CN103773965B - A kind of from containing the method reclaiming tantalum tantalum alloy waste material - Google Patents
A kind of from containing the method reclaiming tantalum tantalum alloy waste material Download PDFInfo
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- CN103773965B CN103773965B CN201410072987.8A CN201410072987A CN103773965B CN 103773965 B CN103773965 B CN 103773965B CN 201410072987 A CN201410072987 A CN 201410072987A CN 103773965 B CN103773965 B CN 103773965B
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- tantalum
- waste material
- alloy waste
- extraction
- liquor
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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
Abstract
The invention provides a kind of from containing the method reclaiming tantalum tantalum alloy waste material, comprise the following steps: one, adopt hydrofluoric acid to carry out leaching process to containing the tantalum in tantalum alloy waste material, obtain leach liquor; Two, adopt hexone to carry out extraction treatment to leach liquor, be extracted liquid; Three, sulfuric acid is adopted to carry out pickling impurity removal to extraction liquid; Four, adopt pure water to carry out back extraction process to the extraction liquid after removal of impurities, obtain strip liquor; Five, in strip liquor, drip ammoniacal liquor, obtain dirty solution; Six, dry after dirty solution being filtered, obtain tantalum hydroxide.The present invention is directed to containing dopant species in tantalum alloy raw material many, this characteristic of tantalum separation difficulty carries out R&D work, and propose a kind of from containing the novel method reclaiming tantalum tantalum waste material, the rate of recovery of tantalum is high, has good industrial prospect.
Description
Technical field
The invention belongs to technical field of wet metallurgy, being specifically related to a kind of from containing the method reclaiming tantalum tantalum alloy waste material.
Background technology
Tantalum belongs to high-melting-point, high boiling point rare metal, there is the characteristic such as high strength under air-breathing, supraconductivity, corrosion-resistant, one pole electroconductibility and high temperature, be widely used in the fields such as electronics, precision glass, Wimet, superconduction, aerospace, nuclear energy, biomedical engineering.China tantalum reserves are considerable, but grade is on the low side, and cost of winning is high, 2007, and China's tantalum ore annual production is respectively tantalum: 136t(amounts to into Ta
2o
5meter), far can not meet domestic smelting demand, and tantalum is important strategic reserves metal, its import is by about international situation, and containing a considerable number of tantalum in superalloy, 2006, China's superalloy annual production was about 5000 tons, and the annual high-temperature alloy waste material produced from relevant producers such as each aviation factories is also at thousands of tons of, therefore from high-temperature alloy waste material, Separation and Recovery tantalum has huge potentiality.
Compared to the recovery of tantalum in traditional ore, from the high-temperature alloy waste material containing tantalum element, carry out the recovery of tantalum, needed for it, separating impurity element is more, and Separation and Recovery difficulty is larger.Up to now, not yet find from containing the report carrying out the high efficiente callback of tantalum tantalum alloy waste material.
Summary of the invention
Technical problem to be solved by this invention is for the deficiencies in the prior art, provides a kind of from containing the method reclaiming tantalum tantalum alloy waste material.The method is for many containing dopant species in tantalum alloy waste material, and this characteristic of tantalum separation difficulty, propose a kind of from containing the novel method reclaiming tantalum tantalum waste material, the rate of recovery of tantalum is high, has good industrial prospect.
For solving the problems of the technologies described above, the technical solution used in the present invention is: a kind of from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the method comprises the following steps:
Step one, employing hydrofluoric acid are that leaching agent carries out leaching process to containing the tantalum in tantalum alloy waste material, obtain leach liquor; Described is 20% ~ 35% containing the mass percentage of tantalum in tantalum alloy waste material, and the described temperature leaching process is 70 DEG C ~ 90 DEG C, and the described time of leaching process is 1.5h ~ 2.5h, and the described solid-to-liquid ratio containing tantalum alloy waste material and hydrofluoric acid is 1: (6 ~ 9);
Step 2, employing hexone carry out extraction treatment for extraction agent to leach liquor described in step one, get upper organic phase, be extracted liquid after stratification; The volume ratio of described hexone and leach liquor is (3 ~ 5): 1;
Step 3, to be added in extraction liquid described in step 2 by sulfuric acid and carry out pickling impurity removal, the volume ratio of described sulfuric acid and extraction liquid is (3 ~ 5): 1, gets upper organic phase, obtain the extraction liquid after removal of impurities after stratification;
Step 4, employing pure water carry out back extraction process for reverse-extraction agent to the extraction liquid after removal of impurities described in step 3, take off a layer aqueous phase, obtain strip liquor after stratification; The volume ratio of the extraction liquid after described pure water and removal of impurities is (3 ~ 5): 1;
Step 5, in strip liquor described in step 4, drip ammoniacal liquor, be till 8 ~ 10 until the pH value of strip liquor, then have the strip liquor of ammoniacal liquor to stir dropping, obtain dirty solution;
Step 6, dirty solution described in step 5 to be filtered, then the solid trapped substance after filtering is placed in loft drier dry, after naturally cooling, obtains tantalum hydroxide.
