

[0012] Preferably, in Step S2, ammonium paratungstate screen head material is added to the reaction kettle, steam is introduced to raise the temperature, and the jacket heating method is adopted, and the temperature of the reaction kettle solution is controlled at 30-45°C.

[0013] Preferably, in Step S3, the wet ammonium paratungstate 1 is further washed with pure water having a conductivity less than 15 μS / cm, and the pure water has a conductivity less than 10 μS / cm.

[0014] Preferably, in Step S3, the mixed material liquid in the reaction kettle is put into a suction filter tray, the solution is vacuum filtered, and the negative pressure of the vacuum filtration is 0.02-0.05 mpa.

[0015] Compared with the prior art, the beneficial effects of the present invention are:

[0016] 1. The present invention adjusts the process to treat the ammonium paratungstate screen head material, reduces the consumption of auxiliary materials, has low energy consumption, and maintains the original crystal morphology of ammonium paratungstate;

[0017] 2. The ammonium paratungstate product recovered and treated by this method has lower impurity elements than the original undersize ammonium paratungstate product, and the total amount of impurities is 20-30 ppm lower than that before treatment, and the overall product quality is improved. Description of the Drawings

[0018] The drawings are used to provide a further understanding of the present invention, and constitute a part of the specification, and are used to explain the present invention together with the embodiments of the present invention, and do not constitute a limitation to the present invention.

[0019] In the drawings:

[0020] Figure 1 is a schematic flow chart of a method for treating ammonium paratungstate screen head material of the present invention; Detailed Embodiments

[0021] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0022] Given by Figure 1 The present invention relates to a method for treating ammonium paratungstate screen head material, including the following steps:

[0023] Step S1, solution preparation: Add pure water to the reaction kettle, and then supplement ammonium salt to prepare a dilute ammonium salt solution with a concentration of 0.2-0.8%.

[0024] Step S2, dissolution: Start the stirring of the reaction kettle, add ammonium paratungstate screen head material to the reaction kettle, and introduce jacket steam to raise the temperature. The solution temperature is controlled within 50°C, and stir for 1-2 hours.

[0025] Step S3, filtration and washing: Put the mixed material liquid in the reaction kettle in step S2 into the suction filter tray, and vacuum filter it to obtain mother liquor and wet ammonium paratungstate 1. Wet ammonium paratungstate 1 is then washed 1-2 times with pure water with a conductivity less than 15 μS / cm, and the washing water is vacuumed off to obtain wet ammonium paratungstate 2; the mother liquor and washing water are returned to step S1.

[0026] Step S4, drying and screening: The wet ammonium paratungstate obtained in step S3 is dried and screened to obtain qualified ammonium paratungstate products.

[0027] In step S1 of this embodiment, pure water and ammonium salt are added to the reaction kettle, and the concentration of the prepared ammonium salt solution is controlled at 0.3-0.5%. Among them, the ammonium salt is one of ammonium chloride or ammonium nitrate.

[0028] In step S2 of this embodiment, ammonium paratungstate screen head material is added to the reaction kettle, steam is introduced to raise the temperature, and the jacket heating method is adopted. The solution temperature in the reaction kettle is controlled at 30-45°C.

[0029] In step S3 of this embodiment, wet ammonium paratungstate 1 is further washed with pure water with a conductivity less than 15 μS / cm, and the pure water has a conductivity less than 10 μS / cm.

[0030] In step S3 of this embodiment, the mixed material liquid in the reaction kettle is put into the suction filter tray, and the solution is vacuum filtered. The negative pressure of the vacuum filtration is 0.02-0.05 mpa.

[0031] Example 1:

[0032] Add 4 m of pure water to the reaction kettle 3, then add ammonium salt to make a 0.3% ammonium salt solution; start the stirring of the reaction kettle, add 1.5 tons of ammonium paratungstate sieve head material to the reaction kettle, introduce steam to raise the temperature to 35°C, and stir for 1.5 hours; put the mixed material liquid in the reaction kettle into the suction filter plate, vacuum filter it to obtain mother liquor and wet ammonium paratungstate, then wash the wet ammonium paratungstate with pure water once, and vacuum pump out the washing water to obtain wet ammonium paratungstate. Dry the wet ammonium paratungstate and screen it to obtain 1.496 tons of qualified ammonium paratungstate products.

