CN104498718A - Method for treating hard alloy grinding material - Google Patents
Method for treating hard alloy grinding material Download PDFInfo
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- CN104498718A CN104498718A CN201410735235.5A CN201410735235A CN104498718A CN 104498718 A CN104498718 A CN 104498718A CN 201410735235 A CN201410735235 A CN 201410735235A CN 104498718 A CN104498718 A CN 104498718A
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Abstract
The invention relates to a method for treating a waste hard alloy and particularly relates to a method for treating a waste hard alloy grinding material, mainly solving the problems of long nickel-cobalt leaching time, high oxidizing agent consumption, high equipment requirement, long process, high separation difficulty of cobalt and tungsten which are contained in the waste hard alloy grinding material and low purity of an obtained tungsten product in the prior art. The method comprises the following steps of: (a) soda calcination: mixing tungsten carbide filter residues with sodium carbonate and sodium nitrate, and then calcining to obtain a material I; (b) caustic soda leaching: leaching the material I by using liquid caustic soda with [OH-] of 0.5-2.0 mol/l to obtain a sodium tungstate-containing solution and cobalt-nickel-containing filter residues; (c) cobalt-nickel leaching: leaching the cobalt-nickel filter residues by using an acid solution with [H+] of 0.5-2.0 mol/l to obtain a cobalt-nickel-containing solution used for cobalt-nickel recovery; (d) tungsten recovery: adding acid to the sodium tungstate-containing solution to regulate the pH value to 5.0-8.0 to obtain a high-purity tungstic acid precipitate, and washing, drying and calcining to obtain high-purity tungsten trioxide. The method disclosed by the invention can be used for well solving the problems and is worthy of being applied and popularized.
Description
Technical field
The present invention relates to the treatment process of discarded hard alloy, be specifically related to a kind for the treatment of process of discarded hard alloy grinding material.
Background technology
Wimet is mainly made up of tungsten, cobalt etc., along with the widespread use of Wimet and the increase of demand, cause tungsten, cobalt resource in short supply, price increase.In recent years, many countries using the Secondary resource of waste hand alloy material as preciousness, to solve the source of raw material and to reduce the important means of CEMENTED CARBIDE PRODUCTION cost.Therefore reclaim tungsten, cobalt resource is of great immediate significance to developing national economy.
The main method of process Wimet defective material has both at home and abroad at present: SODIUMNITRATE smelting process, zinc melt method, high-temperature oxidation, electro-dissolving etc.Patent 201310003314.2 proposes a kind of recovery and treatment method of scrap hard alloy grinding material, comprise the following steps: a) scrap hard alloy grinding material is mixed with sulphuric acid soln and oxygenant I, filter after reaction, obtain the solution of wolfram varbide filter residue and cobalt-bearing ferronickel; B) roasting after being mixed with sodium carbonate and SODIUMNITRATE by wolfram varbide filter residue, obtains material I; C) material I be impregnated in hot water, obtain the solution containing sodium wolframate; Solution containing sodium wolframate obtains sodium wolframate crystal through concentration and evaporation crystallization; D) solution of cobalt-bearing ferronickel adds oxygenant II under the condition of pH=2-5, after reaction, obtains iron precipitation and the solution containing cobalt nickel; Solution containing cobalt nickel obtains cobalt nickel salt crystal after treatment.The program is simple to equipment requirements, can the various metallic element such as cobalt, tungsten, nickel and iron in synthetical recovery grinding material, and the rate of recovery is high and purity is high, and environmental pollution is little.The problems such as but it is long to there is the extraction times such as cobalt ferronickel, and oxygenant consumption is large.Document CN88105175.6 discloses a kind of method regenerating Footwall drift tungsten, cobalt from waste hand alloy material, the composite technology of use heat process-hydrometallurgy, namely utilize Principles of Heating Processing to carry out oxidation powder process to waste hand alloy material, obtain