CN112877539A - Tungsten-molybdenum separation method - Google Patents
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Abstract
The invention discloses a tungsten-molybdenum separation method, which comprises the following steps: s1, carrying out primary evaporative crystallization on the feed liquid containing tungsten and molybdenum, and filtering for the first time to obtain primary mother liquid and primary crystallization ammonium paratungstate; s2, carrying out secondary evaporation crystallization on the primary mother liquor, and carrying out secondary filtration to obtain secondary mother liquor and secondary crystallization ammonium paratungstate; s3, carrying out tungsten and molybdenum separation on the secondary mother liquor obtained in the step S2; s4, calcining the secondary crystal ammonium paratungstate obtained in the step S2 into yellow tungsten, and adding at least a part of the yellow tungsten into the feed liquid in the step S1; s5, calcining the primary crystalline ammonium paratungstate obtained after adding the yellow tungsten obtained in the step S4 in the step S1 into yellow tungsten, and dissolving the obtained yellow tungsten into concentrated ammonia water to obtain ammonia solution secondary liquid. According to the tungsten-molybdenum separation method, by adopting a mode of twice evaporative crystallization, the tungsten-molybdenum ratio in the high-molybdenum ammonium paratungstate of evaporative crystallization is improved, the ratio of molybdenum entering a subsequent molybdenum removal system is reduced, and the subsequent molybdenum removal cost is reduced.
Description
Technical Field
The invention relates to the technical field of tungsten and molybdenum separation, in particular to a tungsten and molybdenum separation method.
Background
The tungsten and the tungsten product have the advantages of high melting point, high density, high hardness, low thermal expansion coefficient, excellent corrosion resistance, good processability and the like, and can be applied to the technical fields of cutters, lamps, medicines and the like. Because of the reduction of tungsten ore and the reduction of grade, the secondary recovery of tungsten resources is more and more emphasized.
The molybdenum and the molybdenum alloy have high-temperature strength and high-temperature hardness, low thermal expansion coefficient, good processing performance and the like, and can be applied to the technical fields of biological medicines, mechanical processing and the like. Due to the over-exploitation of molybdenum ore, the production capacity is excessive, and the recovery of secondary resources of molybdenum becomes more important.
The problem of deep separation of tungsten and molybdenum in the whole tungsten smelting process always exists. Since the ionic radius of molybdenum is very close to that of tungsten. Because the ion radiuses are similar, the complexing ability of the tungsten and the molybdenum is similar, and the separation of the two elements of the tungsten and the molybdenum is difficult.
The evaporation, crystallization and separation of tungsten and molybdenum are the core processes of the high molybdenum process. How to improve the tungsten-molybdenum ratio of evaporative crystallization high-molybdenum APT (ammonium paratungstate) and reduce molybdenum entering a subsequent molybdenum removal system as much as possible is a key index for measuring the separation effect of tungsten and molybdenum.
In the existing evaporation process in production, high-molybdenum second-stage liquid (the tungsten-molybdenum ratio is about 10) is evaporated and crystallized once until the tungsten-molybdenum ratio in mother liquid is about 1, so that the tungsten-molybdenum ratio in the obtained APT is about 80, the molybdenum content is high, and the subsequent molybdenum removal cost is increased.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a tungsten-molybdenum separation method, which can effectively improve the tungsten-molybdenum ratio in the evaporated and crystallized high-molybdenum ammonium paratungstate, reduce the ratio of molybdenum entering a subsequent molybdenum removal system and reduce the cost of subsequent molybdenum removal.
The tungsten-molybdenum separation method provided by the embodiment of the invention comprises the following steps: s1, carrying out primary evaporative crystallization on the feed liquid containing tungsten and molybdenum, and filtering for the first time to obtain primary mother liquid and primary crystallization ammonium paratungstate; s2, carrying out secondary evaporation crystallization on the primary mother liquor, and carrying out secondary filtration to obtain secondary mother liquor and secondary crystallization ammonium paratungstate; s3, carrying out tungsten and molybdenum separation on the secondary mother liquor obtained in the step S2; s4, after the secondary crystal ammonium paratungstate obtained in the step S2 is calcined into yellow tungsten, adding at least a part of yellow tungsten into the feed liquid in the step S1, and repeating the step S1; s5, calcining the primary crystalline ammonium paratungstate obtained after adding the yellow tungsten obtained in the step S4 in the step S1 into yellow tungsten, and dissolving the obtained yellow tungsten into concentrated ammonia water to obtain ammonia solution secondary liquid.
