CN102925695A - Method for leaching nickel (Ni) and cobalt (Co) from waste high-temperature alloy material - Google Patents
Method for leaching nickel (Ni) and cobalt (Co) from waste high-temperature alloy material Download PDFInfo
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- CN102925695A CN102925695A CN2012104023855A CN201210402385A CN102925695A CN 102925695 A CN102925695 A CN 102925695A CN 2012104023855 A CN2012104023855 A CN 2012104023855A CN 201210402385 A CN201210402385 A CN 201210402385A CN 102925695 A CN102925695 A CN 102925695A
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Abstract
The invention discloses a method for leaching nickel (Ni) and cobalt (Co) from a waste high-temperature alloy material. The method comprises the following steps of: smelting the waste high-temperature alloy material containing the Ni and Co in an intermediate frequency furnace, performing powder spraying to prepare alloy powder, performing ball milling on the alloy powder, and selectively leaching the Ni and Co in the alloy material by using dilute acid to obtain a solution rich in the Ni and Co. The method has the advantages of simple process, low leaching temperature and energy consumption, high Ni and Co leaching rate, environment friendliness, simple subsequent treatment process and the like; the content of metallic Ni in filter residue is less than 7 mass percent, and the content of Co in the filter residue is less than 1 mass percent; the content of Ni in filtrate is more than 10 g/L, the content of Co in the filtrate is more than 1g/L; and the Ni and Co leaching rates are respectively over 98.0 percent. By the method, the Ni and Co in the waste high-temperature alloy material can be effectively leached, a phenomenon that harmful gas is discharged is avoided; by the filter residue, high-temperature metals such as tungsten, molybdenum, rhenium, niobium and zirconium in the waste high-temperature alloy material can be further recycled; the environment is not polluted in the whole process; and the method is environment-friendly and low in cost.
Description
Technical field
The invention belongs to the nonferrous metallurgy field, relate to the method that a kind of nickel cobalt leaches.Particularly relate to a kind of from waste and old superalloy material the method for leaching nickel cobalt.
Background technology
The method of leaching nickel cobalt mainly contains following several in the present waste and old superalloy: the chloride solution electrochemical dissolution is processed, hot acid soaks molten, air blast acidleach, electrochemical dissolution, pressurized acid leaching or chlorine soaks, sulfuric acid and nitric acid nitration mixture chemical dissolution etc.
Hou Xiaochuan discloses the experimental study of leaching nickel and cobalt from useless high temperature nickel cobalt-base alloy in " hydrometallurgy " the 3rd phase of the 28th volume in 2009, adopts chlorine leaching nickel, cobalt, iron, wherein additive Fe
2+Improved leaching rate and improved chlorine utilization, accelerated reaction process, the average turnover rate of nickel, cobalt reaches respectively 99.30% and 97.67%, and in the leached mud, nickel, cobalt massfraction are respectively 0.51% and 0.44%.
Tan Shixiong has reported that in " chemical industry metallurgical " the 3rd phase of the 21st volume in 2000 the employing hot acid soaks the nickel cobalt in the molten method leaching superalloy, wherein Ni contains 13.04%, Co contains 40.1%, behind 5mol/L hydrochloric acid boiling soak, Ni contains 9.6g/L in the leach liquor, Co contains 19.11g/L, and leaching effect is very good.
Cai passes and calculate the comprehensive utilization reported the cobalt superalloy in " China YouSe Acta Metallurgica Sinica ", and it adopts the method for air blast acidleach to leach nickel, cobalt in the superalloy.The test conditions temperature 70 C, liquid-solid ratio 10mL/g, blast volume 0.9m3/h, pressure of blast 300kPa, stirring velocity 90r/min, the once turnover rate that the leaching yield of Co is 91.4%, Ni is 81%, and the method has reduced sour consumption, reduced the consumption of the material of follow-up test, be conducive to reduce the amount of slag and the loss of cobalt and nickel, economical rationality, environmental friendliness.
Liu Song has set forth nickel cobalt in the method leaching nickel based high-temperature alloy that adopts electrochemical dissolution (Ni has contained 70% " inorganic chemicals industry " 1997 the 2nd is interim, Co contains 5%), take alloy as anode, copper sheet is negative electrode, adopt the YJ63 D.C. regulated power supply to carry out electrochemical dissolution, electrolytic solution adopts hydrochloric acid system, and concentration is 4mol/L, current density 1000A/m
2, lysate forms Ni 60g/L, Co4.3g/L, and do contrast with the chemical dissolution of nitric acid and chlorine nitration mixture, and chemical consumption is few, pollutes fewly, does not have waste gas to produce, and process costs is low.
