CN104212972A - Method for manufacturing sodium tungstate from alkali leaching roasting miscellaneous slag charge - Google Patents
Method for manufacturing sodium tungstate from alkali leaching roasting miscellaneous slag charge Download PDFInfo
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- CN104212972A CN104212972A CN201410444869.5A CN201410444869A CN104212972A CN 104212972 A CN104212972 A CN 104212972A CN 201410444869 A CN201410444869 A CN 201410444869A CN 104212972 A CN104212972 A CN 104212972A
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Abstract
The invention belongs to the technical field of tungsten smelting, and particularly relates to a method for manufacturing sodium tungstate from alkali leaching roasting miscellaneous slag charge. In order to overcome the defects that the alkali leaching tungsten extraction recycling rate in an existing single wet process is low, the roasting cost of a single pyrogenic process is high, the dust is large, the production efficiency is low, and the processes are hard to operate and control, the method for manufacturing the sodium tungstate from the alkali leaching roasting miscellaneous slag charge comprises the following steps of A, breaking, B, alkali adding, C, grinding, D, primary filtering and washing, E, roasting, F cooling and fine grinding, G secondary filtering and washing, H, third-time filtering and washing and J, desorption. The method has the beneficial effects that (1) the wet process and the pyrogenic process are combined for use, the recycling rate of tungsten metal is improved, and meanwhile some mineral aggregate hard to decompose can be thoroughly processed; (2) driers are matched with alkali, water and liquid are mixed to enable the mineral aggregate and agents to fully react, and mixing is even; (3) wet feed enters a rotary kiln to be roasted, and dust generation is avoided; (4) scrubbing solutions are returned to grinding materials to be used, and the product quality of tungsten solutions can be improved.
Description
Technical field
The invention belongs to Tungsten smelting technical field, be specifically related to a kind of alkali leaching roasting slag charge of mixing and produce the method for sodium wolframate.
Background technology
At present, low tungstenic material slag extracts the production technique of tungsten metal, generally takes the methods such as alkali leaching, acid decomposition and pyrogenic process roasting removal of impurities to extract W elements, tungsten metal recovery is low often for these single production technique, cost is high, and environmental pollution is large, and manipulation difficulty is large.
Summary of the invention
(1) technical problem that will solve
In order to overcome the lixiviate of existing single wet method alkali, to get tungsten recovery rate low in the present invention, single pyrogenic process roasting cost is high, dust is large, the shortcomings such as production efficiency is low, the difficult manipulation of technique, it is high that the technical problem to be solved in the present invention is to provide a kind of yield, technical process is short, environmental pollution is little, and technology easily manipulates, the new technique that cost is low.
(2) technical scheme
In order to solve the problems of the technologies described above, the invention provides a kind of like this alkali leaching roasting slag charge of mixing and produce the method for sodium wolframate, its step is as follows:
A. broken:
The waste tungsten residue that APT is produced or the assorted material such as tungsten slurry and spent catalyst (spent catalyst is not broken), add step D washings, add buck again, crusher is used to carry out fragmentation, granularity reaches 0.2-0.5cm, and crusher is located in geosyncline, opening for feed and ground level, discharge port adopts open channel device, and broken slip enters band whipping appts and fully stirs in tank groove;
B. alkali is added:
The feed liquid of step A fragmentation is added soda ash by the 30-50% of real weight of material, adds step D filtrate simultaneously, make solid-to-liquid ratio reach 1:1.35, pH value, in 9-11 scopes, then fully stirs 1h with whipping appts at tank body;
C. abrasive material:
Feed liquid step B stirred is levigate to 220 order≤95% at ball mill by gravity flow, and slip enters the tank groove of band whipping appts, and solid-to-liquid ratio is 1:1.39, after fully stirring, to be filtered;