According to the tungsten-molybdenum separation method provided by the embodiment of the invention, through adopting twice evaporative crystallization and returning the secondary crystallization ammonium paratungstate obtained by the twice evaporative crystallization to the once evaporative crystallization, the purposes of improving the tungsten-molybdenum ratio in the ammonium paratungstate, reducing the molybdenum content in the ammonia solution, reducing the production and processing cost of the subsequent procedures and the like can be achieved.
The tungsten-molybdenum separation method according to the embodiment of the invention can also have the following additional technical characteristics:
according to one embodiment of the invention, the tungsten-molybdenum ratio of the feed liquid is 9-10, and WO is contained in the primary mother liquid32-3 of/Mo, wherein WO in the primary crystal ammonium paratungstate3The ratio of Mo to WO is more than or equal to 100, and the secondary mother liquid contains WO30.8-1% of/Mo, wherein WO in the secondary crystallization of ammonium paratungstate3/Mo≤60。
According to an embodiment of the present invention, in step S1, the vapor pressure of the primary evaporative crystallization is 0.1MPa to 0.5MPa, and the vacuum negative pressure is 0.02MPa to 0.05 MPa.
According to an embodiment of the present invention, in step S1, the volume of the mother liquid is controlled to be 0.4 to 0.6 of the total volume.
According to an embodiment of the invention, in step S2, the pressure of the vapor in the secondary evaporation crystallization condition is 0.1MPa to 0.5MPa, and the vacuum negative pressure is 0.02MPa to 0.05 MPa.
According to one embodiment of the present invention, the volume of the mother liquor is controlled to 0.5 to 0.7 of the total volume in step S2.
According to an embodiment of the invention, in the step S4, the solid-liquid mass ratio of the yellow tungsten and the feed liquid returned to the step S1 is 1 (40-85).
According to one embodiment of the invention, in step S5, the concentrated ammonia water is 110 g/L-130 g/L.
According to one embodiment of the invention, in step S5, the solid-liquid mass ratio between the yellow tungsten and the concentrated ammonia water is (2.5-3): 1.
According to an embodiment of the present invention, in step S3, the secondary mother liquor is subjected to ion exchange for tungsten-molybdenum separation.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The above and/or additional aspects and advantages of the present invention will become apparent and readily appreciated from the following description of the embodiments, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a flow diagram of a tungsten molybdenum separation process according to one embodiment of the invention;
fig. 2 is a flow diagram of a tungsten molybdenum separation method according to yet another embodiment of the invention.
Detailed Description
Embodiments of the present invention will be described in detail below, the embodiments described with reference to the drawings being illustrative, and the embodiments of the present invention will be described in detail below.
A tungsten-molybdenum separation method according to an embodiment of the present invention will be described with reference to fig. 1 and 2.
First, as shown in fig. 1, a tungsten-molybdenum separation method according to an embodiment of the present invention includes the steps of:
and S1, carrying out primary evaporative crystallization on the feed liquid containing tungsten and molybdenum, and filtering for the first time to obtain primary mother liquid and primary crystallization ammonium paratungstate. That is, a certain volume of feed liquid containing tungsten and molybdenum is subjected to primary evaporative crystallization, and then primary filtration is performed, so that primary mother liquid and primary crystalline ammonium paratungstate can be obtained through the primary filtration.
Optionally, the feed liquid is a high-molybdenum two-stage liquid, and the tungsten-molybdenum ratio in the feed liquid is approximately 9-10, that is, the tungsten-molybdenum separation method according to the application can be applied to feed liquids with larger tungsten-molybdenum ratio. It should be noted that, when the primary evaporation crystallization is performed, the tungsten crystallization rate is much higher than the molybdenum crystallization rate, and the tungsten-molybdenum ratio in the obtained primary crystalline ammonium paratungstate is relatively high.
Optionally, during the primary evaporative crystallization, the steam pressure can be 0.1MPa to 0.5MPa, and the vacuum negative pressure can be 0.02MPa to 0.05MPa, and by adopting the steam pressure and the vacuum negative pressure within the above numerical range, the primary evaporative crystallization is facilitated, the rate and the evaporation effect of the primary evaporative crystallization can be improved, and the time required by the primary evaporative crystallization is shortened.