[0033] Example 2:

[0034] Add 4m of pure water to the reaction kettle 3 , then add ammonium salt to make a 0.5% ammonium salt solution; start the stirring of the reaction kettle, add 1.6 tons of ammonium paratungstate sieve head material to the reaction kettle, introduce steam to raise the temperature to 33°C, and stir for 1.5 hours; put the mixed material liquid in the reaction kettle into the suction filter plate, vacuum filter it to obtain mother liquor and wet ammonium paratungstate, then wash the wet ammonium paratungstate with pure water once, and vacuum pump out the washing water to obtain wet ammonium paratungstate; dry the wet ammonium paratungstate and screen it to obtain 1.595 tons of qualified ammonium paratungstate products.

[0035] Example 3:

[0036] Add 3m of pure water to the reaction kettle 3 , then add ammonium salt to make a 0.4% ammonium salt solution; start the stirring of the reaction kettle, add 1.1 tons of ammonium paratungstate sieve head material to the reaction kettle, introduce steam to raise the temperature to 40°C, and stir for 1.5 hours; put the mixed material liquid in the reaction kettle into the suction filter plate, vacuum filter it to obtain mother liquor and wet ammonium paratungstate, then wash the wet ammonium paratungstate with pure water once, and vacuum pump out the washing water to obtain wet ammonium paratungstate. Dry the wet ammonium paratungstate and screen it to obtain 1.097 tons of qualified ammonium paratungstate products.

[0037] It should be noted that in this article, relational terms such as first and second are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any actual relationship or order between these entities or operations. Moreover, the term "comprising", "including" or any other variant thereof is intended to cover non-exclusive inclusion, so that a process, method, article or device comprising a series of elements not only includes those elements, but also includes other elements not expressly listed, or also includes elements inherent to such process, method, article or device.

[0038] Although the embodiments of the present invention have been shown and described, for those of ordinary skill in the art, it can be understood that various changes, modifications, substitutions and variations can be made to these embodiments without departing from the principles and spirit of the present invention. The scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A method for treating ammonium paratungstate screen head material, comprising the following steps: Step S1, solution preparation: Add pure water to the reaction kettle, and then supplement ammonium salt to prepare a dilute ammonium salt solution with a concentration of 0.2-0.8%; Step S2, dissolution: Start stirring the reaction kettle, add ammonium paratungstate screen head material to the reaction kettle, and introduce jacket steam to raise the temperature. The solution temperature is controlled within 50 °C, and stir for 1-2 hours; Step S3, filtration and washing: Put the mixed solution in the reaction kettle in Step S2 into a suction filter plate, and vacuum filter it to obtain mother liquor and wet ammonium paratungstate 1. Wet ammonium paratungstate 1 is then washed 1-2 times with pure water with a conductivity less than 15 μS / cm, and the washing water is vacuumed off to obtain wet ammonium paratungstate 2; The mother liquor and washing water are returned to Step S1; Step S4, drying and screening: The wet ammonium paratungstate obtained in Step S3 is dried and screened to obtain qualified ammonium paratungstate products.

2. The processing method of ammonium paratungstate screen head material according to claim 1, characterized in that: In Step S1, when adding pure water and ammonium salt to the reaction kettle, the concentration of the prepared ammonium salt solution is controlled at 0.3-0.5%, and the ammonium salt is one of ammonium chloride or ammonium nitrate.

3. The treatment method of ammonium paratungstate screen head material according to claim 2, characterized in that: In Step S2, when adding ammonium paratungstate screen head material to the reaction kettle and introducing steam to raise the temperature, the jacket heating method is adopted, and the solution temperature in the reaction kettle is controlled at 30-45 °C.

4. The processing method of ammonium paratungstate screen head material according to claim 1, characterized in that: In Step S3, wet ammonium paratungstate 1 is washed with pure water with a conductivity less than 15 μS / cm, and the pure water has a conductivity less than 10 μS / cm.

5. The treatment method of ammonium paratungstate screen head material according to claim 1, characterized in that: In Step S3, the mixed solution in the reaction kettle is put into a suction filter plate, and the solution is vacuum filtered. The negative pressure of the vacuum filtration is 0.02-0.05 mpa.

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