CN106916973B - A method of recycling hafnium from high temperature alloy acid solution - Google Patents
A method of recycling hafnium from high temperature alloy acid solution Download PDFInfo
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- CN106916973B CN106916973B CN201710252612.3A CN201710252612A CN106916973B CN 106916973 B CN106916973 B CN 106916973B CN 201710252612 A CN201710252612 A CN 201710252612A CN 106916973 B CN106916973 B CN 106916973B
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Abstract
The method that the invention discloses a kind of to recycle hafnium from high temperature alloy acid solution, this method are:One, the pH value of high temperature alloy acid solution is adjusted to 0.5~2.5, then the hafnium in high temperature alloy acid solution is adsorbed using ion exchange resin;Two, hafnium is desorbed using hydrochloric acid solution, obtains stripping liquid containing hafnium;Three, stripping liquid containing hafnium is neutralized using ammonium hydroxide or sodium hydroxide solution, control terminal pH is 2.5~11, and filtering and dry after 3~4h of standing can be obtained hafnium enriched substance.The present invention uses weak-base ion-exchange resin selective absorption hafnium, and the hafnium in high temperature alloy acid solution can effectively be avoided to lose, simple for process, good operational environment, and production cost is low.
Description
Technical field
The invention belongs to rare metal resources utilization technology fields, and in particular to one kind is from high temperature alloy acid solution
The method for recycling hafnium.
Background technique
Hafnium is a kind of rare metal granite, have corrosion-resistant, high temperature resistant, high antioxidant, good electrical and thermal conductivity, compared with
The characteristics such as low electron work functon and stronger absorption neutron ability, make it be widely used in the control rod of atomic pile and guarantor
Protection unit, high-temperature alloy material, plasma emitter etc..Hafnium does not have individual mineral, always total with zirconium in nature
Together, the hafnium content in nature zirconium is generally 2%~3% for life.Hafnium is usually that by-product is used as in the production technology of zirconium
Product recycling, the technique of industrial application comparative maturity is that the acid solution of hafnium containing zirconium is extracted using MIBK-HSCN system at present, preferential to extract
Hafnium, zirconium then stay in water phase, efficiently separate zirconium and hafnium, and the process flow is simple, extraction efficiency is high, but its disadvantage has
MIBK toxicity is big, and solubility in water is larger, and loss is serious, and HSCN is unstable, is easy to decompose release noxious material, cause
Environmental pollution.
Waste high-temperature alloy contains 1%~2% metal hafnium, is a kind of important secondary resource for recycling hafnium.It is waste and old at present
The processing of high temperature alloy is usually to use hydrochloric acid or sulfuric acid system molten to high-temperature alloy waste material progress oxidation acid leaching or electricity, about useless
20%~50% hafnium in old high temperature alloy is transferred to solution, and remainder remains in slag, and dissolves in high-temperature alloy waste material
Along with the dissolution of a large amount of base metals such as nickel, cobalt, chromium, aluminium in journey, so that the high temperature obtained after oxidation acid leaching or the molten processing of electricity closes
The hafnium of nickel, cobalt, chromium, aluminium and low concentration in auric acid solution containing high concentration.If do not added to hafnium in high temperature alloy acid solution
With recycling, the waste of hafnium resource will cause.Using the hafnium in traditional chemical precipitation method recycling high temperature alloy acid solution, simple process
It is easy, but other base metals can also avale together while heavy hafnium, cause subsequent hafnium separation difficult.Using solvent extraction
When recycling hafnium in high temperature alloy acid solution, nickel, cobalt, chromium, the aluminium of high concentration will cause extractant poisoning, reduce extraction efficiency.
Summary of the invention
It is a kind of from high temperature conjunction technical problem to be solved by the present invention lies in view of the above shortcomings of the prior art, providing
The method of hafnium is recycled in auric acid solution.This method uses weak-base anion-exchange resin selective absorption hafnium, then uses hydrochloric acid
Solution stripping is supported on the hafnium on resin, and hafnium in high temperature alloy acid solution can effectively be avoided to lose, simple for process, production
It is at low cost.
