CN109468460A - A kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium - Google Patents
A kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium Download PDFInfo
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- CN109468460A CN109468460A CN201811310157.9A CN201811310157A CN109468460A CN 109468460 A CN109468460 A CN 109468460A CN 201811310157 A CN201811310157 A CN 201811310157A CN 109468460 A CN109468460 A CN 109468460A
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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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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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
- C22B34/10—Obtaining titanium, zirconium or hafnium
- C22B34/14—Obtaining zirconium or hafnium
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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
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Abstract
The invention belongs to TBP abstraction technique fields, and in particular to a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium.The following steps are included: step 1: precipitating；Step 2: filtering and washing removing chloride；Step 3: squeezing purging；Step 4: dispersion mixing；Step 5: nitric acid dissolves；Step 6: constant volume degree of thickening；Step 7: filtering.The present invention is used for low chlorine root, the highly selective extraction stoste of TBP extracting and separating zirconium and hafnium.The advantage of this method is that, preparation process is simple, extraction stoste separating factor obtained is big and stablizes, selectivity is high, and chloride content is low, almost corrosion-free to equipment, quality is stablized, it convenient for extracting operation control, can be separated by single extraction, the zirconium solution without hafnium for meeting nuclear leve standard and the hafnium solution without zirconium is made.
Description
Technical field
The invention belongs to TBP abstraction technique fields, and in particular to a kind of for the highly selective of TBP extracting and separating zirconium and hafnium
Extract stoste preparation method.
Background technique
The key of TBP extracting and separating zirconium and hafnium is to extract the preparation of stoste, it is common practice to by ZrOCl2·8H2O is molten
Yu Shui, with HCl and HNO3Adjust acidity and zirconium, hafnium ion concentration.This method is obtained to extract stoste, and separating factor is small, selection
Property it is poor, chloride content is high, severe corrosion to equipment.
Traditional technical solution needs to develop a kind of for TBP extracting and separating zirconium and hafnium due to facing above-mentioned deficiency
Highly selective extraction stoste preparation method, to solve the above problems.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of highly selective extraction for TBP extracting and separating zirconium and hafnium is former
Liquid and preparation method thereof, to realize that preparation process is simple, extraction stoste separating factor obtained is big and stablizes, the high mesh of selectivity
's.
In order to realize the purpose, the technical solution adopted by the present invention is that:
A kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium, comprising the following steps:
Step 1: precipitating
1.1, by ZrOCl2·8H2O is dissolved in 40~60 DEG C of hot water in the ratio of liquid-solid ratio 3:1~5:1mL/g；Liquid is solid
The meaning of ratio is liquid volume: solid weight；
1.2, the product for obtaining step 1.1 is added in the NaOH aqueous solution that mass concentration is 20~32% and precipitates
And aging, obtain slurry；
Step 2: filtering and washing removing chloride
2.1, slurry is filtered with diaphragm filter press, obtains filter cake；
It detects filtrate and detects CL?Content, CL?Continue when > 100mg/L in next step, CL?Step is gone to when≤100mg/L
Three；
2.2, the filter cake that step 2.1 is obtained by filtration is added in the hot water that temperature is 40~60 DEG C, and slurrying stirring is made
Slurry；
Step 2.1 and step 2.2 are repeated, slurrying is filtered repeatedly, until detecting CL in filtrate?≤100mg/L；
Step 3: squeezing purging
3.1, the filter cake for eliminating chloride ion for obtaining step 2 is further squeezed with diaphragm filter press；
3.2, compressed air purging, remaining filtrate in blowing materail tube, diaphragm filter press are used after squeezing；
Step 4: dispersion mixing
4.1, the filter cake Weighing for obtaining step 3 analyzes wherein Zr content；
4.2, dissolution kettle is put into, is crushed dispersion under stirring；
4.3, granular NaNO is put into the material after broken dispersion3Solid is uniformly mixed；
Mixed proportion is Zr:NaNO3Mass ratio be 1:3~1:4；
Step 5: nitric acid dissolves
Under the action of stirring, into the uniformly mixed material that step 4 obtains, be added mass concentration be 98% it is dense
For nitric acid to being completely dissolved, the mass ratio of concentrated nitric acid and mixture is 1:2.5~1:3；
Step 6: constant volume degree of thickening
Into the dissolved liquid material that step 5 obtains, addition industry water adjusts the Zr ion concentration in solution to 60
~91g/L.
