CN109536718A - A method of zr element in recycling abraum salt containing zirconium monochloride - Google Patents
A method of zr element in recycling abraum salt containing zirconium monochloride Download PDFInfo
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- CN109536718A CN109536718A CN201811494887.9A CN201811494887A CN109536718A CN 109536718 A CN109536718 A CN 109536718A CN 201811494887 A CN201811494887 A CN 201811494887A CN 109536718 A CN109536718 A CN 109536718A
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- Prior art keywords
- abraum salt
- containing zirconium
- salt containing
- zirconium monochloride
- roasting
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/002—Dry processes by treating with halogens, sulfur or compounds thereof; by carburising, by treating with hydrogen (hydriding)
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/08—Chloridising roasting
-
- 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
-
- 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 discloses a kind of methods of zr element in recycling abraum salt containing zirconium monochloride to roast 0.5-2h after the abraum salt containing zirconium monochloride is broken, grinding, drying under the conditions of 400-600 DEG C, regrind and carry out chlorination.The method of the present invention not only reduces the volume of cargo in storage of the abraum salt containing zirconium monochloride and the pollution to environment by recycling zr element from abraum salt containing zirconium monochloride, economic and environment-friendly, and this method effectively increases the rate of recovery of zr element.
Description
Technical field
The invention belongs to a kind of sides of zr element in the recycling field of zr element more particularly to recycling abraum salt containing zirconium monochloride
Method.
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, about 40% zr element is contained in the abraum salt of discharge, therefore useless containing zirconium monochloride
Salt treatment 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:
By containing zirconium monochloride abraum salt crushing grinding, after drying, 0.5-2h is roasted under the conditions of 400-600 DEG C, is ground again
It grinds and carries out chlorination.
After the present invention is roasted by will contain zirconium monochloride abraum salt, overwhelming majority effumabilities in abraum salt containing zirconium monochloride
Substance has volatilized, and zr element grade is further promoted in product of roasting, and product of roasting is main are as follows: ZrO2、ZrCl2、HfO2、SiO2、
Al2O3。
Preferably, the temperature of roasting can be 510-600 DEG C, roast 0.5-1h.
It furtherly, is to be ground to 100 mesh or less by the abraum salt initial integral method grinding containing zirconium monochloride.Regrinding is to grind
It is milled to 300 mesh or less.
Furtherly, drying is to react 0.5-2h under the conditions of 95-105 DEG C.Chlorination is under the conditions of 900-1000 DEG C
React 0.2-1h.Preferably, chlorination uses boiling chloridizing furnace.
The utility model has the advantages that compared with prior art, remarkable advantage of the invention are as follows: this method is by from abraum salt containing zirconium monochloride
Middle recycling zr element not only reduces the pollution of the volume of cargo in storage and abraum salt containing zirconium monochloride of the abraum salt containing zirconium monochloride to environment, warp
Ji environmental protection, and this method effectively increases the rate of recovery of zr element.
Detailed description of the invention
Fig. 1 is the product of roasting phase structure figure that the different maturing temperature of the present invention obtains；
Fig. 2 is the product of roasting microscopic appearance figure of 480 DEG C of maturing temperature of the present invention acquisitions；
Fig. 3 is the product of roasting microscopic appearance figure of 510 DEG C of maturing temperature of the present invention acquisitions；
Fig. 4 is the product of roasting microscopic appearance figure of 540 DEG C of maturing temperature of the present invention acquisitions；
Fig. 5 is the product of roasting microscopic appearance figure of 570 DEG C of maturing temperature of the present invention acquisitions；
Fig. 6 is the product of roasting microscopic appearance figure of 600 DEG C of maturing temperature of the present invention acquisitions；
Fig. 7 is influence diagram of the different maturing temperature of the present invention to chloride abraum salt weight-loss ratio.
Specific embodiment
Below with reference to embodiment, further details of the technical solution of the present invention.