Optionally, in step S1, the volume of the mother liquor is controlled to be 0.4-0.6 of the total volume. That is to say, when once evaporation crystallization, can be according to liquid level change control terminal liquid level, final mother liquor volume control is 0.4 ~ 0.6 of total volume.
For convenience of description, the primary evaporative crystallization of the present application will be described below with reference to examples.
For example, the step of primary evaporative crystallization includes: (1) carrying out primary evaporative crystallization on a feed liquid with a certain volume of tungsten-molybdenum ratio of about 9-10, wherein the steam pressure of the primary evaporative crystallization is 0.1-0.5 MPa, and the vacuum pressure is 0.02-0.05 MPa (negative pressure); (2) controlling the end point liquid level according to the liquid level change, and finally controlling the volume of the mother liquor to be 0.4-0.6 of the total volume; (3) WO in primary mother liquor obtained after primary filtration32-3 of/Mo, WO in primary crystallization of ammonium paratungstate3/Mo≥100。
And S2, carrying out secondary evaporation crystallization on the primary mother liquor obtained in the step S1, and carrying out secondary filtration to obtain secondary mother liquor and secondary crystallization ammonium paratungstate. Compared with the primary evaporation crystallization, the concentration of tungsten and molybdenum in the mother liquor of the secondary evaporation crystallization is increased, the crystallization rate of molybdenum is increased, and the tungsten and molybdenum in the obtained secondary crystallization ammonium paratungstate are lower.
Optionally, during secondary evaporation crystallization, the steam pressure is 0.1 MPa-0.5 MPa, and the vacuum negative pressure is 0.02 MPa-0.05 MPa. During secondary evaporation crystallization, steam pressure and vacuum negative pressure in the numerical range are adopted, secondary evaporation crystallization is facilitated, the rate and the evaporation effect of secondary evaporation crystallization can be improved, and the time required by secondary evaporation crystallization is shortened. In addition, the steam pressure range adopted by the primary evaporation crystallization and the secondary evaporation crystallization is the same, and the vacuum negative pressure range is the same, so that the method has the advantages of convenience in operation, simplification of required equipment and the like.
Optionally, in step S2, the volume of the mother liquor is controlled to be 0.5 to 0.7 of the total volume. That is to say, during the secondary evaporation crystallization, the end liquid level can be controlled according to the liquid level change, and the final mother liquor volume is controlled to be 0.5-0.7 of the total volume.
For convenience of description, the secondary evaporative crystallization of the present application will be described below with reference to examples.
For example, the steps of primary evaporative crystallization and secondary evaporative crystallization include: (1) carrying out primary evaporative crystallization on a feed liquid with a certain volume of tungsten-molybdenum ratio of about 9-10, wherein the steam pressure of the primary evaporative crystallization is 0.1-0.5 MPa, and the vacuum pressure is 0.02-0.05 MPa (negative pressure); (2) controlling the end point liquid level according to the liquid level change, and finally controlling the volume of the mother liquor to be 0.4-0.6 of the total volume; (3) WO in primary mother liquor obtained after primary filtration32-3 of/Mo, WO in primary crystallization of ammonium paratungstate3The ratio of Mo to Mo is more than or equal to 100; (4) carrying out secondary evaporation crystallization on the primary mother liquor, wherein the steam pressure is 0.1-0.5 MPa, and the vacuum pressure is 0.02-0.05 MPa (negative pressure); (5) controlling the end point liquid level according to the liquid level change, and finally controlling the volume of the mother liquor to be 0.5-0.7 of the total volume; (6) after secondary filtration, the obtained secondary mother liquor is WO30.8-1% of/Mo, and WO in secondary crystallization of ammonium paratungstate3/Mo≤60。
S3, performing tungsten and molybdenum separation on the secondary mother liquor obtained in the step S2.
Optionally, in step S3, the secondary mother liquor is ion exchanged to perform tungsten-molybdenum separation.
