CN109553130A - A method of zr element in recycling zirconium metallurgy solid waste - Google Patents
A method of zr element in recycling zirconium metallurgy solid waste Download PDFInfo
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- CN109553130A CN109553130A CN201811494886.4A CN201811494886A CN109553130A CN 109553130 A CN109553130 A CN 109553130A CN 201811494886 A CN201811494886 A CN 201811494886A CN 109553130 A CN109553130 A CN 109553130A
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- solid waste
- zirconium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G25/00—Compounds of zirconium
- C01G25/04—Halides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
Abstract
The invention discloses a kind of methods of zr element in recycling zirconium metallurgy solid waste, it first will be after below zirconium metallurgy solid waste crushing grinding to 100 mesh, dissolution, filtering, obtain filtrate and filter residue, secondly after filter residue being cleaned and is dried, it carries out being ground to 300 mesh again hereinafter, carrying out chlorination, and pendular ring is followed and cleaned to filtrate obtained into course of dissolution.Method of the invention not only reduces the pollution of the volume of cargo in storage and the solid waste of metallurgy containing zirconium of the solid waste of metallurgy containing zirconium to environment, and this method effectively increases the rate of recovery of zr element by recycling zr element from zirconium metallurgy solid waste；In addition, as filtrate cycle uses, in filtrate, NaCl, KCl saturation, which are precipitated, can be used in purifying crude ZrCl4Process, micro valuable element is progressively enriched in filtrate, can be extracted after reaching a certain concentration.
Description
Technical field
The invention belongs to a kind of methods of zr element in the recycling field of zr element more particularly to recycling zirconium metallurgy solid waste.
Background technique
Zirconium dioxide (ZrO2) chemical property torpescence, it is insoluble in water, hydrochloric acid and dilute sulfuric acid, and there is high-melting-point, high electricity
The property of resistance rate, high refractive index and low thermal coefficient of expansion is important heat-resisting material, ceramic insulating material and ceramic shading
Agent is also the primary raw material manually bored.Metal zirconium (Zr) has good corrosion resistance, and the hardness and intensity of superelevation are main to use
It is added in aerospace, military project, nuclear reaction, atomic energy and metal superhard material, it may also be used for manufacture shellproof steel alloy and reaction
The clad alloy of uranium fuel in heap.
Zirconium chloride (ZrCl4) it is the intermediate raw material for producing zirconium dioxide, metal zirconium.Zirconium chloride is mainly using boiling chlorine
The production of change method technique, and the corresponding chloride of the generations such as zircon and impurity such as iron, titanium, aluminium, silicon is in gaseous form output.Due to
The boiling point of impurity chlorides is different from the sublimation point of zirconium chloride, hafnium tetrachloride, and control condenser temperature recycles lenticular tetrachloro
Change zirconium, makes itself and impurity initial gross separation.
The fluidizing chlorinations chemical equation such as zirconium oxide and impurity:
It recycles zirconium chloride and alkali metal chloride to form the characteristic of low melting point eutectic, is prepared by fluidizing chlorination technique
Thick zirconium chloride continuous-dissolution in molten salt system, low boiling impurity is in fused salt surface evaporation, high-boiling-point impurity iron, aluminium etc. and alkali
Metal ion forms stable double salt and stays in system, and zirconium chloride temperature raising distillation is separated with impurity, and it is higher that purity is made
Refined zirconium tetrachloride.
Zirconium chloride purifies chemical equation:
FeCl3+NaCl/KCl→Na(K)FeCl4
AlCl3+NaCl/KCl→Na(K)AlCl4
ZrCl4+2NaCl/KCl→Na2(K2)ZrCl6
With the progress of purified reaction, the high-boiling-point impurity constituent content in molten salt system is continuously increased, molten salt system
Physico-chemical property high progression causes purified reaction to be difficult to go on smoothly, so needing after purified reaction carries out a period of time to molten
Salt system carries out salt discharge and adds new salt treatment, and about 40% zr element is contained in the abraum salt of discharge.Therefore in metallurgical solid waste
Reason and its comprehensive utilization of resources are zirconium metallurgy industry urgent problems to be solved.
