CN110129549A - A kind of useless tungsten processing method and processing unit - Google Patents
A kind of useless tungsten processing method and processing unit Download PDFInfo
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- CN110129549A CN110129549A CN201910454910.XA CN201910454910A CN110129549A CN 110129549 A CN110129549 A CN 110129549A CN 201910454910 A CN201910454910 A CN 201910454910A CN 110129549 A CN110129549 A CN 110129549A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention belongs to tungsten recycling and reusing fields of giving up, and disclose a kind of useless tungsten processing method and processing unit.The useless tungsten processing method the following steps are included: S1, by useless tungsten carry out nitre melting reaction, obtain crude sodium tungstate solution；S2, the crude sodium tungstate solution is mixed with desiliconizing agent, and gained mixed liquor is subjected to high-temperature high-voltage reaction in the case where temperature is not less than 100 DEG C, it is separated by solid-liquid separation, high-purity sodium tungstate solution and silicon slag precipitating are obtained, the dosage of the desiliconizing agent and the condition of high-temperature high-voltage reaction make SiO in the high-purity sodium tungstate solution of gained2Concentration is down to 100mg/L or less.Method provided by the invention enables to the sodium metasilicate entered in sodium tungstate solution during nitre melting reaction to precipitate, to which the element silicon in sodium tungstate solution be effectively removed, except silicon rate can achieve 95% or more, high-quality tungsten product production requirement can satisfy.In addition, method provided by the invention is easy to operate, input cost is low, is suitble to industrialized production.
Description
Technical field
The invention belongs to tungsten recycling and reusing fields of giving up, and are related to a kind of useless tungsten processing method and processing unit.
Background technique
Tungsten is important strategic resource, is known as " industrial tooth ".With the increasingly exploitation of tungsten ore, tungsten ore resource reserves day
Benefit reduction, tungsten secondary resource recycling are particularly important.Currently, although a large amount of scientific research technical staff is for tungsten secondary resource
Recycling and reusing is done a lot of work, but since tungsten waste material complicated component multiplicity, the existence of tungsten are difficult to determine, processing is difficult
Degree is big.
The main method of existing useless tungsten recycling includes that mechanical crushing method, zinc melt method, lixiviation process, electrochemical process etc., but this
A little methods still have the type variation that technology is not perfect, industrial application difficulty is big, can not be well adapted for various tungsten waste materials
Defect, and the tungsten product purity produced is low, is unable to satisfy the requirement of high-quality tungsten product.In addition, useless tungsten was recycling
Ground plate in journey etc. can adulterate a large amount of silica, and the silicone content of the useless tungsten raw material now used increasingly increases, and content is up to 2
~20wt% is differed.The silicon removing process of present is all so that silicon is generated precipitating removal by way of adjusting pH value, but adopt
It on the one hand needs to consume a large amount of chemical reagent to existing alkaline sodium tungstate solution with this method, is on the other hand not suitable for existing alkali
Method process flow.
Summary of the invention
The present invention is intended to provide a kind of new useless tungsten processing method and processing unit.
As described above, silicone content increasingly increases in the useless tungsten raw material now used, SiO2Content be up to 2~20wt% not
Deng.For the useless tungsten of this part high silicon content, if handled using nitre smelting technology, give up dioxy contained in tungsten
SiClx can generate sodium metasilicate in conjunction with sodium salt and enter in sodium tungstate solution, thus cause element silicon in sodium tungstate solution exceeded, nothing
Method meets the requirement of high-quality tungsten product.Nitre smelting technology is dexterously carried out high-temperature high-voltage reaction with desiliconizing agent is added by the present invention
Silicon removing process combines, and can effectively remove the element silicon in sodium tungstate solution obtained by nitre smelting technology in this way, except silicon rate is high,
Final gained sodium tungstate solution can satisfy high-quality tungsten product production requirement.Based on this, the present invention is completed.