S4, calcining the secondary crystal ammonium paratungstate obtained in the step S2 into yellow tungsten, adding at least a part of yellow tungsten into the feed liquid in the step S1 for matching, and carrying out primary evaporation crystallization treatment. It should be noted that the addition of a certain amount of seed crystals during the evaporation process facilitates the growth of the crystal grains. And the secondary evaporation crystallization is carried out to obtain secondary crystal ammonium paratungstate, the secondary crystal ammonium paratungstate is calcined into yellow tungsten, and the yellow tungsten is matched and returned to the primary evaporation crystallization, so that the tungsten-molybdenum ratio in the finally obtained Ammonium Paratungstate (APT) is higher, for example, the tungsten-molybdenum ratio is more than 120.
Optionally, in the step S4, the solid-liquid mass ratio of the yellow tungsten and the feed liquid returned to the step S1 is 1 (40-85). When the solid-liquid mass ratio of the yellow tungsten to the feed liquid is too large, the tungsten-molybdenum ratio in the primary crystalline ammonium paratungstate is lowered, and the separation effect of the evaporated crystalline tungsten and molybdenum is affected. When the solid-liquid mass ratio of the yellow tungsten to the feed liquid is smaller, the influence on the separation of the evaporated and crystallized tungsten and molybdenum is smaller, but the normal production is influenced because the yellow tungsten calcined by the secondary crystallization ammonium paratungstate is not processed in time.
S5, calcining the primary crystalline ammonium paratungstate obtained after adding the yellow tungsten obtained in the step S4 in the step S1 into yellow tungsten, and dissolving the obtained yellow tungsten into concentrated ammonia water to obtain ammonia solution secondary liquid. It should be noted that, under the condition of higher crystallization rate, the precipitation rate of molybdenum is rapidly increased, because besides the formation of tungsten-molybdenum heteropoly acid, when the PH of the solution is reduced to about 7, molybdenum is converted from orthomolybdate ions to paramolybdate ions, and the paramolybdate ions and paratungstate ions enter the APT lattice in the form of homogeneous phase. And a certain amount of seed crystals are added in the evaporation process to be beneficial to the growth of crystal grains, and the adding process needs to consider the time for adding the seed crystals and the quality of the seed crystals.
Optionally, in the step S5, the concentration of the concentrated ammonia water is 110g/L to 130g/L, and the concentrated ammonia water in the range is favorable for preparing the ammonia solution secondary solution.
Optionally, in step S5, the solid-liquid mass ratio between the yellow tungsten and the concentrated ammonia water is (2.5-3):1, and WO in the obtained ammonia solution secondary solution3/Mo≥120。
For convenience of description, the tungsten-molybdenum separation method of the present application will be described below with reference to examples.
For example, as shown in fig. 2, the steps of the tungsten-molybdenum separation method include: (1) carrying out primary evaporative crystallization on a feed liquid with a certain volume of tungsten-molybdenum ratio of about 9-10, wherein the steam pressure of the primary evaporative crystallization is 0.1-0.5 MPa, and the vacuum pressure is 0.02-0.05 MPa (negative pressure); (2) controlling the end point liquid level according to the liquid level change, and finally controlling the volume of the mother liquor to be 0.4-0.6 of the total volume; (3) WO in primary mother liquor obtained after primary filtration32-3 of/Mo, WO in primary crystallization of ammonium paratungstate3The ratio of Mo to Mo is more than or equal to 100; (4) carrying out secondary evaporation crystallization on the primary mother liquor, wherein the steam pressure is 0.1-0.5 MPa, and the vacuum pressure is 0.02-0.05 MPa (negative pressure); (5) according to the liquid levelControlling the end point liquid level in a chemical control mode, and controlling the volume of the final mother liquor to be 0.5-0.7 of the total volume; (6) after secondary filtration, the obtained secondary mother liquor is WO30.8-1% of/Mo, and WO in secondary crystallization of ammonium paratungstate3Mo is less than or equal to 60; (7) calcining primary crystalline ammonium paratungstate obtained by primary evaporative crystallization of yellow tungsten added with secondary evaporative crystallization to prepare yellow tungsten, then dissolving the yellow tungsten with concentrated ammonia water with the concentration of 110-130 g/L, wherein the solid-liquid mass ratio between the yellow tungsten and the concentrated ammonia water is (2.5-3):1, and obtaining WO in ammonia solution secondary solution3/Mo≥120。
The tungsten-molybdenum separation method according to the embodiments of the present application will be described in detail with reference to specific examples.
