CN114032395B - Method for recovering copper, nickel and chromium in electroplating sludge by using waste cathode carbon as additive through oxidation-reduction two-step method - Google Patents
Method for recovering copper, nickel and chromium in electroplating sludge by using waste cathode carbon as additive through oxidation-reduction two-step method Download PDFInfo
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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
- C22B7/006—Wet processes
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B15/00—Obtaining copper
- C22B15/0026—Pyrometallurgy
- C22B15/0028—Smelting or converting
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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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/02—Obtaining nickel or cobalt by dry processes
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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
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
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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
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/32—Obtaining chromium
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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
- C22B5/00—General methods of reducing to metals
- C22B5/02—Dry methods smelting of sulfides or formation of mattes
- C22B5/10—Dry methods smelting of sulfides or formation of mattes by solid carbonaceous reducing agents
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- 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
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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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Abstract
The invention discloses a method for recycling copper, nickel and chromium in electroplating sludge by using waste cathode carbon as an additive through an oxidation-reduction two-step method, which comprises the steps of uniformly mixing the electroplating sludge, the waste cathode carbon and calcium oxide according to a certain proportion, feeding the mixture into a roasting furnace for roasting, and enabling the cathode carbon in the furnace to firstly undergo combustion reaction to synchronously realize decomposition of cyanide, naF and Na in the cathode carbon 3 AlF 6 Dissociation of components and thermal conversion of electroplating sludge. After the oxidation process is finished, leaching roasting slag in water, leaching sodium chromate in a large amount, freezing and crystallizing leaching liquid to obtain sodium chromate product, drying leaching slag, transferring to a smelting furnace, carrying out high-temperature smelting reduction on the leaching slag by taking waste cathode carbon as a reducing agent, discharging copper-nickel alloy from a molten metal outlet at the lower part of the smelting furnace, discharging smelting slag from a slag outlet, and discharging smelting flue gas reaching the standard after waste heat recovery and flue gas treatment into the atmosphere. The invention uses waste to treat waste, and has the advantages of short flow, low cost and the like, thereby having good popularization and application prospect.
Description
Technical Field
The invention relates to the technical field of industrial hazardous waste recycling treatment, in particular to a method for recycling copper, nickel and chromium in electroplating sludge by using a two-step oxidation-reduction method with waste cathode carbon as an additive.
Background
Electroplating sludge is a solid waste produced by heavy metal precipitation in the electroplating industry, and is classified as dangerous waste because of its high heavy metal content. The sludge contains various metals such as copper, nickel, chromium, iron, zinc and the like, exists in the form of hydroxide, and also comprises some organic components and complex metal oxides. In China, more than 1000 ten thousand tons of electroplating sludge can be produced each year, if the electroplating sludge is not properly and timely disposed, heavy metals can migrate into the environment to pollute soil and underground water, influence the survival of animals and plants, and even threaten the life health of human beings. The existing treatment method mainly comprises solidification and stabilization, medium-temperature sodium oxidation, acid-base leaching and the like. The solidification and stabilization are that the electroplating sludge is solidified by cement, lime and fly ash and then buried, but the method can release toxic substances into the environment to produce secondary pollution and waste metal resources. The method provides a new idea for recovering metal chromium in electroplating sludge, but excessive sodium carbonate addition amount in the process and high process cost. The acid-base leaching realizes the leaching separation of metals by using the chemical reaction of different metal compounds in electroplating sludge and acid-base, but the method has poor selectivity and can generate a large amount of waste liquid.
The waste cathode carbon is a dangerous solid waste generated in the process of preparing aluminum by electrolysis, and mainly consists of graphite carbon and fluoride (NaF and Na) 3 AlF 6 、CaF 2 Etc.), cyanide (NaCN, na 3 Fe(CN) 6 Etc.) and other inorganic compounds. About 36 ten thousand tons of waste cathode carbon are produced in China every year, and on average, one ton of aluminum is not produced, 10 kilograms of waste cathode carbon are produced, and along with the continuous development of the electrolytic aluminum industry, the production amount of the waste cathode carbon also has a continuous rising trend. Because of their fluoride and cyanide content, they can also present a significant environmental hazard if improperly handled. But has high recovery value because of rich carbon resources. At present, more than 50% of waste cathode carbon is buried, the operation is simple, the cost is low, but a large amount of carbonaceous resources are wasted, and the pollution of soil and underground water is caused. Therefore, some students studied about the properties of the substancesThe physical separation of the waste cathode carbon is realized by floatation by utilizing the difference of the wettability of the surfaces of the carbon and the fluoride, and the conversion of the fluoride and the degradation of the cyanide are realized by high-temperature combustion by utilizing the high heat value of the carbonaceous material in the waste cathode carbon. However, the products recovered by the methods have lower purity or high energy consumption, and waste a large amount of resources, namely harmless conversion is realized, but recycling recovery is not realized to the greatest extent. Although acid leaching and alkaline leaching in the wet method can realize recovery with higher purity, the selectivity is poor, and the treatment of waste liquid generated in the process is also a serious problem.