In order to solve the above technical problems, the technical solution adopted by the present invention is that:One kind is recycled from high temperature alloy acid solution
The method of hafnium, which is characterized in that this approach includes the following steps:
Step 1: the high temperature alloy using saturated solution of sodium bicarbonate or sodium hydroxide saturated solution by pH value less than 0.5
The pH value of acid solution is adjusted to 0.5~2.5, and weak-base anion-exchange resin is then used to close pH value for 0.5~2.5 high temperature
Auric acid solution carries out ion-exchange treatment, is adsorbed on the hafnium in high temperature alloy acid solution on weak-base ion-exchange resin;Institute
State in high temperature alloy acid solution of the pH value less than 0.5 containing nickel, cobalt, chromium, aluminium and hafnium element, wherein the concentration of nickel be 20g/L~
70g/L, the concentration of cobalt are 3g/L~15g/L, and the concentration of chromium is 2g/L~12g/L, and the concentration of aluminium is 1g/L~7g/L, hafnium it is dense
Degree is 0.04g/L~1g/L;
Step 2: the hafnium solution being adsorbed on weak-base ion-exchange resin in step 1 is drawn to liquid using hydrochloric acid solution
Phase obtains stripping liquid containing hafnium;
Step 3: using stripping liquid containing hafnium described in ammonium hydroxide or sodium hydroxide solution neutralization procedure two, and control terminal pH
It is 2.5~11, filters and dry after standing 3h~4h, obtain hafnium enriched substance.
A kind of above-mentioned method that hafnium is recycled from high temperature alloy acid solution, which is characterized in that weak base described in step 1
Property anion exchange resin be D315 resin.
A kind of above-mentioned method that hafnium is recycled from high temperature alloy acid solution, which is characterized in that hydrochloric acid described in step 2
The molar concentration of solution is 4.5mol/L~8mol/L, and the dosage of the hydrochloric acid solution is the weak-base ion-exchange resin body
Long-pending 10~15 times.
A kind of above-mentioned method that hafnium is recycled from high temperature alloy acid solution, which is characterized in that ammonium hydroxide described in step 3
Mass percent concentration be 25%~28%, the mass percent concentration of the sodium hydroxide solution is 20%~40%.
A kind of above-mentioned method that hafnium is recycled from high temperature alloy acid solution, which is characterized in that dried described in step 3
Temperature be 85 DEG C~100 DEG C, time of drying is 3h~6h.
Compared with the prior art, the present invention has the following advantages:
1, technological improvement of the invention is:The present invention is high for Ni, Co, Cr aluminum concentration in high temperature alloy acid solution, hafnium is dense
Low and high acidity feature is spent, uses saturated solution of sodium bicarbonate or sodium hydroxide saturated solution by pH value less than 0.5 first
The pH value of high temperature alloy acid solution is adjusted to 0.5~2.5, not only can guarantee effective absorption of hafnium, but also can be avoided and cause because pH is excessively high
The loss of nickel and cobalt;Then by selective absorption hafnium process, realization hafnium is efficiently separated with other base metals, shortens subsequent place
Science and engineering sequence reduces the shunting loss of hafnium, improves the rate of recovery of hafnium.
2, the present invention uses weak-base anion-exchange resin selective absorption hafnium, saves the separation of hafnium He other base metals
Process, simple for process, good operational environment, production cost are low.
3, the present invention is adaptable to the variation of material composition, is similar to other of high temperature alloy acid solution suitable for ingredient
Solution, hafnium are separated and recovered substantially, and the hafnium rate of recovery is high, are conducive to industrial applications.
4, the present invention realizes the comprehensive reutilization of hafnium secondary resource, has significant economic benefit and environmental benefit.
In conclusion the method for the present invention simple process, good operational environment, at low cost, hafnium rate of recovery height, can effectively solve existing
There is the problems such as process existing for hafnium recovery method is many and diverse, production environment is severe, hafnium loss is larger.
Technical solution of the present invention is described in further detail below by embodiment.
Specific embodiment
Embodiment 1
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using saturated solution of sodium bicarbonate that pH is adjusted to 0.5 for the pH value of -0.8 high temperature alloy acid solution, so
It uses D315 weak-base anion-exchange resin to carry out ion-exchange treatment to pH value for 0.5 high temperature alloy acid solution afterwards, makes
Hafnium in high temperature alloy acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is -0.8 is handed in ion
The chemical component changed before and after the processing is shown in Table 1;
Step 2: preparing the hydrochloric acid solution of 8mol/L by 10 times of weak-base anion-exchange resin volumes first, adopt later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to liquid phase with hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: using mass percent concentration for stripping liquid containing hafnium described in 25% ammonium hydroxide neutralization procedure two, control
Terminal pH is 2.5, filters after standing 4h and dries 6h at 85 DEG C, obtains hafnium enriched substance.
Chemical component/gL of the 1 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 23.31 | 3.84 | 4.09 | 2.10 | 0.84 |
After ion-exchange treatment | 21.89 | 3.65 | 3.84 | 2.04 | 0.012 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 94.05% after the present embodiment is handled.