Step 7: filtering
The liquid material that step 6 is obtained, is filtered with bag type filtering machine, obtains the height for TBP extracting and separating zirconium and hafnium
Selective extraction stoste.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 1.2, precipitation temperature is room temperature, and precipitating endpoint pH is 8~9, and the precipitation reaction time is 60~90min, when aging
Between be 40~60min.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 2.1, the filter pressure control of diaphragm filter press is 0.4~0.6MPa.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 2.2,20~30min is stirred in slurrying.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 2.2, the ratio of filter cake and hot water is liquid-solid ratio 3:1~5:1.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 3.1, squeeze pressure 0.8MPa.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 3.1, the squeezing time is 15~20min.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in step 3.2, the compressed air purging for being 0.6MPa with pressure.
Further, a kind of highly selective extraction stoste preparation side for TBP extracting and separating zirconium and hafnium as described above
Method, in the 5th step, then 120~150min of dissolution first observes whether solid material is completely dissolved, carries out if being completely dissolved
In next step；
Otherwise 70~90 DEG C are warming up to, then extends dissolution time to being completely dissolved.
The beneficial effect of technical solution of the present invention is:
The present invention is used for low chlorine root, the highly selective extraction stoste of TBP extracting and separating zirconium and hafnium.The advantage of this method exists
In preparation process is simple, and extraction stoste separating factor obtained is big and stablizes, and selectivity is high, and chloride content is low, almost to equipment
Corrosion-free, quality is stablized, and controls, can be separated by single extraction convenient for extracting operation, be made meet nuclear leve standard without hafnium
Zirconium solution and hafnium solution without zirconium.
Detailed description of the invention
Fig. 1 is the method for the present invention schematic diagram.
Specific embodiment
Technical solution of the present invention is described in detail in the following with reference to the drawings and specific embodiments.
As shown in Figure 1, a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium of the present invention,
The following steps are included:
Step 1: precipitating
1.1, by ZrOCl2·8H2O is dissolved in 40~60 DEG C of hot water in the ratio of liquid-solid ratio 3:1~5:1mL/g；Liquid is solid
The meaning of ratio is liquid volume: solid weight；
1.2, the product for obtaining step 1.1 is added in the NaOH aqueous solution that mass concentration is 20~32% and precipitates
And aging, obtain slurry；
Precipitation temperature is room temperature, and precipitating endpoint pH is 8~9, and the precipitation reaction time is 60~90min, and ageing time is
40~60min.
Step 2: filtering and washing removing chloride
2.1, slurry is filtered with diaphragm filter press, obtains filter cake；The filter pressure control of diaphragm filter press for 0.4~
0.6MPa。
It detects filtrate and detects CL?Content, CL?Continue when > 100mg/L in next step, CL?Step is gone to when≤100mg/L
Three；
2.2, the filter cake that step 2.1 is obtained by filtration is added in the hot water that temperature is 40~60 DEG C, and slurrying stirring is made
Slurry；The ratio of slurrying 20~30min of stirring, filter cake and hot water is liquid-solid ratio 3:1~5:1.
Step 2.1 and step 2.2 are repeated, slurrying is filtered repeatedly, until detecting CL in filtrate?≤100mg/L；
Step 3: squeezing purging
3.1, the filter cake for eliminating chloride ion for obtaining step 2 is further squeezed with diaphragm filter press；Squeeze pressure is
0.8MPa, squeezing time are 15~20min.
3.2, the compressed air purging for being 0.6MPa with pressure after squeezing blows down materail tube, residual in diaphragm filter press
The filtrate stayed；
Step 4: dispersion mixing
4.1, the filter cake Weighing for obtaining step 3 analyzes wherein Zr content；
4.2, dissolution kettle is put into, is crushed dispersion under stirring；
4.3, granular NaNO is put into the material after broken dispersion3Solid is uniformly mixed；
Mixed proportion is Zr:NaNO3Mass ratio be 1:3~1:4；
Step 5: nitric acid dissolves
Under the action of stirring, into the uniformly mixed material that step 4 obtains, be added mass concentration be 98% it is dense
For nitric acid to being completely dissolved, the mass ratio of concentrated nitric acid and mixture is 1:2.5~1:3；
In the present embodiment, 120~150min is dissolved first, then observes whether solid material is completely dissolved, if completely
Dissolution then carries out in next step；
Otherwise 70~90 DEG C are warming up to, then extends dissolution time to being completely dissolved.