Above-mentioned is a kind of from containing the method reclaiming tantalum tantalum alloy waste material, and it is characterized in that, the concentration of hydrofluoric acid described in step one is 8mol/L ~ 12mol/L.
Above-mentioned is a kind of from containing the method reclaiming tantalum tantalum alloy waste material, and it is characterized in that, the time of extraction treatment described in step 2 is 3min ~ 7min.
Above-mentioned is a kind of from containing the method reclaiming tantalum tantalum alloy waste material, and it is characterized in that, the concentration of sulfuric acid described in step 3 is 2mol/L ~ 6mol/L.
Above-mentioned is a kind of from containing the method reclaiming tantalum tantalum alloy waste material, and it is characterized in that, the time of the process of back extraction described in step 4 is 3min ~ 7min.
Above-mentioned is a kind of from containing the method reclaiming tantalum tantalum alloy waste material, and it is characterized in that, the mass percent concentration of ammoniacal liquor described in step 5 is 25% ~ 28%.
The present invention from containing the principle reclaiming tantalum tantalum alloy waste material is: first, and adopt hydrofluoric acid to carry out acid-soluble leaching to containing tantalum alloy waste material, under the condition that HF is suitably excessive, Ta is mainly with H
2taF
7form proceed in leach liquor, the impurity elements such as Ni, Co, Cr, Ti, Fe, W, Hf, Zr, Nb in alloyed scrap also proceed in leach liquor with fluorine complex ion form; Then, hexone (MIBK) is adopted to extract the leach liquor containing tantalum element and all kinds of impurity New Year's Day, Ta, Nb is made to proceed in upper organic phase, because the partition ratio of the impurity elements such as Ni, Co, Cr, Ti, Fe, W, Hf, Zr in MIBK is far smaller than the partition ratio of Ta, Nb, be therefore easy to divide out with Ta, Nb; Afterwards, by extraction after containing Ta organic phase through sulfuric acid washing removal of impurities, Nb can be separated, and adopt pure water to carry out the back extraction of tantalum, make Ta proceed to aqueous phase, finally adopt the method dripping ammoniacal liquor to carry out precipitation to the tantalum in strip liquor and obtain turbid solution, turbid solution obtains the throw out of tantalum after drying after filtration.Concrete reaction process is:
Hydrofluoric acid Leaching reaction:
NaTaO
3+8HF=H
2TaF
7+NaF+3H
2O
MIBK extractive reaction:
CH
3RCO+H
+=CH
3RCOH
+
2CH
3RCOH
++[TaF
7]
2-=[CH
3RCOH]
+ 2[TaF
7]
2-
Ammonia precipitation process reacts:
H
2TaF
7+7NH
3+5H
2O=Ta(OH)
5↓+7NH
4F
The present invention compared with prior art has the following advantages:
1, compared to the traditional technology reclaiming tantalum from ore, the present invention is directed to the recovery carrying out tantalum containing tantalum alloy waste material, needed for it, separating impurity element is more, Separation and Recovery difficulty is larger, domesticly at present there is no the report carrying out tantalum recovery from alloyed scrap, therefore, the invention provides the new approaches that a tantalum reclaims, there is good industrial prospect.
2, the present invention is directed to China's alloyed scrap mostly degrade utilization and recovery utilization rate this feature low, for the efficiency utilization of strategic non-renewable tantalum resources provides a kind of feasible way.
3, the present invention's operation is easy to realize, and under these processing condition, the rate of recovery of tantalum reaches more than 90%, and the quality purity of gained tantalum hydroxide product reaches more than 99.4%, is suitable for suitability for industrialized production.