tungsten cobalt mixed oxide powder; Utilize hydrometallurgical principle, Reduced separating, extraction are carried out to tungsten cobalt mixed oxide powder, obtain powdery pure metal tungsten and cobalt.This technique can obtain the product of cobalt tungsten, but long flow path, and the rate of recovery of cobalt tungsten is not high, is unsuitable for processing the Wimet containing nickel, iron etc. simultaneously.Zhang Qixun proposes the technique of electro-dissolving process Wimet, and this technique is very effective for block Wimet, but it is not high to there is electroconductibility for grinding material Wimet, the shortcomings such as current efficiency is low.Document CN200910043243.2 discloses a kind of process recovery method of hard alloy scraps.It comprises the following steps: hard alloy scraps and weighting agent carbon black load in graphite boat by a., put into carbon tube furnace high-temperature calcination, calcining temperature 1600 ~ 2400 DEG C, calcination time 30 ~ 80 minutes, hydrogen flowing quantity 1.2 ~ 2.6m3/h under hydrogen; B., after the hard alloy scraps after high-temperature calcination being unloaded boat, clean surface, be broken into jaw crusher and roll crusher two sections the alloy granule that granularity is 2 ~ 8mm; C. the alloy granule after fragmentation is carried out ball milling, ratio of grinding media to material (4 ~ 5): 1, Ball-milling Time 8 ~ 16 hours; D. the alloy powder after ball milling is sieved, for traditional processing technology batching after the detection of sieve lower alloy powder is qualified, manufacture Wimet.Reproduce the technique of Wimet after this method proposing high temperature in reducing atmosphere, ball mill mixing, but containing other impurity in grinding material, as abrasive material, sand, iron filings etc., can not Direct Regeneration be carried out.Document CN200510012779.X discloses a kind of method extracting rare metal from scrap hard alloy.Its technique comprises the following steps: scrap hard alloy through broken, clay into power, calcine, react with sodium hydroxide solution, sodium tungstate solution acquired by utilization adds sulfuric acid and ammoniacal liquor generates ammonium tungstate solution through extraction and back-extraction, add hydrogen reducing become metal tungsten powder through heating evaporation, crystallization, oven dry, again calcining again, and the solids described in utilizing is through extracting cobalt powder, nickel powder, tantalum, niobium with sulfuric acid, ammonium oxalate.Utilize above-mentioned operation tungsten, cobalt metal, metallic nickel and metal tantalum, metal niobium can be extracted from scrap hard alloy.After this method proposing ball milling, alkali roasting, washing, extraction back extraction obtains ammonium tungstate, and residuum is through materials such as acid-soluble precipitation cobalt nickel tantalum niobiums.This process synthesis has reclaimed the various metals in Wimet, but there is the indissociable shortcomings such as alkali roasting is high to equipment requirements, cobalt nickel tantalum niobium.
Summary of the invention
It is long that technical problem to be solved by this invention is that prior art exists nickel cobalt extraction time, and oxygenant consumption is large, and equipment requirements is high, long flow path, in grinding material, cobalt tungsten separating difficulty is large, and the problem that the tungsten product purity obtained is low, provides a kind for the treatment of process of new hard-alloy grinding material.The method nickel cobalt extraction time is short, and oxygenant consumption is little, and equipment requirements is low, and flow process is reasonable, and the separation of cobalt tungsten is simple, and the rate of recovery of tungsten is high.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows: a kind for the treatment of process of hard-alloy grinding material, comprises the following steps:
A) soda roasting: roasting after being mixed with sodium carbonate and SODIUMNITRATE by wolfram varbide filter residue, obtains material I.
B) alkali leaches: leached by material I liquid caustic soda that [OH-] is 0.5-2.0mol/l, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel.
C) cobalt nickel leaches: used by the filter residue containing cobalt nickel the acid solution leaching that [H+] is 0.5-2.0mol/l to obtain containing the solution of cobalt nickel for reclaiming cobalt nickel wherein.
