CN112458317A - Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device - Google Patents

Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device Download PDF

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Publication number
CN112458317A
CN112458317A CN202011313094.XA CN202011313094A CN112458317A CN 112458317 A CN112458317 A CN 112458317A CN 202011313094 A CN202011313094 A CN 202011313094A CN 112458317 A CN112458317 A CN 112458317A
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Prior art keywords
cobalt
tungsten
filter
solution
filter pressing
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CN202011313094.XA
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Inventor
罗名强
罗沙
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Anhua Anren Powder Metallurgy Co ltd
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Anhua Anren Powder Metallurgy Co ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B34/00Obtaining refractory metals
    • C22B34/30Obtaining chromium, molybdenum or tungsten
    • C22B34/36Obtaining tungsten
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00Compounds of tungsten
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00Compounds of cobalt
    • C01G51/06Carbonates
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B23/00Obtaining nickel or cobalt
    • C22B23/04Obtaining nickel or cobalt by wet processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and a filter pressing device are provided, wherein the method comprises the following steps: s1: boiling the tungsten-cobalt-containing waste to produce a sodium tungstate solution; s2: carrying out filter pressing on the sodium tungstate solution for two times to obtain a high-purity sodium tungstate solution, and outputting the high-purity sodium tungstate solution; s3: washing filter residues obtained after filter pressing in the S2, and carrying out filter pressing again on the washed filter liquor and outputting the filter liquor so as to realize tungsten recovery; s4: collecting filter residues obtained after filter pressing in the S3, and then cooking the filter residues with acid to obtain cobalt liquid; s5: carrying out filter pressing on the cobalt solution twice to obtain pure cobalt solution; s6: and reprocessing the pure cobalt solution to obtain the high-purity cobalt solution. The invention also comprises a filter pressing device. The invention has high working efficiency and high recovery rate of tungsten and cobalt, and does not produce pollution in the recovery process.