Embodiment 1
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 100 DEG C, drying time 1h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 480 DEG C of maturing temperature, calcining time 0.5h, roasting is made
Burn product；
(5) product of roasting is ground again, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is sent to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 27.24%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 480 DEG C of -0.5h, it is useless containing zirconium monochloride
Most volatile substances have volatilized in salt, and zr element grade is further promoted to 57.5%.
Embodiment 2
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 100 DEG C, drying time 1h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 510 DEG C of maturing temperature, calcining time 0.5h, roasting is made
Burn product；
(5) product of roasting is ground again, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is sent to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 27.85%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 510 DEG C of -0.5h, it is useless containing zirconium monochloride
Most volatile substances have volatilized in salt, and zr element grade is further promoted to 57.9%.
Embodiment 3
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 100 DEG C, drying time 1h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 540 DEG C of maturing temperature, calcining time 0.5h, roasting is made
Burn product；
(5) product of roasting is subjected to secondary grinding, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is back to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 28.08%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 510 DEG C of -0.5h, it is useless containing zirconium monochloride
Most volatile substances have volatilized in salt, and zr element grade is further promoted to 58.1%.
Embodiment 4
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 100 DEG C, drying time 1h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 570 DEG C of maturing temperature, calcining time 0.5h, roasting is made
Burn product；
(5) product of roasting is subjected to secondary grinding, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is back to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 28.56%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 570 DEG C of -0.5h, it is useless containing zirconium monochloride
Most volatile substances have volatilized in salt, and zr element grade is further promoted to 57.9%.
Embodiment 5
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 100 DEG C, drying time 1h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 600 DEG C of maturing temperature, calcining time 0.5h, roasting is made
Burn product；
(5) product of roasting is subjected to secondary grinding, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is back to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 29.25%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when illustrating roasting condition is 600 DEG C of -0.5h, chlorination containing zirconium
Most volatile substances have volatilized in object abraum salt, and zr element grade is further promoted to 58.5%.
The product of roasting of above-mentioned preparation is subjected to phase structure characterization and microscopic appearance characterization, the result of acquisition such as Fig. 1 is extremely
Shown in Fig. 6.As shown in Figure 1, product of roasting object phase composition is essentially identical under different maturing temperatures, are as follows: ZrO2、ZrCl2、HfO2、
SiO2、Al2O3；By Fig. 2 to Fig. 6 it is found that product of roasting structure is fluffy, 10 μm of size is hereinafter, there is part agglomeration.Meanwhile
Abraum salt weight-loss ratio to embodiment 1 to 5 is studied, the result of acquisition is as shown in fig. 7, by the figure it is found that with roasting
The raising of temperature, abraum salt weight-loss ratio are promoted, but it is little to promote amplitude.
Embodiment 6
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 95 DEG C, drying time 2h, and roasting is made
Burn product；
(4) abraum salt containing zirconium monochloride after drying is roasted, 450 DEG C of maturing temperature, calcining time 1h；
(5) product of roasting is ground again, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is sent to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 26.5%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 450 DEG C of -1h, abraum salt containing zirconium monochloride
Middle overwhelming majority volatile substances have volatilized, and zr element grade is further promoted to 56.2%.
Embodiment 7
The chloride abraum salt 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.
The method that the present invention recycles zr element in abraum salt containing zirconium monochloride includes the following steps:
(1) bulk abraum salt containing zirconium monochloride is crushed；
(2) broken abraum salt containing zirconium monochloride is ground, is ground to 100 mesh or less；
(3) abraum salt containing zirconium monochloride after grinding is dried, drying temperature is 105 DEG C, drying time 0.5h；
(4) abraum salt containing zirconium monochloride after drying is roasted, 400 DEG C of maturing temperature, calcining time 2h, roasting is made
Product；
(5) product of roasting is ground again, is ground to 300 mesh or less；
(6) the following product of roasting of 300 mesh is sent to boiling chloridizing furnace and carries out chlorination.
