CN103739016A - Method for treating crude ammonium tungstate solution - Google Patents
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Abstract
The invention discloses a method for treating a crude ammonium tungstate solution. The method comprises the steps of (1) washing activated carbon powder by utilizing dilute hydrochloric acid; (2) adding an ammonium sulfide solution, a copper sulfate solution and the washed activated carbon powder into the crude ammonium tungstate solution to carry out purification treatment on the crude ammonium tungstate solution; (3) filtering the purified crude ammonium tungstate solution to obtain filter residue containing the activated carbon powder and a pure ammonium tungstate solution; and (4) carrying out evaporation crystallization on the pure ammonium tungstate solution to obtain ammonium paratungstate. By utilizing the method, a lot of sedimentation time and filtering equipment can be saved, the treatment efficiency can be significantly improved, and the treatment cost can be reduced.
Description
Technical field
The invention belongs to chemical field, particularly, the present invention relates to a kind of method of processing thick ammonium tungstate solution.
Background technology
During tungsten is smelted, molybdenum is larger to the performance impact of subsequent product, and tungsten is the element of same subgroup, and character is comparatively similar, more difficult removing.In tungsten is smelted, how to remove molybdenum element is a more thorny and important problem always.
CN101177303A discloses a kind of method except molybdenum, arsenic, antimony, tin that precipitates from tungstate solution, by adding precipitation agent in the tungstate solution containing molybdenum, arsenic, antimony, tin after sulfuration, make the thiosalt of above-mentioned impurity all with it in conjunction with generating insoluble compound precipitation, tungsten compound is retained in solution, thereby obtains pure tungstate solution.The method not only removal of impurity is effective, product purity is high, tungsten loss is little, and can remove plurality of impurities, and flow process is short, equipment is simple, easy to implement, with low cost, but how the material that this patent does not have explanation to be precipitated out carries out filtration treatment, production practice discovery, this is also the problem that needs solve.
Therefore the method for, processing at present ammonium tungstate solution needs further research.
Summary of the invention
The present invention one of is intended to solve the problems of the technologies described above at least to a certain extent or at least provides a kind of useful business to select.For this reason, one object of the present invention is to propose a kind of method of with short production cycle, the thick ammonium tungstate solution of processing that reagent dosage is few and easy and simple to handle.
In one aspect of the invention, the present invention proposes a kind of method of processing thick ammonium tungstate solution, the method comprises: (1) utilizes dilute hydrochloric acid to wash activity charcoal powder; (2) in described thick ammonium tungstate solution, add ammonium sulfide solution, copper-bath and the described activity charcoal powder through washing, to described thick ammonium tungstate solution is carried out to purifying treatment; (3) the thick ammonium tungstate solution through described purifying treatment is filtered, to obtain filter residue and the pure tungsten acid ammonium solution containing activated carbon powder; And (4) carry out evaporative crystallization by described pure tungsten acid ammonium solution, to obtain ammonium paratungstate.According to embodiments of the invention, process the method for thick ammonium tungstate solution by activity charcoal powder is joined in the ammonium tungstate solution after removal of impurities, then directly filter, obtain the direct evaporative crystallization of filtrate and can obtain 0 grade of qualified APT.
In addition, the method for the thick ammonium tungstate solution of processing according to the above embodiment of the present invention can also have following additional technical characterictic:
In some embodiments of the invention, the concentration of described ammonium sulfide solution is that 80g/l(is with S
2+meter); The concentration of described copper-bath is 200g/l.Can remove thus the impurity such as molybdenum ion in thick ammonium tungstate solution.
In some embodiments of the invention, the mean particle size of described activated carbon powder is 46 microns.Thus, can significantly improve the absorption property of activated carbon powder.
In some embodiments of the invention, described thick ammonium tungstate solution based on 200ml, the add-on of described ammonium sulfide solution is 0.98ml, the add-on of described copper-bath is 0.12ml, the add-on of described activity charcoal powder after washing is 2～15g, wherein, in described thick ammonium tungstate solution, Mo ionic concn is 0.015g/l.Can effectively improve the purity of thick ammonium tungstate solution thus.