The people such as Li Changsheng have applied for a kind of patent (application number: 201110384265.2): place copper-bath to dissolve superalloy first that reclaims the iron-cobalt-nickel metal product from high-temperature alloy waste material, temperature is controlled at 70-85 ℃, pH is controlled at 0.5-1, stir with driven stirring rod, accelerate the reaction of alloy and copper-bath.After reaction finished, adding the ammoniacal liquor regulator solution was weakly alkaline, then adds oxalic acid, obtains oxalate precipitation, can obtain metal through high temperature pyrolysis, and copper is intermediate product in this process, can recycle, can save cost.
The method of leaching nickel cobalt is varied from waste and old superalloy material at present, and the present invention has the characteristics such as technique is simple, adaptability to raw material strong, nickel cobalt leaching yield is high, and environmental pollution is few.
Summary of the invention
The purpose of this invention is to provide a kind of from waste and old superalloy the method for leaching nickel cobalt.Technical problem to be solved by this invention is that the surplus or excess alloy material is carried out leaching behind the mechanical activation.Its characterization step is as follows:
1. raw material adopts the intermediate frequency furnace fusing;
2. adopt atomizing to dust after the fusing;
3. powdered alloy adopts mechanical activation;
4. the powdered alloy after the activation adopts the diluted acid selectivity to leach the nickel cobalt,
The concrete steps feature is: 1. waste and old superalloy raw material is put into intermediate frequency furnace and melt; 2. place water atomization equipment to dust the surplus or excess alloy melt, make powdered alloy; 3. carry out mechanical activation, alloy material is put into ball mill carry out ball milling; 4. selectivity leaches the nickel cobalt in the alloy material, filters, and washs, and obtains the solution of rich nickel and cobalt containing.
Step 1. described waste and old superalloy material is aerospace numbers of hot-side engine critical material, contains the metallic elements such as nickel, chromium, cobalt, molybdenum, aluminium, iron, tantalum, niobium, tungsten, rhenium, ruthenium and zirconium, and wherein nickel contains about 50 ~ 70%, and cobalt contains about 10 ~ 18%.
Step is described dusting for adopting water atomization equipment to dust 2..
Step 3. described mechanical activation is conventional ball milling.
Step 4. described waste and old superalloy material selectivity leach acid that the nickel cobalt adopts be in sulfuric acid, hydrochloric acid, the nitric acid one or more, consumption is 10 ~ 30 times of weight alloy ratio.
The material that the present invention uses contains the waste and old superalloy of nickel cobalt as higher-grade, Ni content is 50 ~ 70%, and cobalt contents is 5 ~ 10%.
The present invention leaches the acid used and is in the components such as hydrochloric acid, sulfuric acid, nitric acid one or more, and consumption is 10 ~ 30 times of weight alloy ratio.The present invention leaches the nickel cobalt by melting-dust-mechanical activation-diluted acid selectivity, the technical indicator of acquisition:
(1) Ni content＜7% in the filter residue, Co content＜1%(mass percent);
(2) leaching yield of Ni greater than the leaching yield of 98%, Co greater than 98%;
(3) Ni content in the filtrate〉10g/L, Co content〉1g/L.
Advantage of the present invention mainly is: have that technique is simple, temperature of reaction is low, energy consumption is low, the leaching yield of Ni and Co is high, advantages of environment protection.Adopt the inventive method, can effectively leach Ni and Co in the waste and old superalloy, selectivity leaches reaction and carries out in reactor, discharge without harmful exhaust, filter residue can be used as the raw material usefulness that tungsten, molybdenum, rhenium etc. are reclaimed in the back, whole process environmentally safe, for a kind of environmental friendliness, efficiently, cheaply from the method for waste and old superalloy leaching nickel cobalt.
Description of drawings
Accompanying drawing is process flow diagram of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments the present invention is described in further detail.