Composition detection: the present invention roasting process mass loss of abraum salt containing zirconium monochloride is 22.31%, the main object of product of roasting
Phase are as follows: ZrO2、ZrCl2、HfO2、SiO2、Al2O3.It follows that when roasting condition is 400 DEG C of -2h, abraum salt containing zirconium monochloride
Middle overwhelming majority volatile substances have volatilized, and zr element grade is further promoted to 53.1%.
Claims (7)
1. a kind of method of zr element in recycling abraum salt containing zirconium monochloride, it is characterised in that include the following steps: that zirconium chlorination will be contained
Object abraum salt is broken, grinds, after drying, roasts 0.5-2h under the conditions of 400-600 DEG C, regrinds and carry out chlorination.
2. the method for zr element in recycling abraum salt containing zirconium monochloride according to claim 1, it is characterised in that: the roasting
Temperature be 510-600 DEG C, roast 0.5-1h.
3. the method for zr element in recycling abraum salt containing zirconium monochloride according to claim 1, it is characterised in that: described to contain
Zirconium monochloride abraum salt crushing grinding is to be ground to 100 mesh or less.
4. it is according to claim 1 recycling abraum salt containing zirconium monochloride in zr element method, it is characterised in that: it is described again
Grinding is to be ground to 300 mesh or less.
5. the method for zr element in recycling abraum salt containing zirconium monochloride according to claim 1, it is characterised in that: the drying
It is to react 0.5-2h under the conditions of 95-105 DEG C.
6. the method for zr element in recycling abraum salt containing zirconium monochloride according to claim 1, it is characterised in that: the chlorination
It is to react 0.2-1h under the conditions of 900-1000 DEG C.
7. the method for zr element in recycling abraum salt containing zirconium monochloride according to claim 6, it is characterised in that: the chlorination
Using boiling chloridizing furnace.
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Citations (6)
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|---|---|---|---|---|
| US5171549A (en) * | 1991-05-22 | 1992-12-15 | Teledyne Wah Chang Albany | Process for decreasing the level of impurities in zirconium chloride, titanium chloride and hafnium chloride |
| CN1087604A (en) * | 1993-09-27 | 1994-06-08 | 广西冶金研究院 | From zircon ore concentrate, prepare high-purity zirconium dioxide |
| CN102602993A (en) * | 2012-04-05 | 2012-07-25 | 北京瑞源化工技术有限公司 | Method for recovering zirconium element from zirconium oxychloride crystallized mother liquor raffinate |
| 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 |
| CN106435221A (en) * | 2016-10-10 | 2017-02-22 | 郭爽 | Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium |
| CN107399761A (en) * | 2017-08-22 | 2017-11-28 | 汉川市石金科技有限公司 | A kind of zirconium oxide waste recovery technique and recovery zirconium powder |
-
2018
- 2018-12-07 CN CN201811494887.9A patent/CN109536718A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5171549A (en) * | 1991-05-22 | 1992-12-15 | Teledyne Wah Chang Albany | Process for decreasing the level of impurities in zirconium chloride, titanium chloride and hafnium chloride |
| CN1087604A (en) * | 1993-09-27 | 1994-06-08 | 广西冶金研究院 | From zircon ore concentrate, prepare high-purity zirconium dioxide |
| CN102602993A (en) * | 2012-04-05 | 2012-07-25 | 北京瑞源化工技术有限公司 | Method for recovering zirconium element from zirconium oxychloride crystallized mother liquor raffinate |
| 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 |
| CN106435221A (en) * | 2016-10-10 | 2017-02-22 | 郭爽 | Method for preparing nuclear-grade sponge zirconium and nuclear-grade sponge hafnium |
| CN107399761A (en) * | 2017-08-22 | 2017-11-28 | 汉川市石金科技有限公司 | A kind of zirconium oxide waste recovery technique and recovery zirconium powder |
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Application publication date: 20190329 |