In some embodiments of the invention, the described thick ammonium tungstate solution based on 200ml, the add-on of described activity charcoal powder after washing is 8g.Can further improve the purity of thick ammonium tungstate solution thus, to improve the further filtration efficiency to thick ammonium tungstate solution.
In some embodiments of the invention, in step (2), after adding ammonium sulfide solution, copper-bath and described activity charcoal powder after washing in described thick ammonium tungstate solution, stir described thick ammonium tungstate solution 10～25 minutes.In some embodiments of the invention, stir described thick ammonium tungstate solution 20 minutes.Can improve the purity of thick ammonium tungstate solution thus, and further improve filtration efficiency, shorten the treatment time.
In some embodiments of the invention, the method further comprises: wash the described filter residue containing activated carbon powder (5), to obtain described regeneration activity carbon dust and remove molybdenum slag; And (6) are back to described regeneration activity carbon dust in step (1) and utilize described dilute hydrochloric acid to wash.Can further improve the utilization ratio of activity charcoal powder thus, save processing cost.
Additional aspect of the present invention and advantage in the following description part provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Accompanying drawing explanation
Above-mentioned and/or additional aspect of the present invention and advantage accompanying drawing below combination obviously and is easily understood becoming the description of embodiment, wherein:
Fig. 1 is the schema of the method for the thick ammonium tungstate solution of processing according to an embodiment of the invention.
Fig. 2 is the schema of the method for the thick ammonium tungstate solution of processing according to another embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of identical or similar functions from start to finish.Below by the embodiment being described with reference to the drawings, be exemplary, be intended to for explaining the present invention, and can not be interpreted as limitation of the present invention.
In the present invention, unless otherwise clearly defined and limited, the terms such as term " installation ", " being connected ", " connection ", " fixing " should be interpreted broadly, and for example, can be to be fixedly connected with, and can be also to removably connect, or connect integratedly; Can be mechanical connection, can be to be also electrically connected to; Can be to be directly connected, also can indirectly be connected by intermediary, can be the connection of two element internals.For the ordinary skill in the art, can understand as the case may be above-mentioned term concrete meaning in the present invention.
Existingly to the processing except liquid after molybdenum, all need to adopt certain precipitation time again it to be filtered, filtration process more complicated, first filters by flame filter press, then filters by accurate filter, finally also to, by filtering except molybdenum post, could obtain the ammonium tungstate feed liquid that purity is higher.Therefore, the existing treatment process precipitation time except liquid after molybdenum is longer, causes production efficiency low; Filter plant is too many, and production cost increases; Except the resin in molybdenum post, cannot regenerate, need at set intervals to change resin, cause a large amount of wastes; The amount of each ammonium sulfide adding and copper sulfate is too large, and production cost is higher.
For this reason, according to an aspect of the present invention, the present invention proposes a kind of method of processing thick ammonium tungstate solution.According to a particular embodiment of the invention, the method can specifically comprise:
(1) utilize dilute hydrochloric acid to wash activity charcoal powder;
(2) in thick ammonium tungstate solution, add copper-bath, ammonium sulfide solution and the activity charcoal powder through washing, to thick ammonium tungstate solution is carried out to purifying treatment;
(3) the thick ammonium tungstate solution through purifying treatment is filtered, to obtain filter residue and the pure tungsten acid ammonium solution containing activated carbon powder; And
(4) pure tungsten acid ammonium solution is carried out to evaporative crystallization, to obtain ammonium paratungstate.
Process according to an embodiment of the invention the method for thick ammonium tungstate solution by activity charcoal powder being joined in thick ammonium tungstate solution, can significantly improve thus the purity of the pure tungsten acid ammonium solution obtaining after further filtration efficiency and filtration, and then can significantly improve the purity of ammonium paratungstate, for example the pure tungsten acid ammonium solution of acquisition is carried out to direct evaporative crystallization and can obtain 0 grade of qualified APT.Therefore, utilize the method for the thick ammonium tungstate solution of processing of the above embodiment of the present invention to save a large amount of precipitation time and a large amount of filter plants, significantly improved filtration efficiency, reduced processing cost.
Below with reference to accompanying drawing 1, describe the method for the thick ammonium tungstate solution of processing of the above embodiment of the present invention in detail.