Description

Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device
Technical Field
The invention relates to the technical field of tungsten and cobalt recovery, in particular to a method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and a filter pressing device.
Background
The existing tungsten-cobalt-containing waste material usually contains 15% -30% of valuable metal tungsten and cobalt, and if the waste material is not recycled, resources are wasted, economic benefits cannot be obtained from the waste material, and pollution is caused. Therefore, recycling of these valuable resources is very important.
The existing method for extracting tungsten from tungsten-containing cobalt waste materials is generally as follows: the waste materials are cooked to obtain a sodium tungstate solution, the sodium tungstate solution is subjected to twice filter pressing and then conveyed to an evaporative crystallization kettle for evaporative crystallization, and crystals are centrifugally dehydrated and dried to obtain sodium tungstate. On one hand, the existing filter pressing mode is to transfer from one filter press to another filter press to obtain two times of filter pressing, the mode easily causes material pollution in the conversion process, the working efficiency is low, or circulating filter pressing is carried out in one filter press, the mode only can pass through the same filter screen, and the filtering effect is poor. On the other hand, the existing tungsten recovery mode is to output after secondary filter pressing, and the remaining filter residue is continuously subjected to recovery of other metals, and the filter residue is not subjected to tungsten recovery again, so that the recovery rate of tungsten is reduced.
The existing method for extracting cobalt from tungsten-containing cobalt waste materials is generally as follows: and (3) firstly, the filter residue is boiled by acid to obtain cobalt liquid, and then the cobalt liquid is output after secondary filter pressing, so that the recovery of cobalt is completed. However, this method cannot completely recover cobalt, and the recovery rate is greatly reduced.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a method for extracting tungsten and cobalt from tungsten-containing cobalt waste and a filter pressing device, which have the advantages of high working efficiency and recovery rate, no pollution and low cost.
The technical scheme of the invention is as follows:
the invention relates to a method for extracting tungsten and cobalt from tungsten-cobalt-containing waste, which comprises the following steps:
s1: boiling the tungsten-cobalt-containing waste to produce a sodium tungstate solution;
s2: carrying out filter pressing on the sodium tungstate solution for two times to obtain a high-purity sodium tungstate solution, and outputting the high-purity sodium tungstate solution;
s3: washing the filter residue after filter pressing in S2, and carrying out filter pressing again on the washed filtrate and outputting the filtrate, thereby realizing tungsten
Recovering;
s4: collecting filter residues obtained after filter pressing in the S3, and then cooking the filter residues with acid to obtain cobalt liquid;
s5: carrying out filter pressing on the cobalt solution twice to obtain pure cobalt solution;
s6: and reprocessing the pure cobalt solution to obtain the high-purity cobalt solution.
Further, in S1, the tungsten-containing cobalt waste is digested with sodium hydroxide.
Further, in S4, the acid is dilute hydrochloric acid, dilute sulfuric acid, or dilute nitric acid.
Further, in S6, reacting the pure cobalt solution with sodium carbonate to generate cobalt carbonate, adding hydrogen peroxide into the solution, and performing filter pressing to obtain a high-purity cobalt carbonate solution.
Further, pumping the high-purity sodium tungstate solution into a sodium tungstate evaporative crystallization kettle for evaporative crystallization, centrifugally dehydrating a crystal, and drying to obtain sodium tungstate; pumping the obtained high-purity cobalt carbonate solution into a crystallization kettle, evaporating and crystallizing, dewatering in a centrifuge after crystallization, and drying to obtain the cobalt carbonate.
Further, the two-time filter pressing is continuously carried out in the same filter pressing device.
The invention relates to a filter pressing device, which comprises a cylinder, wherein two layers of filter cloth are arranged in the cylinder at intervals and are used for carrying out two-time filter pressing on a sodium tungstate solution or a cobalt solution; the feed inlet of the barrel is connected with a cooking device, a liquid outlet is arranged below the barrel, and the liquid outlet is connected with another filter pressing device, an evaporative crystallization kettle or a cobalt liquid reprocessing device through a pipeline and a pump body.
Furthermore, the filtering pore diameter of the lower layer of filter cloth is smaller than that of the upper layer of filter cloth.
Further, the liquid outlet is divided into at least two branches by a pipeline and the pump body, and the two branches are provided with control valves; one branch is connected with the other filter pressing device, and the other branch is connected with the evaporation crystallization kettle.
The invention has the beneficial effects that: on one hand, the sodium tungstate solution is subjected to filter pressing twice in the same equipment, and filter residues after filter pressing are washed and subjected to filter pressing again, namely, the sodium tungstate solution is subjected to filter pressing for multiple times in the same filter pressing equipment, so that the purity of the sodium tungstate solution is greatly improved, the working efficiency is high, the sodium tungstate solution does not need to be subjected to conversion and purification for multiple times, the pollution of the sodium tungstate solution is effectively prevented, and the recovery rate of tungsten is up to more than 99%; on the other hand, the cobalt is recovered by further operating the filter residue, namely, the filter residue is subjected to acid cooking and secondary filter pressing, and then reacts with sodium carbonate and is subjected to filter pressing, so that a high-purity cobalt carbonate solution is obtained, and the recovery rate of the cobalt is improved.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