D. once filter, wash:
The feed liquid pressure filter of step C ball milling is carried out first time to filter and washing, filtrate returns step B abrasive material and uses, and washings returns steps A for fragmentation, and filter residue enters rotary kiln and carries out roasting;
E. roasting:
By the filter residue of D step filtration at rotary kiln baking, working temperature: 950 ~ 1100 DEG C, throughput; 16.5 ~ 20.2 t/h; Bank proportion: 2.0 t/m
3; Filling ratio: 7.6%; Rotary kiln rotating speed: 0.3 ~ 1.3 r/min, normal: 1.0 r/min, auxiliary: 0.1 r/min, roasting time is 1.5-2h;
F. cool levigate:
Cool after E step roasting material kiln discharge with G, H step washings, feed liquid mixing crusher or microspheric form grinding system are carried out levigate to-60 orders (that is: being less than 0.246mm) simultaneously, then in the tank body of whipping appts, fully stir 0.5h, then it is levigate to-320 Mu≤95% to enter second time ball milling;
G. secondary filtration, washing:
The feed liquid pressure filter of F step secondary ball milling is carried out second time to filter and washing, filtrate carries out ion-exchange, and washings returns step F for cooling roasting material, filter residue tap water material, treats to filter for three times;
H. filter for three times, wash:
Feed liquid pressure filter after G step filter residue material is carried out third time to filter, filtrate returns F step and uses for cooling roasting material, and filter residue is concentrated and stacked or arrange outward;
J. desorb:
Desorb is carried out in the ion-exchange of G step, the sodium tungstate solution desorbed, W content is at 260 ~ 320g/L, and pH value, 7-9 time, after adding hydrogen peroxide removal of impurities, send APT enterprise production and application.
Preferably, in step, use crusher to carry out fragmentation, granularity reaches 0.4cm; In stepb, make solid-to-liquid ratio reach 1:1.35, pH value 10, then fully stir 1h with whipping appts at tank body; In step e, working temperature: 1000 DEG C, throughput; 18.5t/h, rotary kiln rotating speed: 1r/min; In step J, the solution desorbed, W content, at 260g/L, when pH value is adjusted to 8.5, after adding hydrogen peroxide removal of impurities, is the sodium tungstate solution produced.
(3) beneficial effect
Invention achieves being combined of 1. wet method and pyrogenic process, improve the rate of recovery of tungsten metal.Can process more thorough to some difficult mineral aggregates decomposed simultaneously.2. alkali joined by siccative, and the mixing of water liquid makes mineral aggregate and medicament sufficient reacting, mixes.3. wet feed enters rotary kiln baking, avoids dust and produces.4. washings returns abrasive material use, improves the quality product of tungsten solution.5. the worn-out open type of filter residue directly enter rotary kiln, avoid screw feeder, the drawback such as difficult feed, fed material from being blocked that belt conveying type feed, garden traditional feed-type such as dish feed etc. cause.6. cool in time with washings after roasting kiln discharge, slag tungsten metal is decomposed rapidly.7. filter residue carries out filtering for three times, washing, and last filtrate carries out ion-exchange, and valuable metal obtains high recovery.
Accompanying drawing explanation
Fig. 1 is flow chart of steps of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is further illustrated.
embodiment 1
The method of sodium wolframate produced by alkali leaching roasting slag charge of mixing, and flow chart of steps is shown in Fig. 1, and its step is as follows:
A. broken: the waste tungsten residue produce APT or 5 tons, the assorted material such as tungsten slurry and spent catalyst (spent catalyst is not broken), add step D washings, then add buck 4.5 tons, use crusher to carry out fragmentation, granularity reaches 0.2cm.Crusher is located in geosyncline, opening for feed and ground level, and discharge port adopts open channel device, and broken slip enters band whipping appts and fully stirs in tank groove.
B. add alkali: the feed liquid of step A fragmentation is added soda ash 1.5 tons, add step D filtrate 0.5 ton with inch, make solid-to-liquid ratio reach 1:1.35, pH value 9, then fully stir 1h with whipping appts at tank body.