S100: activity charcoal powder pre-treatment
In certain embodiments, utilize dilute hydrochloric acid to wash activity charcoal powder.According to a particular embodiment of the invention, the mean particle size of the activated carbon powder that can adopt is also not particularly limited, and for example can adopt mean particle size is the activated carbon powder of 46 microns.Contriver finds, by adopting 5% dilute hydrochloric acid to wash activated carbon powder, can effectively remove the impurity such as salt of wormwood in activated carbon powder, further improves thus the absorption property of activated carbon powder.
S200: thick ammonium tungstate solution is carried out to purifying treatment
In certain embodiments, in thick ammonium tungstate solution, add ammonium sulfide solution, copper-bath and the above-mentioned activity charcoal powder through washing, to thick ammonium tungstate solution is carried out to purifying treatment.
According to a particular embodiment of the invention, to thick ammonium tungstate solution, add ammonium sulfide solution, copper-bath, wherein the concentration of ammonium sulfide solution is that 80g/l(is with S
2+meter); The concentration of copper-bath is 200g/l.Can effectively remove the impurity such as molybdenum ion in thick ammonium tungstate solution thus, and then improve the decontamination effect improving to thick ammonium tungstate solution.
According to a particular embodiment of the invention, thick ammonium tungstate solution based on 200ml, wherein in this solution, Mo ionic concn is 0.015g/l, the add-on of ammonium sulfide solution is 0.98ml, the add-on of copper-bath is 0.12ml, and the add-on of the activity charcoal powder after washing is 2～15g.By adding activated carbon powder, significantly improve the purity of thick ammonium tungstate solution thus, can significantly improve next step filtration efficiency thus.
Contriver also finds, the activated carbon powder adding can significantly improve the purity of thick ammonium tungstate solution, and then can reduce in right amount ammonium sulfide and copper sulfate reagent dosage, for example can on the basis of existing ammonium sulfide solution and copper-bath consumption, reduce the add-on of the copper-bath of 1%～5% copper-bath and 5%～20%, can reach equally and purify thick ammonium tungstate solution effect.Reduce copper sulfate consumption adding of activated carbon powder thus, and then can significantly reduce processing cost.
According to a particular embodiment of the invention, the above-mentioned thick ammonium tungstate solution based on 200ml, can add the activity charcoal powder 8g after washing.Can reach on the basis of decontamination index thus, save the cost of activity charcoal powder.
According to a particular embodiment of the invention, after adding ammonium sulfide solution, copper-bath and the activity charcoal powder after washing in thick ammonium tungstate solution, only need to stir thick ammonium tungstate solution 10～25 minutes, thick ammonium tungstate solution just reaches clarification, save thus long precipitation and processed, and then significantly improved the efficiency of processing thick ammonium tungstate solution.According to a particular embodiment of the invention, preferably stir and can filter for 20 minutes.Can further shorten the production cycle thus.
S300: filter
Further, the thick ammonium tungstate solution through purifying treatment is filtered, to obtain filter residue and the pure tungsten acid ammonium solution containing activated carbon powder.According to a particular embodiment of the invention, filtration can be to adopt any filtration unit, for example, can be flame filter press or suction filtration device, and then without accurate filter with except filter plants such as molybdenum posts.Utilize thus the method for the thick ammonium tungstate solution of processing of the present invention to reduce filter plant, and then can significantly simplify treatment process, reduce processing cost.And the thick ammonium tungstate solution that the method for utilizing the thick ammonium tungstate solution of processing of the above embodiment of the present invention is processed 200ml needs the time to be no more than 5 hours, compared with the thick ammonium tungstate solution method of conventional process, need significantly to have shortened above treatment cycle in 10 hours, improved processing efficiency.
S400: evaporative crystallization
Finally pure tungsten acid ammonium solution is carried out to evaporative crystallization, to obtain ammonium paratungstate.
According to a particular embodiment of the invention, the method for the thick ammonium tungstate solution of above-mentioned processing can further include: the filter residue containing activated carbon powder is washed, to obtain regeneration activity carbon dust and remove molybdenum slag; And regeneration activity carbon dust Returning utilization dilute hydrochloric acid is washed it.By obtaining, containing the filter residue of activated carbon powder, through washing, wait that process can regeneration thus, further reduced thus processing cost.