Specifically, the first aspect of the present invention provides a kind of useless tungsten processing method, the mass content of tungsten in the useless tungsten
For 40~95%, SiO2Mass content be 2~20%, wherein method includes the following steps:
S1, the useless tungsten is subjected to nitre melting reaction, obtains crude sodium tungstate solution；
S2, the crude sodium tungstate solution is mixed with desiliconizing agent, and gained mixed liquor is not less than 100 DEG C in temperature
Lower carry out high-temperature high-voltage reaction, then gained reaction product is separated by solid-liquid separation, high-purity sodium tungstate solution and silicon slag precipitating are obtained,
The dosage of the desiliconizing agent and the condition of high-temperature high-voltage reaction make SiO in the high-purity sodium tungstate solution of gained2Concentration is down to
100mg/L or less.
Further, the condition of the nitre melting reaction makes WO in the crude sodium tungstate solution of gained3Concentration be 50~
250g/L, SiO2Concentration be 200~5000mg/L.
Further, during the nitre melting reaction used by useless tungsten and nitre weight ratio be (0.5~
1.25):1。
Further, the temperature of the nitre melting reaction is 700~1000 DEG C, and the time is 2~8h.
Further, the desiliconizing agent is sodium aluminate and/or aluminium oxide.
Further, the amount ratio of the crude sodium tungstate solution and desiliconizing agent is 8.5m3: (3~85) kg, preferably
8.5m3: (15~50) kg.
Further, the condition of the high-temperature high-voltage reaction include temperature be 100~220 DEG C, pressure be 0.1~
1.8MPa, time are 1~5h.
Further, it is 150~180 DEG C that the condition of the high-temperature high-voltage reaction, which includes temperature, and pressure is 0.5~1MPa,
Time is 2~3h.
The second aspect of the present invention provides a kind of useless tungsten processing unit, wherein the useless tungsten processing unit includes successively
Nitre smelting equipment, surge tank, high-temperature high-voltage reaction equipment and the solid-liquid separating equipment of connection.
Further, the useless tungsten processing unit further includes dust collection device, and the dust collection device is set with the nitre melting
Standby top connection.
Further, the useless tungsten processing unit further includes the first dnockout pumps, blow tank, the second dnockout pumps and dense hopper,
First dnockout pumps are arranged between the surge tank and high-temperature high-voltage reaction equipment, the blow tank and the second dnockout pumps edge
Flow of Goods and Materials direction be successively set between the high-temperature high-voltage reaction equipment and solid-liquid separating equipment, the dense hopper and institute
State the liquid-phase outlet connection of solid-liquid separating equipment.
Method provided by the invention enables to the sodium metasilicate entered in sodium tungstate solution during nitre melting reaction
It precipitates, so that the element silicon in sodium tungstate solution be effectively removed, except silicon rate can achieve 95% or more, can satisfy height
Quality tungsten product production requirement.In addition, method provided by the invention is easy to operate, input cost is low, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is a kind of connection schematic diagram of useless tungsten processing unit provided by the invention.
Description of symbols
1- nitre smelting equipment；2- surge tank；3- high-temperature high-voltage reaction equipment；4- solid-liquid separating equipment；5- dust collection device；
The first dnockout pumps of 6-；7- blow tank；The second dnockout pumps of 8-；The dense hopper of 9-.
Specific embodiment
The present invention is described below in detail.
In the present invention, the mass content of tungsten is 40~95%, SiO in the useless tungsten2Mass content be 2~20%.
Wherein, in the useless tungsten mass content of tungsten with WO3Meter.
In the present invention, the specific reaction process of the nitre melting reaction can be same as the prior art.Specifically, will
Useless tungsten and nitre are placed in smelting furnace, and after temperature reaches nitre fusion temperature, melting nitre just can be sent out with useless tungsten raw material
Raw reaction, the sodium tungstate melt of melting pour into the blow tank for filling water, after after being separated by solid-liquid separation acquired solution be crude tungsten
Acid sodium solution.Wherein, the condition of the nitre melting reaction preferably makes WO in the crude sodium tungstate solution of gained3Concentration be 50~
250g/L, SiO2Concentration be 200~5000mg/L.Specifically, during the nitre melting reaction used by useless tungsten and
The weight ratio of nitre is preferably (0.5~1.25): 1.The temperature of the nitre melting reaction is preferably 700~1000 DEG C, the time
Preferably 2~8h.