C. abrasive material: feed liquid step B stirred is levigate to 220 order≤95% at ball mill by gravity flow, and slip enters the tank groove of band whipping appts, and solid-to-liquid ratio is 1:1.39, after fully stirring, to be filtered.
D. once filter, wash: the feed liquid pressure filter of step C ball milling is carried out first time and filter and washing, filtrate returns step B abrasive material and uses, and washings returns steps A for fragmentation, and filter residue enters rotary kiln and carries out roasting.
E. roasting: by the filter residue of D step filtration at rotary kiln baking, working temperature: 950 DEG C, throughput; 16.5t/h; Bank proportion: 2.0t/m
3; Filling ratio: 7.6%; Rotary kiln rotating speed: 0.3r/min is normal: 1.0r/min, auxiliary: 0.1r/min; , roasting time is 1.5h.
F. cool levigate: cool after E step roasting material kiln discharge with G, H step washings, feed liquid mixing crusher or microspheric form grinding system are carried out levigate to-60 orders simultaneously.Then in the tank body of whipping appts, fully stir 0.5h, then it is levigate to-320 Mu≤95% to enter secondary ball milling.
G. secondary filtration, washing: the feed liquid pressure filter of F step secondary ball milling is carried out second time and filter and washing, filtrate carries out ion-exchange, and washings returns step F for cooling roasting material, filter residue tap water material, treats to filter for three times.
H. filter for three times, wash: the feed liquid pressure filter after G step filter residue material is carried out third time and filter, filtrate returns F step and uses for cooling roasting material, and filter residue is concentrated and stacked or arrange outward, and filter residue W content is below 0.5%.
J. desorb: desorb is carried out in the ion-exchange of G step, the solution desorbed, W content, at 260g/L, when pH value is adjusted to 7, after adding hydrogen peroxide removal of impurities, is the sodium tungstate solution produced, and send APT enterprise production and application.
embodiment 2
The method of sodium wolframate produced by alkali leaching roasting slag charge of mixing, and flow chart of steps is shown in Fig. 1, and its step is as follows:
A. broken: the waste tungsten residue produce APT or 5 tons, the assorted material such as tungsten slurry and spent catalyst (spent catalyst is not broken), add step D washings, then add buck 5.5 tons, use crusher to carry out fragmentation, granularity reaches 0.35cm.Crusher is located in geosyncline, opening for feed and ground level, and discharge port adopts open channel device, and broken slip enters band whipping appts and fully stirs in tank groove.
B. add alkali: the feed liquid of step A fragmentation is added soda ash 2 tons, add step D filtrate 0.6 ton with inch, make solid-to-liquid ratio reach 1:1.35, pH value 10, then fully stir 1h with whipping appts at tank body.
C. abrasive material: feed liquid step B stirred is levigate to 220 order≤95% at ball mill by gravity flow, and slip enters the tank groove of band whipping appts, and solid-to-liquid ratio is 1:1.39, after fully stirring, to be filtered.
D. once filter, wash: the feed liquid pressure filter of step C ball milling is carried out first time and filter and washing, filtrate returns step B abrasive material and uses, and washings returns steps A for fragmentation, and filter residue enters rotary kiln and carries out roasting.
E. roasting: by the filter residue of D step filtration at rotary kiln baking, working temperature: 1050 DEG C, throughput; 18.5t/h; Bank proportion: 2.0t/m
3; Filling ratio: 7.6%; Rotary kiln rotating speed: 1r/min is normal: 1.0r/min, auxiliary: 0.1r/min; , roasting time is 1.7h.
F. cool levigate: cool after E step roasting material kiln discharge with G, H step washings, feed liquid mixing crusher or microspheric form grinding system are carried out levigate to-60 orders simultaneously.Then in the tank body of whipping appts, fully stir 0.5h, then it is levigate to-320 Mu≤95% to enter secondary ball milling.