D) recovery of tungsten: the solution containing sodium wolframate is added acid for adjusting pH 5.0-8.0 and obtains high purity tungsten Acid precipitation, obtains high-purity tungstic oxide through washing and drying calcining.
Preferably, described alkali lye is selected from least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, hydrated barta; Described acid solution I is selected from least one in sulfuric acid, hydrochloric acid, nitric acid, perchloric acid; Described acid solution II is selected from least one in hydrochloric acid, nitric acid.
Preferably, the mass ratio of step a) hard-alloy grinding material and sodium carbonate is 1:(0.1-5), maturing temperature is 400-800 DEG C, and roasting time is 1-6 hour.
Preferably, step b) roasting material and liquid caustic soda solid-to-liquid ratio be 1:(0.5-6), alkali leaching temperature is 80-99 DEG C, and the alkali leaching time is 2-8 hour.
Preferably, step c) solid-to-liquid ratio is 1:(2-10), cobalt nickel extraction time is 1-4 hour, and cobalt nickel extraction temperature is 60-90 DEG C.
Preferably, steps d) maturing temperature is 400-800 DEG C, roasting time is 1-6 hour.
The present invention has the following advantages:
1., owing to first passing through roasting, while tungsten oxidation, nickel cobalt is also oxidized, then during leaching nickel cobalt, extraction time shortens greatly, simultaneously the consumption of anaerobic agent
2., owing to being mainly the conventional equipment such as roasting, leaching, avoid some complex apparatus such as electrolyzer, high-energy ball milling equipment.This technique compares other technique, and flow process shortens greatly.
3. achieve thoroughly being separated of tungsten and cobalt nickel by alkali leaching, the tungsten product obtained is high-purity rank, and the purity of tungsten product improves greatly, and the rate of recovery of tungsten can to more than 98.5% simultaneously.
Present method nickel cobalt extraction time is short, and oxygenant consumption is little, and equipment requirements is low, and flow process is reasonable, and the separation of cobalt tungsten is simple, and the rate of recovery of tungsten is high.There is industrialization prospect very much.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated, and scope of the present invention is not by the restriction of these embodiments.
Embodiment 1
Step is as follows:
A) soda roasting: mixed with the mass ratio 1:1 of sodium carbonate by hard-alloy grinding material, maturing temperature is 450 DEG C, and roasting time is 5 hours.
B) alkali leaches: leached by the roasting material sodium hydroxide solution that [OH-] is 1.0mol/l, roasting material and liquid caustic soda solid-to-liquid ratio are 1:3, and alkali leaching temperature is 85 DEG C, and the alkali leaching time is 6 hours, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel.
C) cobalt nickel leaches: gone out by the sulfuric acid immersion that [H+] is 1mol/l by the filter residue containing cobalt nickel, solid-to-liquid ratio is 1:, 5, cobalt nickel extraction time is 3 hours, and cobalt nickel extraction temperature is 85 DEG C.Obtain solution containing cobalt nickel for reclaiming cobalt nickel wherein.
D) recovery of tungsten: the solution containing sodium wolframate is added hydrochloric acid and regulate pH6.5 to obtain high purity tungsten Acid precipitation, through washing and drying calcining, maturing temperature is 550 DEG C, and roasting time is 3 hours, the tungstic oxide purity finally obtained is 99.98%, and the rate of recovery of tungsten is 99.1%.
Embodiment 2
Step is as follows:
A) soda roasting: mixed with the mass ratio 1:2 of sodium carbonate by hard-alloy grinding material, maturing temperature is 450 DEG C, and roasting time is 4 hours.
B) alkali leaches: leached by the roasting material sodium hydroxide solution that [OH-] is 1.0mol/l, roasting material and liquid caustic soda solid-to-liquid ratio are 1:4, and alkali leaching temperature is 80 DEG C, and the alkali leaching time is 6 hours, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel.