Compare with the method for the thick ammonium tungstate solution of existing processing, the method for the thick ammonium tungstate solution of processing of the above embodiment of the present invention also has following advantages:
1, to the ammonium tungstate feed liquid except after molybdenum, add the activity charcoal powder washing through dilute hydrochloric acid in ammonium tungstate solution, only need to stir 10-25 minute, shorten the production cycle;
2, can reduce ammonium sulfide and copper sulfate reagent dosage;
3, reduce and produce filter plant, without filtering except molybdenum post;
4, the filtration obtaining can regeneration through processing such as washings containing the slag of activity charcoal powder.Cost-saving.
Below with reference to specific embodiment, present invention is described, it should be noted that, these embodiment are only descriptive, and do not limit the present invention in any way.
Embodiment 1
Utilize dilute hydrochloric acid to wash activity charcoal powder, the activity charcoal powder physical properties after washing is in Table 1.
Table 1
| Activity charcoal powder granularity | Sub-blue decolouring (ml/0.1) | Iodine sorption value (mg/g) | PH value |
| 325 orders (46 microns) | 13 | 1104 | 10.5 |
With reference to figure 2, to the thick ammonium tungstate solution of 200ml, containing Mo concentration, be 0.015g/l, add ammonium sulfide solution (with S
2+meter, concentration is 80g/l) 0.98ml, copper-bath (200g/l) 0.12ml and the activity charcoal powder 8g through washing, stir 20 minutes, utilize suction filtration device to filter.Filtrate is carried out to evaporative crystallization, the pH=6.7 of terminal, detected result is in Table 2.
Table 2
| K | Na | P | S | Al | As | Bi | Ca | Cd | Co | Cr | Cu |
| 4 | 3 | <5 | <5 | <4 | <8 | <1 | <5 | <1 | <4 | <4 | 1 |
| Fe | Mg | Mn | Mo | Ni | Pb | Sb | Si | Sn | Ti | V | ? |
| <5 | <3 | <5 | 5 | <3 | <1 | <5 | <5 | <1 | <4 | <4 | ? |
Filter residue containing activated carbon powder is washed, obtain regeneration activity carbon dust and except molybdenum slag, utilize dilute hydrochloric acid to wash this partial regeneration activated carbon powder.Above-mentioned processing total time is for being no more than 5 hours.
As shown in Table 2, by aforesaid method, can process and obtain 0 grade of qualified ATP.
Embodiment 2
Utilize dilute hydrochloric acid to wash activity charcoal powder, the activity charcoal powder physical properties after washing is in Table 1.
With reference to figure 2, to the thick ammonium tungstate solution of 200ml, containing Mo concentration, be 0.015g/l, add ammonium sulfide solution (with S
2+meter, concentration is 80g/l) 0.98ml, copper-bath (200g/l) 0.12ml and the activity charcoal powder 15g through washing, stir 20 minutes, utilize suction filtration device to filter.Filtrate is carried out to evaporative crystallization, the pH=6.7 of terminal, detected result is in Table 3.
Table 3
| K | Na | P | S | Al | As | Bi | Ca | Cd | Co | Cr | Cu |
| 8 | 6 | <5 | <5 | <4 | <8 | <1 | <5 | <1 | <4 | <4 | 1 |
| Fe | Mg | Mn | Mo | Ni | Pb | Sb | Si | Sn | Ti | V | ? |
| <5 | <3 | <5 | 5 | <3 | <1 | <5 | <5 | <1 | <4 | <4 | ? |
Filter residue containing activated carbon powder is washed, obtain regeneration activity carbon dust and except molybdenum slag, utilize dilute hydrochloric acid to wash this partial regeneration activated carbon powder.Above-mentioned processing total time is for being no more than 5 hours.
As shown in Table 3, by aforesaid method, can process and obtain 0 grade of qualified ATP.