G. secondary filtration, washing: the feed liquid pressure filter of F step secondary ball milling is carried out second time and filter and washing, filtrate carries out ion-exchange, and washings returns step F for cooling roasting material, filter residue tap water material, treats to filter for three times.
H. filter for three times, wash: the feed liquid pressure filter after G step filter residue material is carried out third time and filter, filtrate returns F step and uses for cooling roasting material, and filter residue is concentrated and stacked or arrange outward, and filter residue W content is below 0.42%.
J. desorb: desorb is carried out in the ion-exchange of G step, the solution desorbed, W content, at 290g/L, when pH value is adjusted to 8, after adding hydrogen peroxide removal of impurities, is the sodium tungstate solution produced, and send APT enterprise production and application.
embodiment 3
The method of sodium wolframate produced by alkali leaching roasting slag charge of mixing, and flow chart of steps is shown in Fig. 1, and its step is as follows:
A. broken: the waste tungsten residue produce APT or 5 tons, the assorted material such as tungsten slurry and spent catalyst (spent catalyst is not broken), add step D washings, then add buck 6.5 tons, use crusher to carry out fragmentation, granularity reaches 0.5cm.Crusher is located in geosyncline, opening for feed and ground level, and discharge port adopts open channel device, and broken slip enters band whipping appts and fully stirs in tank groove.
B. add alkali: the feed liquid of step A fragmentation is added soda ash 2.5 tons, add step D filtrate 0.8 ton with inch, make solid-to-liquid ratio reach 1:1.35, pH value 11, then fully stir 1h with whipping appts at tank body.
C. abrasive material: feed liquid step B stirred is levigate to 220 order≤95% at ball mill by gravity flow, and slip enters the tank groove of band whipping appts, and solid-to-liquid ratio is 1:1.39, after fully stirring, to be filtered.
D. once filter, wash:
The feed liquid pressure filter of step C ball milling is carried out first time to filter and washing, filtrate returns step B abrasive material and uses, and washings returns steps A for fragmentation, and filter residue enters rotary kiln and carries out roasting.
E. roasting: by the filter residue of D step filtration at rotary kiln baking, working temperature: 1100 DEG C, throughput; 20.2t/h; Bank proportion: 2.0t/m
3; Filling ratio: 7.6%; Rotary kiln rotating speed: 1.3 r/min is normal: 1.0r/min, auxiliary: 0.1r/min; , roasting time is 2h.
F. cool levigate: cool after E step roasting material kiln discharge with G, H step washings, feed liquid mixing crusher or microspheric form grinding system are carried out levigate to-60 orders simultaneously.Then in the tank body of whipping appts, fully stir 0.5h, then it is levigate to-320 Mu≤95% to enter secondary ball milling.
G. secondary filtration, washing: the feed liquid pressure filter of F step secondary ball milling is carried out second time and filter and washing, filtrate carries out ion-exchange, and washings returns step F for cooling roasting material, filter residue tap water material, treats to filter for three times.
H. filter for three times, wash: the feed liquid pressure filter after G step filter residue material is carried out third time and filter, filtrate returns F step and uses for cooling roasting material, and filter residue is concentrated and stacked or arrange outward, and filter residue W content is below 0.28%.
J. desorb: desorb is carried out in the ion-exchange of G step, the solution desorbed, W content, at 320g/L, during pH value 9, after adding hydrogen peroxide removal of impurities, is the sodium tungstate solution produced, and send APT enterprise production and application.