A method for extracting tungsten and cobalt from tungsten-containing cobalt waste comprises the following steps:
s101: and (3) stewing the tungsten-cobalt-containing waste to produce a sodium tungstate solution.
Specifically, the tungsten-containing cobalt waste is cooked by sodium hydroxide, and the tungsten-containing cobalt waste reacts with the sodium hydroxide to generate a sodium tungstate solution.
S102: and carrying out filter pressing on the sodium tungstate solution for two times to obtain high-purity sodium tungstate solution, and outputting the high-purity sodium tungstate solution.
Specifically, if only one filter pressing is performed, complete recovery of tungsten cannot be guaranteed, and therefore, twice filter pressing is employed, which can improve the recovery rate. The two filter presses of the embodiment are carried out twice in the same filter press device, but not enter two filter presses to complete the two filter presses. The filter pressing device comprises a cylinder, wherein two layers of filter cloth are arranged in the cylinder at intervals and are used for carrying out two-time filter pressing on a sodium tungstate solution or a cobalt solution; the feed inlet of barrel is connected with boiling device, and the below of barrel is equipped with the liquid outlet, and the liquid outlet is through pipeline and pump body connection evaporation crystallization cauldron. Through set up two-layer filter cloth in the barrel, sodium tungstate solution is from boiling device output back, and earlier through first layer filter cloth, filters out the great filter residue of a part granule, and through second layer filter cloth, filters out the filter residue that the granule is less, and the filter aperture of second layer filter cloth is less than the filter aperture of first layer filter cloth promptly. After two-layer filter pressing, high-purity sodium tungstate solution can be obtained. This embodiment is through carrying out twice filtration in succession in same filter pressing device, and not only greatly reduced cost improves work efficiency, and sodium tungstate solution can not cause the pollution because of the secondary is transported moreover. Sodium tungstate solution after two times of filter pressing is pumped into a sodium tungstate evaporative crystallization kettle for evaporative crystallization, and the crystals are centrifugally dehydrated and dried to obtain sodium tungstate.
S103: and (4) washing filter residues obtained after filter pressing in the step (S102), and carrying out filter pressing again on the washed filter liquor, and outputting the filter liquor, so that the tungsten is recovered.
Specifically, because the filter residue can remain on two-layer filter cloth, in order to further extract tungsten, the filter residue on the filter cloth can be washed by water, which is equivalent to carrying out third-time filter pressing, the washed solution is output to another filter pressing device from the filter pressing device, the solution is subjected to twice filter pressing in another filter pressing device, and then is conveyed to a sodium tungstate evaporation crystallization kettle for evaporation crystallization, and the crystal is subjected to centrifugal dehydration and is dried to obtain sodium tungstate, so that the recovery of tungsten is completed. It can be said that the recovery rate of tungsten in this embodiment is as high as 99% or more.
S104: and (4) collecting filter residues obtained after filter pressing in the step (S103), and then cooking the filter residues with acid to obtain a cobalt solution.
Specifically, since cobalt is dissolved in acid, such as dilute hydrochloric acid, dilute nitric acid, and dilute sulfuric acid, to achieve cobalt recovery, in this embodiment, dilute nitric acid is preferably used to cook the filter residue to improve the cobalt recovery rate, so as to obtain cobalt nitrate solution.
S105: and carrying out filter pressing on the cobalt nitrate solution twice to obtain a pure cobalt nitrate solution.
The specific operation manner is the same as S102, and is not described here again. The cooking device for residue cooking in this embodiment is different from the cooking device in step S101, and does not share one device, and the filter-pressing device in S102 and the filter-pressing device for cobalt nitrate solution do not share one device.
S106: and reprocessing the pure cobalt nitrate solution to obtain a high-purity cobalt carbonate solution.
Specifically, reacting a pure cobalt nitrate solution with sodium carbonate to generate cobalt carbonate, adding hydrogen peroxide, and performing filter pressing to obtain a high-purity cobalt carbonate solution; and pumping the obtained high-purity cobalt carbonate solution into a crystallization kettle, evaporating and crystallizing, dewatering in a centrifugal machine after crystallization, and drying to obtain the cobalt carbonate. In the embodiment, cobalt nitrate reacts with sodium carbonate to generate cobalt carbonate precipitate, so that cobalt is further purified; by adding hydrogen peroxide in the filter pressing process, precipitation and filtration can be kept, so that the cobalt carbonate solution is purer.
In summary, on one hand, the sodium tungstate solution is subjected to filter pressing twice in the same device, and filter residues after filter pressing are washed and subjected to filter pressing again, which is equivalent to multiple filter pressing in the same filter pressing device, so that the purity of the sodium tungstate solution is greatly improved, the working efficiency is high, the sodium tungstate solution does not need to be converted and purified for multiple times, the pollution of the sodium tungstate solution is effectively prevented, and the recovery rate of tungsten is up to more than 99%; on the other hand, the cobalt is recovered by further operating the filter residue, namely, the filter residue is subjected to acid cooking and secondary filter pressing, and then reacts with sodium carbonate and is subjected to filter pressing, so that a high-purity cobalt carbonate solution is obtained, and the recovery rate of the cobalt is improved.