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Accompanying drawing explanation
Fig. 1 is that the present invention is from containing the process flow sheet reclaiming tantalum tantalum alloy waste material.
Embodiment
Embodiment 1
What the present embodiment was pending containing the major metal component of tantalum alloy waste material is by weight percentage: Ta34.98%, Ti17.27%, Hf16.93%, W1.74%, Fe0.96%, Ni0.75%, Cr0.36%.Composition graphs 1, the present embodiment comprises the following steps from containing the method reclaiming tantalum tantalum alloy waste material:
Step one, take containing tantalum alloy waste material 15g, the hydrofluoric acid that 90mL concentration is 12mol/L is measured again according to solid-to-liquid ratio 1:6, then hydrofluoric acid is adopted to be that leaching agent carries out leaching process to containing the tantalum in tantalum alloy waste material, the temperature leaching process is 90 DEG C, the time of leaching process is 1.5h, obtains the leach liquor containing tantalum element; In specific implementation process, can by hydrofluoric acid with containing being placed in 500mL polytetrafluoroethylene beaker together with tantalum alloy waste material, then use plastics film sealed beaker mouth, then put into water-bath and carry out constant temperature agitation leach;
Step 2, employing hexone (MIBK) carry out extraction treatment 7min for extraction agent to leach liquor described in step one, make tantalum proceed in organic phase, after stratification, get upper organic phase, obtain the extraction liquid containing tantalum element; The volume ratio of described hexone and leach liquor is 5:1;
Step 3, to be added in extraction liquid described in step 2 by the sulfuric acid of concentration 6mol/L and carry out pickling impurity removal, the volume ratio of described sulfuric acid and extraction liquid is 5:1, after stratification, get upper organic phase, obtains the extraction liquid after removal of impurities;
Step 4, employing pure water carry out back extraction process 7min for reverse-extraction agent to the extraction liquid after removal of impurities described in step 3, make tantalum back extraction enter in aqueous phase, take off a layer aqueous phase after stratification, obtain the strip liquor containing tantalum element; The volume ratio of the extraction liquid after described pure water and removal of impurities is 5:1;
Step 5, in strip liquor described in step 4, drip the ammoniacal liquor that mass percent concentration is 28%, make tantalum and ammoniacal liquor generation precipitin reaction, until the pH value of strip liquor is 9 rear stoppings drip ammoniacal liquor, then there is the strip liquor of ammoniacal liquor to stir dropping, obtain dirty solution;
Step 6, dirty solution described in step 5 to be filtered, then the solid trapped substance after filtration is placed in loft drier dry, adopt fourier to change infrared spectrum analysis instrument after naturally cooling and FTIR detection analysis is carried out to dried solid matter, record in reclaimed solid matter and be rich in tantalum, and tantalum mainly exists with the form of tantalum hydroxide.
The main chemical compositions of tantalum hydroxide prepared by the present embodiment is as shown in table 1.Draw as calculated and adopt the rate of recovery of tantalum after the present embodiment process to be 91.58%.