Comparative example 1
With reference to figure 2, to the thick ammonium tungstate solution of 200ml, containing Mo concentration, be 0.015g/l, add ammonium sulfide solution (with S
2+meter, concentration is 80g/l) 0.98ml, copper-bath (200g/l) 0.12ml and without the activity charcoal powder 8g of olefin(e) acid washing, stir 20 minutes, utilize suction filtration device to filter.Filtrate is carried out to evaporative crystallization, the pH=6.7 of terminal, detected result is in Table 4.
Table 4
| K | Na | P | S | Al | As | Bi | Ca | Cd | Co | Cr | Cu |
| 13 | 3 | 5 | 7 | <4 | <8 | <1 | 5 | <1 | <4 | <4 | 1 |
| Fe | Mg | Mn | Mo | Ni | Pb | Sb | Si | Sn | Ti | V | ? |
| <5 | <3 | <5 | 11 | <3 | <1 | <5 | <5 | <1 | <4 | <4 | ? |
Filter residue containing activated carbon powder is washed, obtain regeneration activity carbon dust and except molybdenum slag, utilize dilute hydrochloric acid to wash this partial regeneration activated carbon powder.Above-mentioned processing total time is for being no more than 5 hours.
As shown in Table 3, adopt the activated carbon powder do not pass through olefin(e) acid carrying out washing treatment, in the ammonium paratungstate obtaining after processing the content of impurity K, S, Mo apparently higher than in embodiment 1 through the foreign matter content of the activated carbon powder of olefin(e) acid washing.
Comparative example 2
Utilize dilute hydrochloric acid to wash activity charcoal powder, the activity charcoal powder physical properties after washing is in Table 1.
With reference to figure 2, to the thick ammonium tungstate solution of 200ml, containing Mo concentration, be 0.015g/l, add ammonium sulfide solution (with S
2+meter, concentration is 80g/l) 0.98ml, copper-bath (200g/l) 0.12ml and the activity charcoal powder 1g through washing, stir 30 minutes, utilize suction filtration device to filter.Filtrate is carried out to evaporative crystallization, the pH=6.7 of terminal, detected result is in Table 5.
Table 5
| K | Na | P | S | Al | As | Bi | Ca | Cd | Co | Cr | Cu |
| 5 | 4 | <5 | 7 | <4 | <8 | <1 | 10 | <1 | <4 | <4 | 6 |
| Fe | Mg | Mn | Mo | Ni | Pb | Sb | Si | Sn | Ti | V | ? |
| 5 | <3 | <5 | 8 | <3 | <1 | <5 | 7 | 1 | <4 | <4 | ? |
Filter residue containing activated carbon powder is washed, obtain regeneration activity carbon dust and except molybdenum slag, utilize dilute hydrochloric acid to wash this partial regeneration activated carbon powder.Above-mentioned processing total time is 5～6 hours.
As shown in Table 5, Cu and Mo foreign matter content are higher.
Comparative example 3
The concrete steps of the thick ammonium tungstate solution of conventional process are: first to the thick ammonium tungstate solution of 200ml, containing Mo concentration, be 0.015g/l, add ammonium sulfide solution (with S
2+meter, concentration is 80g/l) 1ml, stir revulcanization 3.5 hours 0.5 hour; Then add copper-bath (200g/l) 0.15ml, stir 0.5 hour, then precipitation 5.5 hours; By suction filtration device, filter, then filter by accurate filter, finally also will, by filtering except molybdenum post, could obtain the ammonium tungstate feed liquid that purity is higher.Although can obtain equally 0 grade of qualified APT, the reaching total time more than 10 hours of pure ammonium tungstate feed liquid from vulcanizing to obtaining.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means to be contained at least one embodiment of the present invention or example in conjunction with specific features, structure, material or the feature of this embodiment or example description.In this manual, the schematic statement of above-mentioned term is not necessarily referred to identical embodiment or example.And the specific features of description, structure, material or feature can be with suitable mode combinations in any one or more embodiment or example.
Although illustrated and described embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention in the situation that not departing from principle of the present invention and aim, modification, replacement and modification.