Summary of the invention
Goal of the invention: the object of the present invention is to provide a kind of methods of zr element rate of recovery for improving zirconium metallurgical process.
Technical solution: the method that the present invention recycles zr element in zirconium metallurgy solid waste includes the following steps:
(1) by after below zirconium metallurgy solid waste crushing grinding to 100 mesh, dissolution, filtering obtain filtrate and filter residue；
(2) it after filter residue being cleaned and dried, carries out being ground to 300 mesh again hereinafter, carrying out chlorination, and obtained
The filtrate cycle obtained is into course of dissolution.
Abraum salt composition is complex, and thus the present invention is by being dissolved, and filter residue is mainly ZrO after dissolving2And C,
Further it can be used to chlorination for after filter residue cleaning, dry, grinding on the basis of this；Micro valuable element is being filtered in filtrate simultaneously
It is gradually enriched in liquid cyclic process.
Furtherly, in step (1), the dissolution that uses can be to be water-soluble or sour molten, wherein hydrochloric acid is used when acid is molten, it is dense
Degree≤5mol/L.Preferably, the temperature of dissolution can be 40-80 DEG C, dissolve 0.5-2h.It is molten that acid further preferably can be used, it is molten
The temperature of solution is 55-75 DEG C, dissolves 1-2h.
It further says, in step (2), the drying of use is to react 0.5-2h under the conditions of 95-105 DEG C.The chlorine of use
Change is to react 0.2-1h under the conditions of 900-1000 DEG C.Preferably, chlorination uses boiling chloridizing furnace or Molten salt chlorination furnace.
Furtherly, in step (2), the cleaning solution obtained after filter residue cleaning is recycled in course of dissolution.
The utility model has the advantages that compared with prior art, remarkable advantage of the invention are as follows: this method from high metallurgical solid waste by returning
Zr element is received, not only reduces the pollution of the volume of cargo in storage and the solid waste of metallurgy containing zirconium of the solid waste of metallurgy containing zirconium to environment, and this method has
Effect improves the rate of recovery of zr element；It can be used in mentioning in addition, NaCl, KCl saturation are precipitated as filtrate cycle uses, in filtrate
Pure thick ZrCl4Process, micro valuable element is progressively enriched in filtrate, can be extracted after reaching a certain concentration.
Detailed description of the invention
Fig. 1 is the zirconium metallurgy solid waste phase composition figure that the present invention uses；
Fig. 2 is the water-soluble filter residue cleaning, drying of the present invention treated object phase composition figure；
Fig. 3 is the chemical component figure after the water-soluble filtering washery slag drying and processing of the present invention；
Fig. 4 is the microscopic appearance figure of the water-soluble filter residue cleaning, drying of the present invention treated 3500 times of amplification；
Fig. 5 is the microscopic appearance figure of the water-soluble filter residue cleaning, drying of the present invention treated 1900 times of amplification.
Specific embodiment
Below with reference to embodiment, further details of the technical solution of the present invention.
Embodiment 1
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng as shown in Figure 1.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing the zirconium progress after grinding is water-soluble, 55 DEG C of water solution temperature, water-soluble time 1h；
(4) solution after will be water-soluble is filtered, and filtrate is circularly used for water-soluble process, and filter residue starts the cleaning processing,
Cleaning solution is equally circularly used for water-soluble process；
(5) drying and processing 2h is carried out under the conditions of 105 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 300 mesh or less；
(7) finally the following filter residue of 300 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 950 DEG C.
Composition detection: the filter residue that the present embodiment step (6) are obtained carries out composition detection, the result of acquisition such as Fig. 2 and Fig. 3
It is shown.By Fig. 2 and Fig. 3 it is found that object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3、C、ZrSiO4Deng chemical component is
49.7%Zr-0.36%Hf-0.36%Al-16.9%C-32.67%O.And the pattern of the filter residue is probed into, the knot of acquisition
Fruit is as shown in Figures 4 and 5, and by two figure it is found that filter residue particle size is at 5 μm or so, structure is fluffy, and surface attachment is more thin
Little particle, this filter residue are more advantageous to chlorination recycling.