Embodiment 2:
What the present embodiment was pending containing the major metal component of tantalum alloy waste material is by weight percentage: Ta31.75%, Nb15.26%, Ti13.58%, Hf11.36%, W1.17%, Zr1.03%, Fe0.78%, Ni0.66%, Cr0.55%.Composition graphs 1, the present embodiment comprises the following steps from containing the method reclaiming tantalum tantalum alloy waste material:
Step one, take containing tantalum alloy waste material 15g, the hydrofluoric acid that 135mL concentration is 11mol/L is measured again according to solid-to-liquid ratio 1: 9, then hydrofluoric acid is adopted to be that leaching agent carries out leaching process to containing the tantalum in tantalum alloy waste material, the temperature leaching process is 85 DEG C, the time of leaching process is 2.5h, obtains the leach liquor containing tantalum element; In specific implementation process, can by hydrofluoric acid with containing being placed in 500mL polytetrafluoroethylene beaker together with tantalum alloy waste material, then use plastics film sealed beaker mouth, then put into water-bath and carry out constant temperature agitation leach;
Step 2, employing hexone (MIBK) carry out extraction treatment 5min for extraction agent to leach liquor described in step one, make tantalum proceed in organic phase, after stratification, get upper organic phase, obtain the extraction liquid containing tantalum element; The volume ratio of described hexone and leach liquor is 4:1;
Step 3, to be added in extraction liquid described in step 2 by the sulfuric acid of concentration 2.5mol/L and carry out pickling impurity removal, the volume ratio of described sulfuric acid and extraction liquid is 4:1, after stratification, get upper organic phase, obtains the extraction liquid after removal of impurities;
Step 4, employing pure water carry out back extraction process 5min for reverse-extraction agent to the extraction liquid after removal of impurities described in step 3, make tantalum back extraction enter in aqueous phase, take off a layer aqueous phase after stratification, obtain the strip liquor containing tantalum element; The volume ratio of the extraction liquid after described pure water and removal of impurities is 4:1;
Step 5, in strip liquor described in step 4, drip the ammoniacal liquor that mass percent concentration is 25%, make tantalum and ammoniacal liquor generation precipitin reaction, until the pH value of strip liquor is 10 rear stoppings drip ammoniacal liquor, then there is the strip liquor of ammoniacal liquor to stir dropping, obtain dirty solution;
Step 6, dirty solution described in step 5 to be filtered, then the solid trapped substance after filtration is placed in loft drier dry, adopt fourier to change infrared spectrum analysis instrument after naturally cooling and FTIR detection analysis is carried out to dried solid matter, record in reclaimed solid matter and be rich in tantalum, and tantalum mainly exists with the form of tantalum hydroxide.
The main chemical compositions of tantalum hydroxide prepared by the present embodiment is as shown in table 1.Draw as calculated and adopt the rate of recovery of tantalum after the present embodiment process to be 92.46%.
Embodiment 3:
What the present embodiment was pending containing the major metal component of tantalum alloy waste material is by weight percentage: Ta20.12%, Nb17.58%, Ti13.11%, Hf13.06%, Zr4.15%, Fe0.62%, Ni0.49%, Cr0.47%, Co0.11%.Composition graphs 1, the present embodiment comprises the following steps from containing the method reclaiming tantalum tantalum alloy waste material:
Step one, take containing tantalum alloy waste material 15g, the hydrofluoric acid that 120mL concentration is 8mol/L is measured again according to solid-to-liquid ratio 1: 8, then hydrofluoric acid is adopted to be that leaching agent carries out leaching process to containing the tantalum in tantalum alloy waste material, the temperature leaching process is 70 DEG C, the time of leaching process is 2h, obtains the leach liquor containing tantalum element; In specific implementation process, can by hydrofluoric acid with containing being placed in 500mL polytetrafluoroethylene beaker together with tantalum alloy waste material, then use plastics film sealed beaker mouth, then put into water-bath and carry out constant temperature agitation leach;
Step 2, employing hexone (MIBK) carry out extraction treatment 3min for extraction agent to leach liquor described in step one, make tantalum proceed in organic phase, after stratification, get upper organic phase, obtain the extraction liquid containing tantalum element; The volume ratio of described hexone and leach liquor is 3:1;
Step 3, to be added in extraction liquid described in step 2 by the sulfuric acid of concentration 2mol/L and carry out pickling impurity removal, the volume ratio of described sulfuric acid and extraction liquid is 3:1, after stratification, get upper organic phase, obtains the extraction liquid after removal of impurities;
Step 4, employing pure water carry out back extraction process 3min for reverse-extraction agent to the extraction liquid after removal of impurities described in step 3, make tantalum back extraction enter in aqueous phase, take off a layer aqueous phase after stratification, obtain the strip liquor containing tantalum element; The volume ratio of the extraction liquid after described pure water and removal of impurities is 3:1;
Step 5, in strip liquor described in step 4, drip the ammoniacal liquor that mass percent concentration is 26%, make tantalum and ammoniacal liquor generation precipitin reaction, until the pH value of strip liquor is 8 rear stoppings drip ammoniacal liquor, then there is the strip liquor of ammoniacal liquor to stir dropping, obtain dirty solution;
Step 6, dirty solution described in step 5 to be filtered, then the solid trapped substance after filtration is placed in loft drier dry, adopt fourier to change infrared spectrum analysis instrument after naturally cooling and FTIR detection analysis is carried out to dried solid matter, record in reclaimed solid matter and be rich in tantalum, and tantalum mainly exists with the form of tantalum hydroxide.