Step 6: constant volume degree of thickening
Into the dissolved liquid material that step 5 obtains, addition industry water adjusts the Zr ion concentration in solution to 60
~91g/L.
Step 7: filtering
The liquid material that step 6 is obtained, is filtered with bag type filtering machine, obtains the height for TBP extracting and separating zirconium and hafnium
Selective extraction stoste.
Example one: ZrOCl is weighed2·8H2O about 400kg, is dissolved in 1.5m360 DEG C of industrial hot water in, be slow added into
Precipitated into the liquid alkaline of 20% (wt), obtained slurry is filtered with diaphragm filter press, filter cake with liquid-solid ratio for 5:1 ratio with 60
DEG C industrial hot water slurrying washing and filters pressing, 4 times repeatedly.Filter cake after being washed with diaphragm filter press to last time carries out physics
Squeezing, squeeze pressure 0.8MPa, the NaNO of filter cake and 400kg3After mixing, the concentrated nitric acid 480kg of 98% (wt) is added,
Material to be mixed is all after dissolution, adjusts the concentration of Zr (Hf) ion to 1mol/L with industry water.Extraction stoste obtained is clear thorough
It is bright, for TBP extracting and separating zirconium and when hafnium, anti-stripping agent be meet nuclear leve standard without hafnium zirconium nitrate solution, extracting extraction raffinate is
Meet nuclear leve standard without zirconium hafnium nitrate solution.
Example two: ZrOCl is weighed2·8H2O about 800kg, is dissolved in 4m345 DEG C of industrial hot water in, be slow added into
Precipitated in the liquid alkaline of 32% (wt), obtained slurry is filtered with diaphragm filter press, filter cake with liquid-solid ratio for 5:1 ratio with 45 DEG C
Industrial hot water slurrying washing and filters pressing, 4 times repeatedly.Filter cake after being washed with diaphragm filter press to last time carries out physics pressure
It squeezes, squeeze pressure 0.8MPa, the NaNO of filter cake and 750kg3After mixing, the concentrated nitric acid 950kg of 98% (wt) is added, to
Mixture all after dissolution, adjusts the concentration of Zr (Hf) ion to 1mol/L with industry water.Extraction stoste obtained is transparent,
For TBP extracting and separating zirconium and when hafnium, anti-stripping agent be meet nuclear leve standard without hafnium zirconium nitrate solution, extracting extraction raffinate is to meet
Nuclear leve standard without zirconium hafnium nitrate solution.
Example three: ZrOCl is weighed2·8H2O about 400kg, is dissolved in 2m350 DEG C of industrial hot water in, be slow added into
Precipitated in the liquid alkaline of 32% (wt), obtained slurry is filtered with diaphragm filter press, filter cake with liquid-solid ratio for 5:1 ratio with 50 DEG C
Industrial hot water slurrying washing and filters pressing, 4 times repeatedly.Filter cake after being washed with diaphragm filter press to last time carries out physics pressure
It squeezes, squeeze pressure 0.8MPa, the NaNO of filter cake and 400kg3After mixing, the concentrated nitric acid 500kg of 98% (wt) is added, to
Mixture all after dissolution, adjusts the concentration of Zr (Hf) ion to 1mol/L with industry water.Extraction stoste obtained is transparent,
For TBP extracting and separating zirconium and when hafnium, anti-stripping agent be meet nuclear leve standard without hafnium zirconium nitrate solution, extracting extraction raffinate is to meet
Nuclear leve standard without zirconium hafnium nitrate solution.