Claims (9)

1. A method for extracting tungsten and cobalt from tungsten-containing cobalt waste is characterized by comprising the following steps:
s1: boiling the tungsten-cobalt-containing waste to produce a sodium tungstate solution;
s2: carrying out filter pressing on the sodium tungstate solution for two times to obtain a high-purity sodium tungstate solution, and outputting the high-purity sodium tungstate solution;
s3: washing filter residues obtained after filter pressing in the S2, and carrying out filter pressing again on the washed filter liquor and outputting the filter liquor so as to realize tungsten recovery;
s4: collecting filter residues obtained after filter pressing in the S3, and then cooking the filter residues with acid to obtain cobalt liquid;
s5: carrying out filter pressing on the cobalt solution twice to obtain pure cobalt solution;
s6: and reprocessing the pure cobalt solution to obtain the high-purity cobalt solution.
2. The method for extracting tungsten and cobalt from tungsten-containing cobalt waste as claimed in claim 1, wherein in S1, sodium hydroxide is used to cook the tungsten-containing cobalt waste.
3. The method for extracting tungsten and cobalt from tungsten-containing cobalt waste material as claimed in claim 1 or 2, wherein in S4, the acid is dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
4. The method for extracting tungsten and cobalt from the tungsten-cobalt-containing waste material as claimed in claim 1 or 2, wherein in S6, the pure cobalt solution is reacted with sodium carbonate to generate cobalt carbonate, and hydrogen peroxide is added into the solution for filter pressing to obtain high-purity cobalt carbonate solution.
5. The method for extracting tungsten and cobalt from the tungsten-cobalt-containing waste material according to claim 1 or 2, characterized in that a high-purity sodium tungstate solution is pumped into a sodium tungstate evaporation crystallization kettle for evaporation and crystallization, and a crystal is centrifugally dehydrated and dried to obtain sodium tungstate; pumping the obtained high-purity cobalt carbonate solution into a crystallization kettle, evaporating and crystallizing, dewatering in a centrifuge after crystallization, and drying to obtain the cobalt carbonate.
6. The method for extracting tungsten and cobalt from tungsten-containing cobalt waste material according to claim 1 or 2, wherein the two filter pressing steps are performed in the same filter pressing device in a continuous manner.
7. A filter pressing device is characterized by comprising a cylinder body, wherein two layers of filter cloth are arranged in the cylinder body at intervals and are used for carrying out two-time filter pressing on a sodium tungstate solution or a cobalt solution; the feed inlet of the barrel is connected with a cooking device, a liquid outlet is arranged below the barrel, and the liquid outlet is connected with another filter pressing device, an evaporative crystallization kettle or a cobalt liquid reprocessing device through a pipeline and a pump body.
8. The pressure filtration device as claimed in claim 7, wherein the lower filter cloth has a smaller filtration pore size than the upper filter cloth.
9. A filter-pressing arrangement as claimed in claim 7 or 8 wherein the outlet is divided into at least two branches by a conduit and a pump body, and wherein both branches are provided with control valves; one branch is connected with the other filter pressing device, and the other branch is connected with the evaporation crystallization kettle.
CN202011313094.XA 2020-11-20 2020-11-20 Method for extracting tungsten and cobalt from tungsten-cobalt-containing waste and filter pressing device Pending CN112458317A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI763517B (en) * 2021-06-02 2022-05-01 聯友金屬科技股份有限公司 Method for recovering cobalt in waste cemented carbide

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CN102814063A (en) * 2012-08-14 2012-12-12 佛山市金凯地过滤设备有限公司 Pressure filter and pressure filtration method thereof
CN102963911A (en) * 2012-11-14 2013-03-13 中湘钨业股份有限公司 Method of recycling residual alkali from sodium tungstate solution in tungsten smelting
KR20160120614A (en) * 2015-04-08 2016-10-18 주식회사 포스코 Apparatus for recovering byproducts from nickel extraction process
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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
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
TWI763517B (en) * 2021-06-02 2022-05-01 聯友金屬科技股份有限公司 Method for recovering cobalt in waste cemented carbide

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