In the present invention, the desiliconizing agent is particularly preferably sodium aluminate and/or aluminium oxide.The dosage of the desiliconizing agent should
Depending on the content of silicon in crude sodium tungstate solution, the content of silicon in the high-purity sodium tungstate solution of final gained is reduced enough to
Low level is (by SiO2Concentration is down to 100mg/L or less) subject to.Specifically, the use of the crude sodium tungstate solution and desiliconizing agent
Amount is than being preferably 8.5m3: (3~85) kg, more preferably 8.5m3: (15~50) kg.
In the present invention, the temperature of the high-temperature high-voltage reaction, which should control, is being not less than 100 DEG C, so can be by nitre
Sodium metasilicate caused by during stone melting reaction effectively removes.Specifically, the condition of the high-temperature high-voltage reaction includes temperature
Preferably 100~220 DEG C, more preferably 150~180 DEG C, pressure is preferably 0.1~1.8MPa, is more preferably 0.5~1MPa,
Time is preferably 1~5h, more preferably 2~3h.In the present invention, the pressure refers both to gauge pressure.
As shown in Figure 1, useless tungsten processing unit provided by the invention includes nitre smelting equipment 1, the surge tank being sequentially communicated
2, high-temperature high-voltage reaction equipment 3 and solid-liquid separating equipment 4.Wherein, the nitre smelting equipment 1 is used to carry out nitre to useless tungsten molten
Refining reaction.The surge tank 2 is for mixing the resulting crude sodium tungstate solution of nitre melting reaction with desiliconizing agent.It is described
High-temperature high-voltage reaction equipment 3 is used to carry out high-temperature high-voltage reaction to the mixed material for being originated from surge tank 2 to remove silicon therein.
The solid-liquid separating equipment 4 is for being separated by solid-liquid separation the resulting reaction product of high-temperature high-voltage reaction, to obtain high-purity wolframic acid
Sodium solution and silicon slag precipitating.
The useless tungsten processing unit further preferably includes dust collection device 5, the dust collection device 5 and the nitre smelting equipment 1
Top connection, for recycling the dust generated in nitre smelting equipment 1.
The useless tungsten processing unit can also include the first dnockout pumps 6, blow tank 7, the second dnockout pumps 8 and dense hopper 9, institute
It states the first dnockout pumps 6 to be arranged between the surge tank 2 and high-temperature high-voltage reaction equipment 3, the blow tank 7 and the second dnockout pumps
8 are successively set between the high-temperature high-voltage reaction equipment 3 and solid-liquid separating equipment 4 along Flow of Goods and Materials direction, the dense material
Slot 9 is connected to the liquid-phase outlet of the solid-liquid separating equipment 4.Wherein, first dnockout pumps 6 and the second dnockout pumps 8 are used to
Material is transmitted.The blow tank 7 is for caching high-temperature high-voltage reaction product.The dense hopper 9 is used for most
Resulting high-purity sodium tungstate solution is cached eventually.
The nitre smelting equipment 1, surge tank 2, high-temperature high-voltage reaction equipment 3, solid-liquid separating equipment 4, dust collection device 5,
First dnockout pumps 6, blow tank 7, the second dnockout pumps 8 and dense hopper 9 various can realize above functions to be existing respectively
Equipment, its specific structure is not particularly limited, this those skilled in the art can be known, therefore not to repeat here.
In most preferred embodiment of the invention, as shown in Figure 1, the useless tungsten processing unit includes the nitre being sequentially communicated
Stone smelting equipment 1, surge tank 2, the first dnockout pumps 6, high-temperature high-voltage reaction equipment 3, blow tank 7, the second dnockout pumps 8 and solid-liquid point
From equipment 4, the dust collection device 5 being connected to the top of the nitre smelting equipment 1, and the liquid with the solid-liquid separating equipment 4
The dense hopper 9 of phase outlet.At this point, corresponding useless tungsten processing method includes that useless tungsten is carried out nitre in nitre smelting equipment 1
Stone melting reaction, the dust that nitre melting reaction generates in the process are recycled by dust collection device 5, and nitre melting reaction product introduces
It is mixed in surge tank 2 with desiliconizing agent, gained mixed liquor introduces high-temperature high-voltage reaction under the action of the first dnockout pumps 6 and sets
High-temperature high-voltage reaction is carried out in standby 3, gained reaction product discharges to blow tank 7, and introduces admittedly under the action of the second dnockout pumps 8
It is separated by solid-liquid separation in liquid separation equipment 4, gained silicon slag precipitates outlet, and the high-purity sodium tungstate solution of gained discharges into dense hopper 9.