C) cobalt nickel leaches: leached with the hydrochloric acid solution that [H+] is 1mol/l by the filter residue containing cobalt nickel, solid-to-liquid ratio is 1:, 5, cobalt nickel extraction time is 2 hours, and cobalt nickel extraction temperature is 80 DEG C.Obtain solution containing cobalt nickel for reclaiming cobalt nickel wherein.
D) recovery of tungsten: the solution containing sodium wolframate is added hydrochloric acid and regulate pH7.5 to obtain high purity tungsten Acid precipitation, through washing and drying calcining, maturing temperature is 500 DEG C, and roasting time is 2.5 hours, the tungstic oxide purity finally obtained is 99.99%, and the rate of recovery of tungsten is 99.2%.
Embodiment 3
Step is as follows:
A) soda roasting: mixed with the mass ratio 1:2.5 of sodium carbonate by hard-alloy grinding material, maturing temperature is 600 DEG C, and roasting time is 4 hours.
B) alkali leaches: leached by the roasting material ammonia soln that [OH-] is 1.0mol/l, roasting material and liquid caustic soda solid-to-liquid ratio are 1:4, and alkali leaching temperature is 80 DEG C, and the alkali leaching time is 6 hours, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel.
C) cobalt nickel leaches: leached with the hydrochloric acid solution that [H+] is 1mol/l by the filter residue containing cobalt nickel, solid-to-liquid ratio is 1:, 5, cobalt nickel extraction time is 2 hours, and cobalt nickel extraction temperature is 80 DEG C.Obtain solution containing cobalt nickel for reclaiming cobalt nickel wherein.
D) recovery of tungsten: the solution containing sodium wolframate is added nitric acid and regulate pH7.5 to obtain high purity tungsten Acid precipitation, through washing and drying calcining, maturing temperature is 600 DEG C, and roasting time is 2.5 hours, the tungstic oxide purity finally obtained is 99.98%, and the rate of recovery of tungsten is 99.3%.
Embodiment 4
Step is as follows:
A) soda roasting: mixed with the mass ratio 1:3 of sodium carbonate by hard-alloy grinding material, maturing temperature is 700 DEG C, and roasting time is 4 hours.
B) alkali leaches: leached by the roasting material potassium hydroxide solution that [OH-] is 1.0mol/l, roasting material and liquid caustic soda solid-to-liquid ratio are 1:3, and alkali leaching temperature is 80 DEG C, and the alkali leaching time is 6 hours, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel.
C) cobalt nickel leaches: leached with the hydrochloric acid solution that [H+] is 1mol/l by the filter residue containing cobalt nickel, solid-to-liquid ratio is 1:, 5, cobalt nickel extraction time is 2 hours, and cobalt nickel extraction temperature is 80 DEG C.Obtain solution containing cobalt nickel for reclaiming cobalt nickel wherein.
D) recovery of tungsten: the solution containing sodium wolframate is added nitric acid and regulate pH7.0 to obtain high purity tungsten Acid precipitation, through washing and drying calcining, maturing temperature is 650 DEG C, and roasting time is 2.5 hours, the tungstic oxide purity finally obtained is 99.98%, and the rate of recovery of tungsten is 99.2%.
Comparative example 1
Other conditions are constant, only mixed with the mass ratio 1:0.05 of sodium carbonate by hard-alloy grinding material in embodiment 1, and the rate of recovery of final tungsten is 76.8%.
Comparative example 2
Other conditions are constant, and only regulate pH4.0 by adding hydrochloric acid in embodiment 2, the purity of the tungstic oxide finally obtained is 98.2%.
Above-described embodiment is the present invention's preferably embodiment; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from spirit of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (6)
1. the treatment process of hard-alloy grinding material, comprises the following steps:
A) soda roasting: roasting after being mixed with sodium carbonate by hard-alloy grinding material, obtains roasting material;
B) alkali leaches: leached by the roasting material liquid caustic soda that [OH-] is 0.5-2.0mol/l, obtains the solution containing sodium wolframate and the filter residue containing cobalt nickel;
C) cobalt nickel leaches: used by the filter residue containing cobalt nickel the acid solution I leaching that [H+] is 0.5-2.0mol/l to obtain containing the solution of cobalt nickel for reclaiming cobalt nickel wherein;
D) recovery of tungsten: the solution containing sodium wolframate is added acid solution II and regulate pH5.0-8.0 to obtain high purity tungsten Acid precipitation, obtain high-purity tungstic oxide through washing and drying calcining.