The above embodiment only have expressed the preferred embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion, improvement and substitute, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (2)
1. the method for sodium wolframate produced by alkali leaching roasting slag charge of mixing, and it is characterized in that, its step is as follows:
A. broken: the waste tungsten residue that APT is produced or the assorted material such as tungsten slurry and spent catalyst, add step D washings, add buck again, crusher is used to carry out fragmentation, granularity reaches 0.2-0.5cm, and crusher is located in geosyncline, opening for feed and ground level, discharge port adopts open channel device, and broken slip enters band whipping appts and fully stirs in tank groove;
B. add alkali: the feed liquid of step A fragmentation is added soda ash by the 30-50% of real weight of material, add step D filtrate simultaneously, make solid-to-liquid ratio reach 1:1.35, pH value, in 9-11 scopes, then fully stirs 1h with whipping appts at tank body;
C. abrasive material: feed liquid step B stirred is levigate to 220 order≤95% at ball mill by gravity flow, and slip enters the tank groove of band whipping appts, and solid-to-liquid ratio is 1:1.39, after fully stirring, to be filtered;
D. once filter, wash: the feed liquid pressure filter of step C ball milling is carried out first time and filter and washing, filtrate returns step B abrasive material and uses, and washings returns steps A for fragmentation, and filter residue enters rotary kiln and carries out roasting;
E. roasting: by the filter residue of D step filtration at rotary kiln baking, working temperature: 950 ~ 1100 DEG C, throughput; 16.5 ~ 20.2 t/h; Bank proportion: 2.0 t/m
3; Filling ratio: 7.6%; Rotary kiln rotating speed: 0.3 ~ 1.3 r/min, normal: 1.0 r/min, auxiliary: 0.1 r/min, roasting time is 1.5-2h;
F. cool levigate: cool after E step roasting material kiln discharge with G, H step washings, feed liquid mixing crusher or microspheric form grinding system are carried out levigate to-60 orders simultaneously, then in the tank body of whipping appts, fully stir 0.5h, then it is levigate to-320 Mu≤95% to enter second time ball milling;
G. secondary filtration, washing: the feed liquid pressure filter of F step secondary ball milling is carried out second time and filter and washing, filtrate carries out ion-exchange, and washings returns step F for cooling roasting material, filter residue tap water material, treats to filter for three times;
H. filter for three times, wash: the feed liquid pressure filter after G step filter residue material is carried out third time and filter, filtrate returns F step and uses for cooling roasting material, and filter residue is concentrated and stacked or arrange outward;
J. desorb: desorb is carried out in the ion-exchange of G step, the sodium tungstate solution desorbed, W content is at 260 ~ 320g/L, and pH value, 7-9 time, after adding hydrogen peroxide removal of impurities, send APT enterprise production and application.
2. the method for sodium wolframate produced by a kind of alkali leaching roasting according to claim 1 slag charge of mixing, and it is characterized in that, in step, use crusher to carry out fragmentation, granularity reaches 0.4cm; In stepb, make solid-to-liquid ratio reach 1:1.35, pH value 10, then fully stir 1h with whipping appts at tank body; In step e, working temperature: 1000 DEG C, throughput; 18.5t/h, rotary kiln rotating speed: 1r/min; In step J, the solution desorbed, W content, at 260g/L, when pH value is adjusted to 8.5, after adding hydrogen peroxide removal of impurities, is the sodium tungstate solution produced.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628037A (en) * | 2015-02-10 | 2015-05-20 | 江西稀有金属钨业控股集团有限公司 | Method for purifying sodium tungstate with high impurity-tungsten ratio |
| CN104878212A (en) * | 2015-04-30 | 2015-09-02 | 鹤庆北衙矿业有限公司 | Method and system for treating gold-containing slag |
-
2014
- 2014-09-03 CN CN201410444869.5A patent/CN104212972A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104628037A (en) * | 2015-02-10 | 2015-05-20 | 江西稀有金属钨业控股集团有限公司 | Method for purifying sodium tungstate with high impurity-tungsten ratio |
| CN104628037B (en) * | 2015-02-10 | 2016-08-24 | 江西稀有金属钨业控股集团有限公司 | A kind of method purifying high miscellaneous tungsten wolframic acid sodium |
| CN104878212A (en) * | 2015-04-30 | 2015-09-02 | 鹤庆北衙矿业有限公司 | Method and system for treating gold-containing slag |
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