By the filter residue progress composition detection after above-mentioned chlorination it is found that the hydrotrope in zirconium metallurgy solid waste accounts for 15.6%, filter residue
Middle object phase: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 49.7%Zr-0.4%Hf-
0.4%Al-16.9%C-32.7%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content about 50%, zirconium are metallurgical
The zr element rate of recovery is up to 91.1% in solid waste.
Embodiment 2
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing the zirconium progress after grinding is water-soluble, 75 DEG C of water solution temperature, water-soluble time 1h；
(4) solution is filtered after will be water-soluble, and filtrate is circularly used for water-soluble process, and filter residue starts the cleaning processing, clearly
Washing lotion is equally circularly used for water-soluble process；
(5) drying and processing 2h is carried out under the conditions of 105 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 300 mesh or less；
(7) finally the following filter residue of 300 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 950 DEG C.
Composition detection: the filter residue after above-mentioned chlorination is subjected to content detection it is found that the hydrotrope accounts in zirconium metallurgy solid waste
15.9%, object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 51.2%Zr-
0.5%Hf-0.5%Al-16.5%C-32.1%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content is about
51%.The zr element rate of recovery is up to 91.5% in abraum salt.
Embodiment 3
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing zirconium after grinding is subjected to sour molten, 55 DEG C of sour solubility temperature, acid dissolution time 1h；
(4) the molten rear solution of acid is filtered, filtrate is circularly used for acid dissolution, and filter residue starts the cleaning processing, clearly
Washing lotion is equally circularly used for acid dissolution；
(5) drying and processing 2h is carried out under the conditions of 105 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 300 mesh or less；
(7) finally the following filter residue of 300 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 950 DEG C.
Composition detection: the filter residue after above-mentioned chlorination is subjected to content detection it is found that acid-soluble material accounts in zirconium metallurgy solid waste
21.5%, object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 53.4%Zr-
0.4%Hf-0.6%Al-16.8%C-28.5%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content is about
53%.The zr element rate of recovery is up to 92.1% in abraum salt.
Embodiment 4
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing zirconium after grinding is subjected to sour molten, 75 DEG C of sour solubility temperature, acid dissolution time 1h；
(4) the molten rear solution of acid is filtered, filtrate is circularly used for acid dissolution, and filter residue starts the cleaning processing, clearly
Washing lotion is equally circularly used for acid dissolution；
(5) drying and processing 2h is carried out under the conditions of 105 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 100 mesh or less；
(7) finally the following filter residue of 100 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 950 DEG C.
Composition detection: the filter residue after above-mentioned chlorination is subjected to content detection it is found that the hydrotrope accounts in zirconium metallurgy solid waste
22.3%, object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 54.1%Zr-
0.6%Hf-0.4%Al-17.1%C-27.8%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content is about
54%.The zr element rate of recovery is up to 92.8% in abraum salt.
Embodiment 5
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing zirconium after grinding is subjected to sour molten, 40 DEG C of sour solubility temperature, acid dissolution time 2h；
(4) the molten rear solution of acid is filtered, filtrate is circularly used for acid dissolution, and filter residue starts the cleaning processing, clearly
Washing lotion is equally circularly used for acid dissolution；
(5) drying and processing 1h is carried out under the conditions of 100 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 300 mesh or less；
(7) finally the following filter residue of 300 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 900 DEG C.
Composition detection: the filter residue after above-mentioned chlorination is subjected to content detection it is found that the hydrotrope accounts in zirconium metallurgy solid waste
22.5%, object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 54.2%Zr-
0.5%Hf-0.5%Al-17.3%C-27.6%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content is about
54%.The zr element rate of recovery is up to 92.5% in abraum salt.
Embodiment 6
The zirconium metallurgy solid waste ingredient used in the examples are as follows: 36.2%Zr-0.25%Hf-1.4%Na-3.1%K-
1.0%Al-21.2%C-23.5%O-12.8%Cl, object mutually have: ZrO2、ZrSiO4、ZrCl2、SiO2、HfO2、Al2O3、Fe3
(CO)12、C、C60、K3C60Deng.