The main chemical compositions of tantalum hydroxide prepared by the present embodiment is as shown in table 1.Draw as calculated, after adopting the present embodiment process, the rate of recovery of tantalum is 90.31%.
Table 1 embodiment of the present invention 1 to 3 reclaims the main chemical compositions of the tantalum hydroxide product obtained
| Content (wt%) | Tantalum hydroxide | Niobium hydroxide | Chromium hydroxide | Titanium hydroxide |
| Embodiment 1 | 99.78 | - | 0.08 | 0.06 |
| Embodiment 2 | 99.49 | 0.28 | 0.10 | 0.07 |
| Embodiment 3 | 99.42 | 0.31 | 0.08 | 0.05 |
As shown in Table 1, the quality purity of the tantalum hydroxide that the embodiment of the present invention 1 to 3 prepares is up to more than 99.4%, and foreign matter content is low.It can thus be appreciated that the present invention is directed to containing dopant species in tantalum alloy raw material many, this characteristic of tantalum separation difficulty carries out R&D work, propose a kind of from containing the novel method reclaiming tantalum tantalum waste material, the rate of recovery of tantalum is high, has good industrial prospect.
The above is only preferred embodiment of the present invention, not imposes any restrictions the present invention.Every above embodiment is done according to invention technical spirit any simple modification, change and equivalence change, all still belong in the protection domain of technical solution of the present invention.
Claims (5)
1., from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the method comprises the following steps:
Step one, employing hydrofluoric acid are that leaching agent carries out leaching process to containing the tantalum in tantalum alloy waste material, obtain leach liquor; Described is 20% ~ 35% containing the mass percentage of tantalum in tantalum alloy waste material, the described temperature leaching process is 70 DEG C ~ 90 DEG C, the described time of leaching process is 1.5h ~ 2.5h, the described solid-to-liquid ratio containing tantalum alloy waste material and hydrofluoric acid is 1: (6 ~ 9), the described unit containing tantalum alloy waste material is g, and the unit of described hydrofluoric acid is mL; The concentration of described hydrofluoric acid is 8mol/L ~ 12mol/L;
Step 2, employing hexone carry out extraction treatment for extraction agent to leach liquor described in step one, get upper organic phase, be extracted liquid after stratification; The volume ratio of described hexone and leach liquor is (3 ~ 5): 1;
Step 3, to be added in extraction liquid described in step 2 by sulfuric acid and carry out pickling impurity removal, the volume ratio of described sulfuric acid and extraction liquid is (3 ~ 5): 1, gets upper organic phase, obtain the extraction liquid after removal of impurities after stratification;
Step 4, employing pure water carry out back extraction process for reverse-extraction agent to the extraction liquid after removal of impurities described in step 3, take off a layer aqueous phase, obtain strip liquor after stratification; The volume ratio of the extraction liquid after described pure water and removal of impurities is (3 ~ 5): 1;
Step 5, in strip liquor described in step 4, drip ammoniacal liquor, be till 8 ~ 10 until the pH value of strip liquor, then have the strip liquor of ammoniacal liquor to stir dropping, obtain dirty solution;
Step 6, dirty solution described in step 5 to be filtered, then the solid trapped substance after filtering is placed in loft drier dry, after naturally cooling, obtains tantalum hydroxide.
2. according to claim 1 a kind of from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the time of extraction treatment described in step 2 is 3min ~ 7min.
3. according to claim 1 a kind of from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the concentration of sulfuric acid described in step 3 is 2mol/L ~ 6mol/L.
4. according to claim 1 a kind of from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the time of the process of back extraction described in step 4 is 3min ~ 7min.
5. according to claim 1 a kind of from containing the method reclaiming tantalum tantalum alloy waste material, it is characterized in that, the mass percent concentration of ammoniacal liquor described in step 5 is 25% ~ 28%.
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| CN110510671A (en) * | 2019-09-18 | 2019-11-29 | 广东先导稀材股份有限公司 | A method of recycling prepares high-purity tantalum pentoxide from waste and old tantalum target |
| CN111057879A (en) * | 2020-01-02 | 2020-04-24 | 荆门德威格林美钨资源循环利用有限公司 | Process method for separating tantalum and niobium elements from hard alloy |
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