2. the treatment process of hard-alloy grinding material according to claim 1, is characterized in that described alkali lye is selected from least one in sodium hydroxide, potassium hydroxide, ammoniacal liquor, hydrated barta; Described acid solution I is selected from least one in sulfuric acid, hydrochloric acid, nitric acid, perchloric acid; Described acid solution II is selected from least one in hydrochloric acid, nitric acid.
3. the treatment process of hard-alloy grinding material according to claim 1, in it is characterized in that step is a), the mass ratio of hard-alloy grinding material and sodium carbonate is 1:(0.1-5), maturing temperature is 400-800 DEG C, and roasting time is 1-6 hour.
4. the treatment process of hard-alloy grinding material according to claim 1, is characterized in that step b) in, roasting material and liquid caustic soda solid-to-liquid ratio are 1:(0.5-6), alkali leaching temperature is 80-99 DEG C, and the alkali leaching time is 2 ~ 8 hours.
5. the treatment process of hard-alloy grinding material according to claim 1, is characterized in that step c) in, solid-to-liquid ratio is 1:(2-10), cobalt nickel extraction time is 1-4 hour, and cobalt nickel extraction temperature is 60-90 DEG C.
6. the treatment process of hard-alloy grinding material according to claim 1, is characterized in that steps d) in, maturing temperature is 400-800 DEG C, and roasting time is 1-6 hour.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104942303A (en) * | 2015-07-01 | 2015-09-30 | 崇义章源钨业股份有限公司 | Method for preparing tungsten powder |
| CN105483412A (en) * | 2016-01-27 | 2016-04-13 | 郑州大学 | Method for preparing high-purity tungsten-molybdenum alloy with low-grade tungsten-molybdenum bulk concentrate |
| CN105586491A (en) * | 2016-01-18 | 2016-05-18 | 重庆科技学院 | Comprehensive recycling method for waste hard alloy |
| CN106498172A (en) * | 2016-12-14 | 2017-03-15 | 荆门市格林美新材料有限公司 | Hard-alloy grinding material tungsten-cobalt disperses the recovery method of tungsten in separating |
| CN107792883A (en) * | 2016-08-30 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of high purity reagent tungstic acid |
| CN108220602A (en) * | 2016-12-22 | 2018-06-29 | 荆门德威格林美钨资源循环利用有限公司 | The separation and recovery method of tungsten and titanium in waste hand alloy material |
| CN108728657A (en) * | 2018-07-15 | 2018-11-02 | 安化县众旺钨业有限公司 | A method of recycling tungsten, cobalt, silver, copper and tantalum from hard-alloy grinding waste material |
| CN109536719A (en) * | 2018-12-12 | 2019-03-29 | 株洲金韦硬质合金有限公司 | It is a kind of regenerate WC post-processing approach and its application |
| CN111020235A (en) * | 2019-12-27 | 2020-04-17 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| CN111020234A (en) * | 2019-12-27 | 2020-04-17 | 厦门钨业股份有限公司 | Method for preparing APT (ammonium paratungstate) by utilizing tungsten-containing waste |
| CN111041208A (en) * | 2019-11-30 | 2020-04-21 | 福达合金材料股份有限公司 | Method for efficiently recycling copper and tungsten in copper-tungsten alloy waste |
| CN111057880A (en) * | 2019-12-27 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| CN111057882A (en) * | 2019-12-31 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from nickel-tungsten-based alloy powder |
| CN111534699A (en) * | 2020-06-16 | 2020-08-14 | 江西一元再生资源有限公司 | Method for recovering valuable substances from cemented carbide scrap |