Embodiment 1, and referring to accompanying drawing, experiment takes by weighing alloy material 5000g(and contains Ni67.12%, Co14.01%), place ball mill to carry out mechanical activation, then time 3.5h adds sulfuric acid 650mL, concentration 50%, reaction times 10h, stirring velocity 400 r/min, 100 ℃ of temperature, washing was five times after reaction finished, each water 300mL, the amount of filtrate volume, the slag dry for standby is through leaching, filter and washing, obtain the enrichment solution of Ni and Co, the leaching yield 98.23% of Ni, the leaching yield 98.76% of Co.
Embodiment 2, and referring to accompanying drawing, experiment takes by weighing alloy material 6000g(and contains Ni62.07%, Co12.48%), place ball mill to carry out mechanical activation, then time 5.0h adds sulfuric acid 550mL, concentration 45%, reaction times 15h, stirring velocity 450 r/min, 100 ℃ of temperature, washing was five times after reaction finished, each water 300mL, the amount of filtrate volume, the slag dry for standby is through leaching, filter and washing, obtain the enrichment solution of Ni and Co, the leaching yield 98.82% of Ni, the leaching yield 99.02% of Co.
Embodiment 3, and referring to accompanying drawing, experiment takes by weighing alloy material 8000g(and contains Ni58.47%, Co10.97%), place ball mill to carry out mechanical activation, then time 7.5h adds sulfuric acid 650mL, concentration 50%, reaction times 10h, stirring velocity 350 r/min, 90 ℃ of temperature, washing was five times after reaction finished, each water 300mL, the amount of filtrate volume, the slag dry for standby is through leaching, filter and washing, obtain the enrichment solution of Ni and Co, the leaching yield 98.43% of Ni, the leaching yield 98.86% of Co.
Embodiment 4, and referring to accompanying drawing, experimental amount alloy material 3000g(contains Ni59.44%, Co11.56%), place ball mill to carry out mechanical activation, then time 6.5h adds sulfuric acid 600mL, concentration 35%, reaction times 15h, stirring velocity 400 r/min, 80 ℃ of temperature, washing was five times after reaction finished, each water 300mL, the amount of filtrate volume, the slag dry for standby is through leaching, filter and washing, obtain the enrichment solution of Ni and Co, the leaching yield 98.03% of Ni, the leaching yield 98.16% of Co.
Embodiment 5, and referring to accompanying drawing, experimental amount alloy material 7000g(contains Ni55.59%, Co13.68%), place ball mill to carry out mechanical activation, then time 9.5h adds sulfuric acid 650mL, concentration 45%, reaction times 12h, stirring velocity 400 r/min, 100 ℃ of temperature, washing was five times after reaction finished, each water 300mL, the amount of filtrate volume, the slag dry for standby is through leaching, filter and washing, obtain the enrichment solution of Ni and Co, the leaching yield 99.03% of Ni, the leaching yield 99.12% of Co.
Claims (5)
1. the method for a leaching nickel cobalt from waste and old high-temperature alloy waste material, its characterization step is as follows:
1. raw material adopts the intermediate frequency furnace fusing;
2. adopt atomizing to dust after the fusing;
3. powdered alloy adopts mechanical activation;
4. the powdered alloy after the activation adopts the diluted acid selectivity to leach the nickel cobalt,
Concrete steps are: 1. waste and old superalloy raw material is put into intermediate frequency furnace and melt; 2. place water atomization equipment to dust the surplus or excess alloy melt, make powdered alloy; 3. carry out mechanical activation, alloy material is put into ball mill carry out ball milling; 4. selectivity leaches the nickel cobalt in the alloy material, filters, and washs, and obtains the solution of rich nickel and cobalt containing.
According to claim 1 a kind of from waste and old superalloy the method for leaching nickel cobalt, it is characterized in that step 1. described waste and old superalloy material be aerospace numbers of hot-side engine critical material, contain nickel, chromium, cobalt, molybdenum, aluminium, iron, tantalum, niobium, tungsten, rhenium, ruthenium and zirconium metallic element, wherein nickel contains about 50 ~ 70%, and cobalt contains about 10 ~ 18%.
According to claim 1 a kind of from waste and old superalloy material the method for leaching nickel cobalt, it is characterized in that step 2. described dusting adopt water atomization equipment to dust.
According to claim 1 a kind of from waste and old superalloy material the method for leaching nickel cobalt, it is characterized in that step 3. described mechanical activation be conventional ball milling.