Claims (10)
1. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium, it is characterised in that: including following
Step:
Step 1: precipitating
1.1, by ZrOCl2·8H2O is dissolved in 40~60 DEG C of hot water in the ratio of liquid-solid ratio 3:1~5:1mL/g；Liquid-solid ratio
Meaning is liquid volume: solid weight；
1.2, the product for obtaining step 1.1, which is added in the NaOH aqueous solution that mass concentration is 20~32%, carries out precipitating and old
Change, obtains slurry；
Step 2: filtering and washing removing chloride
2.1, slurry is filtered with diaphragm filter press, obtains filter cake；
It detects filtrate and detects CL?Content, CL?Continue when > 100mg/L in next step, CL?Step 3 is gone to when≤100mg/L；
2.2, the filter cake that step 2.1 is obtained by filtration is added in the hot water that temperature is 40~60 DEG C, and slurry is made in slurrying stirring
Material；
Step 2.1 and step 2.2 are repeated, slurrying is filtered repeatedly, until detecting CL in filtrate?≤100mg/L；
Step 3: squeezing purging
3.1, the filter cake for eliminating chloride ion for obtaining step 2 is further squeezed with diaphragm filter press；
3.2, compressed air purging, remaining filtrate in blowing materail tube, diaphragm filter press are used after squeezing；
Step 4: dispersion mixing
4.1, the filter cake Weighing for obtaining step 3 analyzes wherein Zr content；
4.2, dissolution kettle is put into, is crushed dispersion under stirring；
4.3, granular NaNO is put into the material after broken dispersion3Solid is uniformly mixed；
Mixed proportion is Zr:NaNO3Mass ratio be 1:3~1:4；
Step 5: nitric acid dissolves
Under the action of stirring, into the uniformly mixed material that step 4 obtains, the concentrated nitric acid that mass concentration is 98% is added
To being completely dissolved, the mass ratio of concentrated nitric acid and mixture is 1:2.5~1:3；
Step 6: constant volume degree of thickening
Into the dissolved liquid material that step 5 obtains, be added industry water adjust Zr ion concentration in solution to 60~
91g/L；
Step 7: filtering
The liquid material that step 6 is obtained, is filtered with bag type filtering machine, obtains the high selection for TBP extracting and separating zirconium and hafnium
Property extraction stoste.
2. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in step 1.2, precipitation temperature is room temperature, and precipitating endpoint pH is 8~9, and the precipitation reaction time is 60~90min,
Ageing time is 40~60min.
3. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in step 2.1, the filter pressure control of diaphragm filter press is 0.4~0.6MPa.
4. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in step 2.2,20~30min is stirred in slurrying.
5. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in step 2.2, the ratio of filter cake and hot water is liquid-solid ratio 3:1~5:1.
6. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
It is characterized in that: in step 3.1, squeeze pressure 0.8MPa.
7. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in step 3.1, the squeezing time is 15~20min.
8. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
It is characterized in that: in step 3.2, the compressed air purging for being 0.6MPa with pressure.
9. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
Be characterized in that: in the 5th step, then 120~150min of dissolution first observes whether solid material is completely dissolved, if being completely dissolved
It then carries out in next step；
Otherwise 70~90 DEG C are warming up to, then extends dissolution time to being completely dissolved.
10. a kind of highly selective extraction stoste preparation method for TBP extracting and separating zirconium and hafnium as described in claim 1,
It is characterized by: precipitation temperature is room temperature in step 1.2, precipitating endpoint pH is 8~9, the precipitation reaction time is 60~
90min, ageing time are 40~60min；
In step 2.1, the filter pressure control of diaphragm filter press is 0.4~0.6MPa；
In step 2.2,20~30min is stirred in slurrying, and the ratio of filter cake and hot water is liquid-solid ratio 3:1~5:1；
In step 3.1, squeeze pressure 0.8MPa, the squeezing time is 15~20min；
In step 3.2, the compressed air purging for being 0.6MPa with pressure；
In 5th step, first dissolution 120~150min, then observe solid material whether be completely dissolved, if being completely dissolved into
Row is in next step；
Otherwise 70~90 DEG C are warming up to, then extends dissolution time to being completely dissolved.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112723413A (en) * | 2020-11-20 | 2021-04-30 | 中核二七二铀业有限责任公司 | Production method of nuclear-grade zirconium dioxide |
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| CN1438335A (en) * | 2002-01-29 | 2003-08-27 | Ati资产公司 | Method for separating hafnium from zirconium |
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| CN112723413A (en) * | 2020-11-20 | 2021-04-30 | 中核二七二铀业有限责任公司 | Production method of nuclear-grade zirconium dioxide |
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