The present invention will be described in detail by way of examples below.
Embodiment 1
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 80%, SiO2Mass content be 10%) at 700 DEG C into
The weight ratio of row nitre melting reaction 8h, useless tungsten and nitre is controlled in 0.5:1, obtains WO3Concentration be 150g/L and SiO2It is dense
Degree is the crude sodium tungstate solution 8.5m of 1000mg/L3。
S2, sodium aluminate 25kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 2h under conditions of temperature is 150 DEG C, pressure is 0.5MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 142g/L, SiO2Concentration be 48mg/L.
Embodiment 2
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 40%, SiO2Mass content be 4%) at 800 DEG C into
The weight ratio of row nitre melting reaction 6h, useless tungsten and nitre is controlled in 0.75:1, obtains WO3Concentration be 50g/L and SiO2It is dense
Degree is the crude sodium tungstate solution 8.5m of 200mg/L3。
S2, sodium aluminate 25kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 3h under conditions of temperature is 120 DEG C, pressure is 0.3MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 45g/L, SiO2Concentration be 10mg/L.
Embodiment 3
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 60%, SiO2Mass content be 20%) at 1000 DEG C
Nitre melting reaction 2h is carried out, the weight ratio control of useless tungsten and nitre obtains WO in 1.25:13Concentration be 250g/L and SiO2
Concentration be 5000mg/L crude sodium tungstate solution 8.5m3。
S2, sodium aluminate 85kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 2h under conditions of temperature is 200 DEG C, pressure is 1.8MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 238g/L, SiO2Concentration be 88mg/L.
Embodiment 4
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 60%, SiO2Mass content be 15%) at 900 DEG C into
The weight ratio of row nitre melting reaction 4h, useless tungsten and nitre is controlled in 1:1, obtains WO3Concentration be 200g/L and SiO2Concentration
For the crude sodium tungstate solution 8.5m of 3000mg/L3。
S2, aluminium oxide 40kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 4h under conditions of temperature is 180 DEG C, pressure is 1.6MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 188g/L, SiO2Concentration be 95mg/L.
Embodiment 5
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 95%, SiO2Mass content be 5%) at 850 DEG C into
The weight ratio of row nitre melting reaction 4h, useless tungsten and nitre is controlled in 0.9:1, obtains WO3Concentration be 180g/L and SiO2It is dense
Degree is the crude sodium tungstate solution 8.5m of 2500mg/L3。
S2, aluminium oxide 30kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 4h under conditions of temperature is 180 DEG C, pressure is 1.6MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 165g/L, SiO2Concentration be 98mg/L.
Embodiment 6
S1, by useless tungsten (with WO3The mass content of the tungsten of meter is 50%, SiO2Mass content be 3%) at 800 DEG C into
The weight ratio of row nitre melting reaction 6h, useless tungsten and nitre is controlled in 0.6:1, obtains WO3Concentration be 100g/L and SiO2It is dense
Degree is the crude sodium tungstate solution 8.5m of 1500mg/L3。
S2, sodium aluminate 25kg is added into the crude sodium tungstate solution that step S1 is obtained, through dnockout pumps disk after stirring evenly
Enter in high-temperature high-pressure reaction kettle (autoclave), reacts 2h under conditions of temperature is 150 DEG C, pressure is 0.5MPa.It is passed through after discharging
Filter press filters out silicon slag precipitating, obtains high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3's
Concentration is 95g/L, SiO2Concentration be 55mg/L.
Comparative example 1
Useless tungsten is handled according to the method for embodiment 1, unlike, the temperature of high-temperature high-voltage reaction is 80 DEG C of (pressures
Power varies with temperature), other conditions are constant, obtain high-purity sodium tungstate solution.Through analyzing, in the final high-purity sodium tungstate solution of gained
WO3Concentration be 140g/L, SiO2Concentration be 500mg/L.