Embodiment 2
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using sodium hydroxide saturated solution that pH is adjusted to 1.5 for the pH value of 0.45 high temperature alloy acid solution, so
It uses D315 weak-base anion-exchange resin to carry out ion-exchange treatment to pH value for 1.5 high temperature alloy acid solution afterwards, makes
Hafnium in high temperature alloy acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is 0.45 is handed in ion
The chemical component changed before and after the processing is shown in Table 2;
Step 2: preparing the hydrochloric acid solution of 6mol/L by 12 times of weak-base anion-exchange resin volumes first, adopt later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to liquid phase with hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: mass percent concentration is used to desorb to contain hafnium described in 30% sodium hydroxide solution neutralization procedure two
Liquid, control terminal pH are 4, filter after standing 3h and dry 5h at 90 DEG C, obtain hafnium enriched substance.
Chemical component/gL of the 2 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 67.28 | 13.90 | 11.84 | 6.66 | 0.053 |
After ion-exchange treatment | 65.34 | 12.57 | 10.75 | 6.12 | 0.002 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 93.58% after the present embodiment is handled.
Embodiment 3
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using sodium hydroxide saturated solution that pH is adjusted to 2 for the pH value of -0.28 high temperature alloy acid solution, so
It uses D315 weak-base anion-exchange resin to carry out ion-exchange treatment to pH value for 2 high temperature alloy acid solution afterwards, makes height
Hafnium in temperature alloy acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is -0.28 is handed in ion
The chemical component changed before and after the processing is shown in Table 3;
Step 2: the hydrochloric acid solution of 4.5mol/L is prepared by 14 times of weak-base anion-exchange resin volumes first, later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to by liquid phase using hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: mass percent concentration is used to desorb to contain hafnium described in 40% sodium hydroxide solution neutralization procedure two
Liquid, control terminal pH are 9, filter after standing 4h and dry 4h at 95 DEG C, obtain hafnium enriched substance.
Chemical component/gL of the 3 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 55.38 | 11.06 | 10.75 | 5.24 | 0.42 |
After ion-exchange treatment | 54.09 | 9.86 | 9.07 | 4.87 | 0.009 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 95.26% after the present embodiment is handled.
Embodiment 4
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using saturated solution of sodium bicarbonate that pH is adjusted to 2.5 for the pH value of 0.25 high temperature alloy acid solution, so
It uses D315 weak-base anion-exchange resin to carry out ion-exchange treatment to pH value for 2.5 high temperature alloy acid solution afterwards, makes
Hafnium in high temperature alloy acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is 0.25 is handed in ion
The chemical component changed before and after the processing is shown in Table 4;
Step 2: the hydrochloric acid solution of 6.5mol/L is prepared by 13 times of weak-base anion-exchange resin volumes first, later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to by liquid phase using hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: using mass percent concentration for stripping liquid containing hafnium described in 28% ammonium hydroxide neutralization procedure two, control
Terminal pH is 11, filters after standing 3h and dries 3h at 100 DEG C, obtains hafnium enriched substance.
Chemical component/gL of the 4 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 20.87 | 14.79 | 11.92 | 6.84 | 0.96 |
After ion-exchange treatment | 20.46 | 14.12 | 11.56 | 6.65 | 0.031 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 93.86% after the present embodiment is handled.
Embodiment 5
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using saturated solution of sodium bicarbonate that pH is adjusted to 2 for the pH value of -1.56 high temperature alloy acid solution, so
It uses D315 weak-base anion-exchange resin to carry out ion-exchange treatment to pH value for 2 high temperature alloy acid solution afterwards, makes height
Hafnium in temperature alloy acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is -1.56 is handed in ion
The chemical component changed before and after the processing is shown in Table 5;
Step 2: the hydrochloric acid solution of 5.5mol/L is prepared by 15 times of weak-base anion-exchange resin volumes first, later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to by liquid phase using hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: mass percent concentration is used to desorb to contain hafnium described in 20% sodium hydroxide solution neutralization procedure two
Liquid, control terminal pH are 10, filter after standing 3.5h and dry 4h at 90 DEG C, obtain hafnium enriched substance.
Chemical component/gL of the 5 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 68.95 | 3.54 | 2.34 | 1.47 | 0.046 |
After ion-exchange treatment | 68.71 | 3.28 | 2.15 | 1.31 | 0.001 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 94.75% after the present embodiment is handled.