Claims (8)
1. process a method for thick ammonium tungstate solution, it is characterized in that, comprising:
(1) utilize dilute hydrochloric acid to wash activity charcoal powder;
(2) in described thick ammonium tungstate solution, add ammonium sulfide solution, copper-bath and the described activity charcoal powder through washing, to described thick ammonium tungstate solution is carried out to purifying treatment;
(3) the thick ammonium tungstate solution through described purifying treatment is filtered, to obtain filter residue and the pure tungsten acid ammonium solution containing activated carbon powder; And
(4) described pure tungsten acid ammonium solution is carried out to evaporative crystallization, to obtain ammonium paratungstate.
2. method according to claim 1, is characterized in that, the concentration of described ammonium sulfide solution is 80g/l; The concentration of described copper-bath is 200g/l.
3. method according to claim 1, is characterized in that, the mean particle size of described activated carbon powder is 46 microns.
4. method according to claim 1, it is characterized in that, described thick ammonium tungstate solution based on 200ml, the add-on of described ammonium sulfide solution is 0.98ml, the add-on of described copper-bath is 0.12ml, the add-on of described activity charcoal powder after washing is 2～15g, and wherein, in described thick ammonium tungstate solution, Mo ionic concn is 0.015g/l.
5. method according to claim 4, is characterized in that, the described thick ammonium tungstate solution based on 200ml, and the add-on of described activity charcoal powder after washing is 8g.
6. method according to claim 1, it is characterized in that, in step (2), after adding ammonium sulfide solution, copper-bath and described activity charcoal powder after washing in described thick ammonium tungstate solution, stir described thick ammonium tungstate solution 10～25 minutes.
7. method according to claim 6, is characterized in that, stirs described thick ammonium tungstate solution 20 minutes.
8. method according to claim 1, is characterized in that, further comprises:
(5) the described filter residue containing activated carbon powder is washed, to obtain described regeneration activity carbon dust and remove molybdenum slag; And
(6) described regeneration activity carbon dust is back in step (1) and utilizes described dilute hydrochloric acid to wash.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104386754A (en) * | 2014-10-09 | 2015-03-04 | 江西稀有金属钨业控股集团有限公司 | Technology for preparing ammonium tungstate solution |
| CN106044857A (en) * | 2016-08-02 | 2016-10-26 | 南昌航空大学 | Method for separating and purifying ammonium paratungstate from ammonium tungstate solution |
| CN109231275A (en) * | 2018-12-01 | 2019-01-18 | 湖南懋天世纪新材料有限公司 | The method that a kind of pair of ammonium tungstate solution carries out deeply removing vanadium |
| CN112301218A (en) * | 2020-09-02 | 2021-02-02 | 崇义章源钨业股份有限公司 | Method for separating molybdenum-containing precipitate in tungstate solution by adopting filtration-adsorption column |
| CN117566799A (en) * | 2024-01-15 | 2024-02-20 | 崇义章源钨业股份有限公司 | Method for preparing ammonium paratungstate |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104386754A (en) * | 2014-10-09 | 2015-03-04 | 江西稀有金属钨业控股集团有限公司 | Technology for preparing ammonium tungstate solution |
| CN106044857A (en) * | 2016-08-02 | 2016-10-26 | 南昌航空大学 | Method for separating and purifying ammonium paratungstate from ammonium tungstate solution |
| CN109231275A (en) * | 2018-12-01 | 2019-01-18 | 湖南懋天世纪新材料有限公司 | The method that a kind of pair of ammonium tungstate solution carries out deeply removing vanadium |
| CN112301218A (en) * | 2020-09-02 | 2021-02-02 | 崇义章源钨业股份有限公司 | Method for separating molybdenum-containing precipitate in tungstate solution by adopting filtration-adsorption column |
| CN117566799A (en) * | 2024-01-15 | 2024-02-20 | 崇义章源钨业股份有限公司 | Method for preparing ammonium paratungstate |
| CN117566799B (en) * | 2024-01-15 | 2024-03-15 | 崇义章源钨业股份有限公司 | Method for preparing ammonium paratungstate |
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Denomination of invention: Method for treating crude ammonium tungstate solution Effective date of registration: 20200317 Granted publication date: 20160629 Pledgee: Ganzhou branch of Jiujiang Bank Co., Ltd Pledgor: CHONGYI ZHANGYUAN TUNGSTEN Co.,Ltd. Registration number: Y2020360000013 |
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