Example 1:
(1) will be 7.5m3High molybdenum two-stage liquid (WO)3: 215.1g/L, Mo: 16.5g/L), carrying out primary evaporation crystallization, and carrying out primary filtration to obtain primary mother liquor and primary crystallization Ammonium Paratungstate (APT). In the process of primary evaporation crystallization, the steam pressure is 0.25MPa, the vacuum pressure is-0.025 MPa, and the evaporation liquid level reaches about 4m3The final mother liquor volume was 0.53 of the total volume. Filtering with filter, sampling, and analyzing to obtain WO in primary mother liquor3: 75.2g/L, Mo: 30.2g/L, and obtaining WO in the APT primary crystal after alkali dissolution3/Mo：145。
(2) And (3) carrying out secondary evaporation and crystallization on the primary mother liquor to obtain secondary mother liquor and secondary crystallization Ammonium Paratungstate (APT). Obtaining WO in secondary crystallization APT after alkali dissolution3Mo: 45, calcining the secondary crystallization APT, and then matching with 100kg of primary mother liquor (the solid-liquid mass ratio is 1:75) to the next batch for primary evaporation crystallization.
(3) Dissolving the obtained primary crystal APT in ammonia water with the concentration of 120g/L according to the solid-liquid mass ratio of 2.5:1, filtering after reaction to obtain ammonia solution secondary liquid, wherein WO is contained in the ammonia solution secondary liquid3The ratio/Mo was 125.
Example 2:
(1) will be 7.5m3High molybdenum two-stage liquid (WO)3: 210.1g/L, Mo: 12.5g/L), carrying out primary evaporation crystallization, and carrying out primary filtration to obtain primary mother liquor and primary crystallization Ammonium Paratungstate (APT). In one evaporation crystallizationIn the process, the steam pressure is 0.3MPa, the vacuum pressure is-0.03 MPa, and the evaporation is carried out until the end-point liquid level is about 3.8m3The final mother liquor volume was 0.51 of the total volume. Filtering with filter, sampling, and analyzing to obtain WO in primary mother liquor3: 65.2g/L, Mo: 25.1g/L, and obtaining WO in the primary crystal APT after alkali dissolution3/Mo：135。
(2) And (3) carrying out secondary evaporation and crystallization on the primary mother liquor to obtain secondary mother liquor and secondary crystallization Ammonium Paratungstate (APT). Obtaining WO in secondary crystallization APT after alkali dissolution3Mo: and 55, calcining the secondary crystallization APT, and then matching with 120kg of primary mother liquor (the solid-liquid mass ratio is 1:63) until the next batch of primary evaporation crystallization.
(3) Dissolving the obtained primary crystal APT in ammonia water with the concentration of 120g/L according to the solid-liquid mass ratio of 2.5:1, filtering after reaction to obtain ammonia solution secondary liquid, wherein WO is contained in the ammonia solution secondary liquid3The ratio/Mo was 120.
Example 3:
(1) will be 7.5m3High molybdenum two-stage liquid (WO)3: 209.1g/L, Mo: 11.5g/L), carrying out primary evaporation crystallization, and carrying out primary filtration to obtain primary mother liquor and primary crystallization Ammonium Paratungstate (APT). In the process of primary evaporation crystallization, the steam pressure is 0.28MPa, the vacuum pressure is-0.035 MPa, and the evaporation is carried out until the end liquid level is about 4.5m3The final mother liquor volume was 0.6 of the total volume. Filtering with filter, sampling, and analyzing to obtain WO in primary mother liquor3: 66.3g/L, Mo: 28.6g/L of WO in the APT primary crystal obtained after alkali dissolution3/Mo：130。
(2) Carrying out secondary evaporation crystallization on the primary mother liquor to obtain secondary mother liquor and secondary crystallization Ammonium Paratungstate (APT), and carrying out alkali dissolution to obtain WO in the secondary crystallization APT3Mo: 46, after the APT of the secondary crystallization is calcined, 90kg of primary mother liquor (the solid-liquid mass ratio is 1:83) is added to the next batch for primary evaporation crystallization.
(3) Dissolving the obtained primary crystal APT in ammonia water with the concentration of 120g/L according to the solid-liquid mass ratio of 2.5:1, filtering after reaction to obtain ammonia solution secondary liquid, wherein WO is contained in the ammonia solution secondary liquid3The ratio/Mo was 130.