| CN114045396A (en) * | 2021-10-13 | 2022-02-15 | 湖北和兴环境材料科技有限公司 | Process for recycling rare metals from solid waste and iron oxide heating roasting furnace |
| CN114317982A (en) * | 2021-12-30 | 2022-04-12 | 湖北绿钨资源循环有限公司 | Method for separating and recovering tungsten and cobalt from cobalt solution recovered from hard alloy grinding material |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104942303A (en) * | 2015-07-01 | 2015-09-30 | 崇义章源钨业股份有限公司 | Method for preparing tungsten powder |
| CN105586491A (en) * | 2016-01-18 | 2016-05-18 | 重庆科技学院 | Comprehensive recycling method for waste hard alloy |
| CN105483412A (en) * | 2016-01-27 | 2016-04-13 | 郑州大学 | Method for preparing high-purity tungsten-molybdenum alloy with low-grade tungsten-molybdenum bulk concentrate |
| CN107792883A (en) * | 2016-08-30 | 2018-03-13 | 天津市科密欧化学试剂有限公司 | A kind of preparation method of high purity reagent tungstic acid |
| CN106498172A (en) * | 2016-12-14 | 2017-03-15 | 荆门市格林美新材料有限公司 | Hard-alloy grinding material tungsten-cobalt disperses the recovery method of tungsten in separating |
| CN108220602B (en) * | 2016-12-22 | 2019-05-14 | 荆门德威格林美钨资源循环利用有限公司 | The separation and recovery method of tungsten and titanium in waste hand alloy material |
| CN108220602A (en) * | 2016-12-22 | 2018-06-29 | 荆门德威格林美钨资源循环利用有限公司 | The separation and recovery method of tungsten and titanium in waste hand alloy material |
| CN108728657A (en) * | 2018-07-15 | 2018-11-02 | 安化县众旺钨业有限公司 | A method of recycling tungsten, cobalt, silver, copper and tantalum from hard-alloy grinding waste material |
| CN109536719A (en) * | 2018-12-12 | 2019-03-29 | 株洲金韦硬质合金有限公司 | It is a kind of regenerate WC post-processing approach and its application |
| CN111041208A (en) * | 2019-11-30 | 2020-04-21 | 福达合金材料股份有限公司 | Method for efficiently recycling copper and tungsten in copper-tungsten alloy waste |
| CN111041208B (en) * | 2019-11-30 | 2021-06-22 | 福达合金材料股份有限公司 | Method for efficiently recycling copper and tungsten in copper-tungsten alloy waste |
| CN111020235A (en) * | 2019-12-27 | 2020-04-17 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| CN111057880A (en) * | 2019-12-27 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from tungsten-containing waste material |
| CN111020234A (en) * | 2019-12-27 | 2020-04-17 | 厦门钨业股份有限公司 | Method for preparing APT (ammonium paratungstate) by utilizing tungsten-containing waste |
| CN111057882A (en) * | 2019-12-31 | 2020-04-24 | 厦门钨业股份有限公司 | Method for recovering tungsten from nickel-tungsten-based alloy powder |
| CN111534699A (en) * | 2020-06-16 | 2020-08-14 | 江西一元再生资源有限公司 | Method for recovering valuable substances from cemented carbide scrap |
| CN114045396A (en) * | 2021-10-13 | 2022-02-15 | 湖北和兴环境材料科技有限公司 | Process for recycling rare metals from solid waste and iron oxide heating roasting furnace |
| CN114317982A (en) * | 2021-12-30 | 2022-04-12 | 湖北绿钨资源循环有限公司 | Method for separating and recovering tungsten and cobalt from cobalt solution recovered from hard alloy grinding material |
| CN114317982B (en) * | 2021-12-30 | 2023-10-03 | 湖北绿钨资源循环有限公司 | Method for separating and recovering tungsten and cobalt from cobalt-dissolving liquid recovered from hard alloy grinding material |
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Application publication date: 20150408 |