Embodiment 6
The method that the present embodiment recycles hafnium from high temperature alloy acid solution includes the following steps:
Step 1: using sodium hydroxide saturated solution that pH is adjusted to 1 for the pH value of 0 high temperature alloy acid solution, then adopt
Ion-exchange treatment is carried out with the high temperature alloy acid solution that D315 weak-base anion-exchange resin is 1 to pH value, closes high temperature
Hafnium in auric acid solution is adsorbed on ion exchange resin;The high temperature alloy acid solution that the pH is 0 is before ion-exchange treatment
Chemical component afterwards is shown in Table 6;
Step 2: preparing the hydrochloric acid solution of 7mol/L by 11 times of weak-base anion-exchange resin volumes first, adopt later
The hafnium solution being adsorbed on ion exchange resin in step 1 is drawn to liquid phase with hydrochloric acid solution, obtains stripping liquid containing hafnium;
Step 3: using mass percent concentration for stripping liquid containing hafnium described in 26.5% ammonium hydroxide neutralization procedure two, control
Terminal pH processed is 7, filters after standing 3.5h and dries 3h at 100 DEG C, obtains hafnium enriched substance.
Chemical component/gL of the 6 the present embodiment high temperature alloy acid solution of table before and after ion-exchange treatment-1
Element | Ni | Co | Cr | Al | Hf |
Before ion-exchange treatment | 42.38 | 8.76 | 6.97 | 4.38 | 0.64 |
After ion-exchange treatment | 42.02 | 8.53 | 6.75 | 4.12 | 0.009 |
Constituent analysis is carried out to hafnium enriched substance manufactured in the present embodiment using x ray fluorescence spectrometry, obtains hafnium enrichment
The chemical component of object is shown in Table 7.By being calculated, the rate of recovery of hafnium is 95.82% after the present embodiment is handled.
The x ray fluorescence spectrometry of hafnium enriched substance obtained by 7 Examples 1 to 6 of table analyzes result
As shown in Table 7, the present invention is by the hafnium enriching and recovering in high temperature alloy acid solution, the grade containing hafnium of gained hafnium enriched substance
Greater than 50%, there is very high economic value.
The above is only presently preferred embodiments of the present invention, is not intended to limit the invention in any way.It is all according to invention skill
Art any simple modification, change and equivalence change substantially to the above embodiments, still fall within technical solution of the present invention
Protection scope in.
Claims (4)
1. a kind of method for recycling hafnium from high temperature alloy acid solution, which is characterized in that this approach includes the following steps:
Step 1: the high temperature alloy acid using saturated solution of sodium bicarbonate or sodium hydroxide saturated solution by pH value less than 0.5 is molten
The pH value of liquid is adjusted to 0.5~2.5, then uses weak-base anion-exchange resin sour for 0.5~2.5 high temperature alloy to pH value
Solution carries out ion-exchange treatment, is adsorbed on the hafnium in high temperature alloy acid solution on weak-base ion-exchange resin;The pH
It is worth in the high temperature alloy acid solution less than 0.5 and contains nickel, cobalt, chromium, aluminium and hafnium element, wherein the concentration of nickel is 20g/L~70g/
L, the concentration of cobalt are 3g/L~15g/L, and the concentration of chromium is 2g/L~12g/L, and the concentration of aluminium is 1g/L~7g/L, and the concentration of hafnium is
0.04g/L~1g/L;The weak-base anion-exchange resin is D315 resin;
Step 2: the hafnium solution being adsorbed on weak-base ion-exchange resin in step 1 is drawn to liquid phase using hydrochloric acid solution, obtain
To stripping liquid containing hafnium;
Step 3: using stripping liquid containing hafnium described in ammonium hydroxide or sodium hydroxide solution neutralization procedure two, and controlling terminal pH is 2.5
~11, it filters and dries after standing 3h~4h, obtain hafnium enriched substance.
2. a kind of method for recycling hafnium from high temperature alloy acid solution according to claim 1, which is characterized in that step 2
Described in the molar concentration of hydrochloric acid solution be 4.5mol/L~8mol/L, the dosage of the hydrochloric acid solution is the weakbase ion
10~15 times of exchanger resin volume.
3. a kind of method for recycling hafnium from high temperature alloy acid solution according to claim 1, which is characterized in that step 3
Described in the mass percent concentration of ammonium hydroxide be 25%~28%, the mass percent concentration of the sodium hydroxide solution is 20%
~40%.
4. a kind of method for recycling hafnium from high temperature alloy acid solution according to claim 1, which is characterized in that step 3
Described in the temperature of drying be 85 DEG C~100 DEG C, time of drying is 3h~6h.
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CN103789552A (en) * | 2014-02-27 | 2014-05-14 | 西北有色金属研究院 | Method for recovering rhenium from high-temperature alloy pickle liquor |
CN104646659A (en) * | 2013-11-22 | 2015-05-27 | 北京有色金属研究总院 | Method for preparing low-oxygen high-pure metal hafnium powder |
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CN103789552A (en) * | 2014-02-27 | 2014-05-14 | 西北有色金属研究院 | Method for recovering rhenium from high-temperature alloy pickle liquor |
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