Comparative example 2
Useless tungsten is handled according to the method for embodiment 2, unlike, the dosage of sodium aluminate is changed to 1kg, other conditions
It is constant, obtain high-purity sodium tungstate solution.Through analyzing, WO in the final high-purity sodium tungstate solution of gained3Concentration be 46g/L, SiO2's
Concentration is 150mg/L.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. a kind of useless tungsten processing method, the mass content of tungsten is 40~95%, SiO in the useless tungsten2Mass content be 2~
20%, which is characterized in that method includes the following steps:
S1, the useless tungsten is subjected to nitre melting reaction, obtains crude sodium tungstate solution；
S2, the crude sodium tungstate solution is mixed with desiliconizing agent, and by gained mixed liquor temperature not less than at 100 DEG C into
Row high-temperature high-voltage reaction, then gained reaction product is separated by solid-liquid separation, high-purity sodium tungstate solution and silicon slag precipitating are obtained, it is described
The dosage of desiliconizing agent and the condition of high-temperature high-voltage reaction make SiO in the high-purity sodium tungstate solution of gained2Concentration be down to 100mg/L with
Under.
2. useless tungsten processing method according to claim 1, which is characterized in that the condition of the nitre melting reaction makes gained
WO in crude sodium tungstate solution3Concentration be 50~250g/L, SiO2Concentration be 200~5000mg/L.
3. useless tungsten processing method according to claim 2, which is characterized in that employed in the nitre melting reaction process
Useless tungsten and nitre weight ratio be (0.5~1.25): 1.
4. useless tungsten processing method according to claim 2, which is characterized in that the temperature of the nitre melting reaction is 700
~1000 DEG C, the time is 2~8h.
5. useless tungsten processing method described according to claim 1~any one of 4, which is characterized in that the desiliconizing agent is aluminium
Sour sodium and/or aluminium oxide.
6. useless tungsten processing method described according to claim 1~any one of 4, which is characterized in that the crude sodium tungstate
The amount ratio of solution and desiliconizing agent is 8.5m3: (3~85) kg, preferably 8.5m3: (15~50) kg.
7. useless tungsten processing method described according to claim 1~any one of 4, which is characterized in that the high temperature high pressure reverse
The condition answered includes that temperature is 100~220 DEG C, and pressure is 0.1~1.8MPa, and the time is 1~5h；Preferably, the high temperature is high
The condition of pressure reaction includes that temperature is 150~180 DEG C, and pressure is 0.5~1MPa, and the time is 2~3h.
8. a kind of useless tungsten processing unit, which is characterized in that the useless tungsten processing unit include the nitre smelting equipment being sequentially communicated,
Surge tank, high-temperature high-voltage reaction equipment and solid-liquid separating equipment.
9. useless tungsten processing unit according to claim 8, which is characterized in that the useless tungsten processing unit further includes gathering dust to set
Standby, the dust collection device is connected to the top of the nitre smelting equipment.
10. useless tungsten processing unit according to claim 8 or claim 9, which is characterized in that the useless tungsten processing unit further includes
One dnockout pumps, blow tank, the second dnockout pumps and dense hopper, first dnockout pumps are arranged in the surge tank and high temperature high pressure reverse
It answers between equipment, the blow tank and the second dnockout pumps are successively set on the high-temperature high-voltage reaction along Flow of Goods and Materials direction and set
It is standby between solid-liquid separating equipment, the dense hopper is connected to the liquid-phase outlet of the solid-liquid separating equipment.
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| CN110484740A (en) * | 2019-09-29 | 2019-11-22 | 株洲市炎陵县华南冶金科技有限公司 | A kind of open hearth used from the method and this method of tungsten tin copper-lead waste residue recycling tantalum niobium |
| CN110484740B (en) * | 2019-09-29 | 2021-04-27 | 株洲市炎陵县华南冶金科技有限公司 | Method for recovering tantalum and niobium from tungsten-tin-copper-lead waste residues and open hearth furnace used by method |
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