Therefore, according to the tungsten-molybdenum separation method provided by the embodiment of the invention, during evaporation crystallization according to the characteristics of tungsten and molybdenum, evaporation crystallization is carried out in two times, the tungsten crystallization rate during the first evaporation crystallization is greatly higher than the molybdenum crystallization rate, the tungsten and molybdenum content in the obtained first-crystallization APT is higher, the tungsten and molybdenum concentration in the mother liquor during the second evaporation crystallization is increased, the molybdenum crystallization rate is increased, and the tungsten and molybdenum content in the obtained second-crystallization APT is lower. And calcining APT (ammonium paratungstate) obtained by secondary evaporation crystallization into yellow tungsten, and then returning to the primary evaporation crystallization in a matching manner, so that the tungsten-molybdenum ratio in the finally obtained ammonia solution secondary liquid can reach more than 120.
In summary, according to the method for separating tungsten and molybdenum of the embodiment of the invention, by adopting two times of evaporative crystallization and returning the secondary crystallization APT obtained by the secondary evaporative crystallization to the primary evaporative crystallization, the purposes of increasing the ratio of tungsten and molybdenum in the high-molybdenum APT, reducing the content of molybdenum in the ammonia solution, reducing the production and processing costs of the subsequent processes, and the like can be achieved.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an illustrative embodiment," "an example," "a specific example," or "some examples" or the like mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example.
While embodiments of the invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (10)
1. A tungsten-molybdenum separation method is characterized by comprising the following steps:
s1, carrying out primary evaporative crystallization on the feed liquid containing tungsten and molybdenum, and filtering for the first time to obtain primary mother liquid and primary crystallization ammonium paratungstate;
s2, carrying out secondary evaporation crystallization on the primary mother liquor, and carrying out secondary filtration to obtain secondary mother liquor and secondary crystallization ammonium paratungstate;
s3, carrying out tungsten and molybdenum separation on the secondary mother liquor obtained in the step S2;
s4, after the secondary crystal ammonium paratungstate obtained in the step S2 is calcined into yellow tungsten, adding at least a part of yellow tungsten into the feed liquid in the step S1, and repeating the step S1;
s5, calcining the primary crystalline ammonium paratungstate obtained after adding the yellow tungsten obtained in the step S4 in the step S1 into yellow tungsten, and dissolving the obtained yellow tungsten into concentrated ammonia water to obtain ammonia solution secondary liquid.
2. The method according to claim 1, wherein the feed liquid has a tungsten-molybdenum ratio of 9-10, and WO is contained in the primary mother liquid32-3 of/Mo, wherein WO in the primary crystal ammonium paratungstate3The ratio of Mo to WO is more than or equal to 100, and the secondary mother liquid contains WO30.8-1% of/Mo, wherein WO in the secondary crystallization of ammonium paratungstate3/Mo≤60。
3. The method as claimed in claim 1, wherein in step S1, the pressure of vapor in the primary evaporation crystallization condition is 0.1 MPa-0.5 MPa, and the vacuum negative pressure is 0.02 MPa-0.05 MPa.
4. The method according to claim 1, wherein in step S1, the volume of the mother liquor is controlled to be 0.4-0.6 of the total volume.
5. The method as claimed in claim 1, wherein in step S2, the pressure of vapor in the secondary evaporation crystallization condition is 0.1 MPa-0.5 MPa, and the vacuum negative pressure is 0.02 MPa-0.05 MPa.
6. The method according to claim 1, wherein in step S2, the volume of the mother liquor is controlled to be 0.5-0.7 of the total volume.
7. The method according to claim 1, wherein in step S4, the solid-liquid mass ratio of the yellow tungsten and the feed liquid returned to step S1 is 1 (40-85).
8. The method of claim 1, wherein in step S5, the concentrated ammonia water is 110 g/L-130 g/L.
9. The method according to claim 8, wherein in step S5, the solid-liquid mass ratio between the yellow tungsten and the concentrated ammonia water is (2.5-3): 1.
10. The method of claim 1, wherein in step S3, the secondary mother liquor is ion exchanged for tungsten-molybdenum separation.
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| CN105858731A (en) * | 2016-05-20 | 2016-08-17 | 江钨高技术开发应用有限公司 | Method for directly preparing pyrochlore type tungsten oxide from ammonium tungstate solution |
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