The method that the present invention recycles zr element from zirconium metallurgy solid waste includes the following steps:
(1) the bulk solid waste of metallurgy containing zirconium is crushed；
(2) the broken solid waste of metallurgy containing zirconium is ground, is ground to 100 mesh or less；
(3) solid waste of metallurgy containing zirconium after grinding is subjected to sour molten, 80 DEG C of sour solubility temperature, acid dissolution time 0.5h；
(4) the molten rear solution of acid is filtered, filtrate is circularly used for acid dissolution, and filter residue starts the cleaning processing, clearly
Washing lotion is equally circularly used for acid dissolution；
(5) drying and processing 0.5h is carried out under the conditions of 95 DEG C after filter residue cleaning；
(6) filter residue after drying and processing is regrind, is ground to 300 mesh or less；
(7) finally the following filter residue of 300 mesh is sent to chlorination furnace, chlorination 0.5h under the conditions of 1000 DEG C.
Composition detection: the filter residue after above-mentioned chlorination is subjected to content detection it is found that the hydrotrope accounts in zirconium metallurgy solid waste
22.8%, object phase in filter residue: ZrO2、SiO2、HfO2、Al2O3, C etc., with ZrO2, based on C；Filter residue chemical component: 54.9%Zr-
0.5%Hf-0.5%Al-17.0%C-27.2%O, wherein Zr, C, O tri- kinds of element accountings about 100%, Zr constituent content is about
55%.The zr element rate of recovery is up to 92.9% in abraum salt.
Claims (8)
1. a kind of method of zr element in recycling zirconium metallurgy solid waste, it is characterised in that include the following steps:
(1) by after below zirconium metallurgy solid waste crushing grinding to 100 mesh, dissolution, filtering obtain filtrate and filter residue；
(2) it after filter residue being cleaned and dried, carries out being ground to 300 mesh again hereinafter, carry out chlorination, and it is obtained
Filtrate cycle is into course of dissolution.
2. the method for zr element in recycling zirconium metallurgy solid waste according to claim 1, it is characterised in that: in step (1), institute
The temperature for stating dissolution is 40-80 DEG C, dissolves 0.5-2h.
3. the method for zr element in recycling zirconium metallurgy solid waste according to claim 1, it is characterised in that: in step (1), institute
State be dissolved as it is water-soluble or sour molten, wherein acid it is molten when use hydrochloric acid, concentration≤5mol/L.
4. the method for zr element in recycling zirconium metallurgy solid waste according to claim 3, it is characterised in that: described to be dissolved as acid
Molten, the temperature of dissolution is 55-75 DEG C, dissolves 1-2h.
5. the method for zr element in recycling zirconium metallurgy solid waste according to claim 1, it is characterised in that: in step (2), institute
Stating drying is to react 0.5-2h under the conditions of 95-105 DEG C.
6. the method for zr element in recycling zirconium metallurgy solid waste according to claim 1, it is characterised in that: in step (2), institute
Stating chlorination is to react 0.2-1h under the conditions of 900-1000 DEG C.
7. the method for zr element in recycling zirconium metallurgy solid waste according to claim 6, it is characterised in that: the chlorination uses
Boiling chloridizing furnace or Molten salt chlorination furnace.
8. the method for zr element in recycling zirconium metallurgy solid waste according to claim 1, it is characterised in that: in step (2), institute
The cleaning solution obtained after filter residue cleaning is stated to be recycled in the course of dissolution of step (1).
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| CN108275720A (en) * | 2018-01-26 | 2018-07-13 | 江西晶安新资源有限公司 | A kind of method that zirconium oxychloride white residue takes off zirconium |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006036576A (en) * | 2004-07-26 | 2006-02-09 | Daiichi Kigensokagaku Kogyo Co Ltd | Zirconia-based porous body and its production method |
| CN1803601A (en) * | 2006-01-06 | 2006-07-19 | 宜兴新兴锆业有限公司 | Preparation of white carbon black by silica residue zirconium |
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| CN102628104A (en) * | 2012-05-11 | 2012-08-08 | 冯会壮 | Production process for extracting high-purity rare earth and zirconium compound from solid waste |
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Application publication date: 20190402 |