According to claim 1 a kind of from waste and old superalloy the method for leaching nickel cobalt, it is characterized in that step 4. described waste and old superalloy material selectivity leach acid that the nickel cobalt adopts be in sulfuric acid, hydrochloric acid, the nitric acid one or more, consumption is 10 ~ 30 times of weight alloy ratio.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131859A (en) * | 2013-03-06 | 2013-06-05 | 昆明理工大学 | Comprehensive recycling method for metals in superalloy scrap |
| CN103334017A (en) * | 2013-07-01 | 2013-10-02 | 贵研铂业股份有限公司 | Method for preparing high-purity nickel powder from waste high-temperature alloy |
| CN103436721A (en) * | 2013-07-08 | 2013-12-11 | 贵研铂业股份有限公司 | Preparation method for ammonium rhenate from waste high temperature alloy enriched material |
| CN104651620A (en) * | 2015-03-20 | 2015-05-27 | 西安瑞鑫科金属材料有限责任公司 | Method for regenerating high-purity nickel sulfate from nickel-based alloy waste material |
| CN106282566A (en) * | 2015-05-27 | 2017-01-04 | 云南锡业集团有限责任公司研究设计院 | A kind of method of the tungsten cobalt waste residue cobalt carbonate of iron content |
| CN109913667A (en) * | 2019-03-20 | 2019-06-21 | 东北大学 | A method of the Call Provision from nickel base superalloy waste cut materials |
| CN110257630A (en) * | 2019-05-31 | 2019-09-20 | 荆门德威格林美钨资源循环利用有限公司 | A method of from mentioning synthetical recovery cobalt nickel in tungsten waste material |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
| CN111334666A (en) * | 2020-03-31 | 2020-06-26 | 中国科学院金属研究所 | Method for comprehensively utilizing valuable elements in ultrasonic leaching high-temperature alloy waste |
| CN111410240A (en) * | 2020-03-31 | 2020-07-14 | 中国科学院金属研究所 | Method for preparing nickel-cobalt hydroxide battery grade raw material by using high-temperature alloy waste |
| CN111575502A (en) * | 2019-02-19 | 2020-08-25 | 中国科学院过程工程研究所 | Method for extracting nickel element from nickel ore |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103131859A (en) * | 2013-03-06 | 2013-06-05 | 昆明理工大学 | Comprehensive recycling method for metals in superalloy scrap |
| CN103334017A (en) * | 2013-07-01 | 2013-10-02 | 贵研铂业股份有限公司 | Method for preparing high-purity nickel powder from waste high-temperature alloy |
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| CN104651620A (en) * | 2015-03-20 | 2015-05-27 | 西安瑞鑫科金属材料有限责任公司 | Method for regenerating high-purity nickel sulfate from nickel-based alloy waste material |
| CN106282566A (en) * | 2015-05-27 | 2017-01-04 | 云南锡业集团有限责任公司研究设计院 | A kind of method of the tungsten cobalt waste residue cobalt carbonate of iron content |
| CN106282566B (en) * | 2015-05-27 | 2020-01-21 | 云南锡业集团有限责任公司研究设计院 | Method for preparing cobalt carbonate from iron-containing tungsten-cobalt waste residue |
| CN111575502A (en) * | 2019-02-19 | 2020-08-25 | 中国科学院过程工程研究所 | Method for extracting nickel element from nickel ore |
| CN109913667A (en) * | 2019-03-20 | 2019-06-21 | 东北大学 | A method of the Call Provision from nickel base superalloy waste cut materials |
| CN110257630A (en) * | 2019-05-31 | 2019-09-20 | 荆门德威格林美钨资源循环利用有限公司 | A method of from mentioning synthetical recovery cobalt nickel in tungsten waste material |
| CN110616330A (en) * | 2019-09-30 | 2019-12-27 | 江苏奇纳新材料科技有限公司 | Method for recovering rare and noble metals in rhenium-containing high-temperature alloy waste |
| CN111334666A (en) * | 2020-03-31 | 2020-06-26 | 中国科学院金属研究所 | Method for comprehensively utilizing valuable elements in ultrasonic leaching high-temperature alloy waste |
| CN111410240A (en) * | 2020-03-31 | 2020-07-14 | 中国科学院金属研究所 | Method for preparing nickel-cobalt hydroxide battery grade raw material by using high-temperature alloy waste |
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