Disclosure of Invention
Aiming at the problems, the invention provides a method for recycling copper, nickel and chromium in electroplating sludge by using waste cathode carbon as an additive through an oxidation-reduction two-step method. The invention takes waste cathode carbon as an additive, extracts chromium, copper and nickel in electroplating sludge step by step and effectively recovers the chromium, copper and nickel in electroplating sludge by a two-step oxidation and reduction method, and completely decomposes cyanide in the waste cathode carbon to realize harmless treatment, wherein fluorine exists in a smelting slag phase stably in a calcium fluoride form. The method realizes the treatment of waste by waste, has the advantages of short flow, low cost and the like, and has good popularization and application prospect. The invention is realized by the following technical scheme.
A method for recovering copper, nickel and chromium in electroplating sludge by using waste cathode carbon as an additive through an oxidation-reduction two-step method comprises the following specific steps:
(1) Firstly, uniformly mixing electroplating sludge, waste cathode carbon and calcium oxide according to a certain proportion, wherein the addition amount of the waste cathode carbon is that of the waste cathode carbon: electroplating sludge = 1:0.5 to 2.5, the addition amount of the calcium oxide is calcium oxide: electroplating sludge = 0.09-0.2:1, a step of;
(2) The mixture is sent into a roasting furnace for roasting, and parameters such as roasting temperature, roasting time, oxygen introduction amount and the like are controlled in the process to finish the directional conversion of chromium and the preliminary fixation of fluorine, wherein the roasting temperature is 400-800 ℃, the roasting time is 1-3h, and the oxygen introduction amount is 1.5-3.5 times of the oxygen demand required by the complete combustion of cathode carbon;
(3) Leaching the roasting slag, and controlling the leaching temperature, time and water-solid ratio to realize leaching separation of sodium chromate, wherein the leaching temperature is 20-50 ℃, the leaching time is 30-100min, and the water-solid ratio is (3-7): 1, a step of;
(4) The leaching solution is frozen and crystallized to obtain sodium chromate product, the leaching slag is dried and then is transferred into a smelting furnace, the waste cathode carbon is used as a reducing agent to carry out high-temperature melting reduction, the adding amount of a slag former, the melting reduction temperature and the melting reduction time are controlled in the process, the copper and nickel phases are fully reduced and then are subjected to sedimentation and enrichment in a copper-nickel alloy form, and the adding amount of silicon dioxide of the slag former is controlled to be CaO/SiO 2 The ratio of the waste cathode carbon to the leaching residue is 1:1-2, the adding amount of the waste cathode carbon is 4-10% of the leaching residue mass, the smelting reduction temperature is 1150-1300 ℃, and the smelting reduction time is 1-3h;
(5) After the reduction process is finished, the copper-nickel alloy is discharged from a molten metal outlet at the lower part of the smelting furnace, smelting slag is discharged from a slag outlet, and smelting flue gas is discharged into the atmosphere after waste heat recovery and flue gas treatment reach standards.
The beneficial effects of the invention are as follows:
1. according to the preparation method, through coupling treatment of electroplating sludge and waste cathode carbon, toxic component cyanide in the waste cathode carbon can be completely decomposed to realize harmless treatment, and fluorine exists in a smelting slag phase stably in a calcium fluoride form;
2. according to the preparation method, the chromium component in the electroplating sludge can be directionally converted into sodium chromate, and then high-efficiency separation and recovery are realized through water leaching, so that the problems of large dispersion of chromium and low recovery rate in the traditional process are overcome;
(3) The preparation method of the invention uses waste to treat waste, has the advantages of short flow, low cost and the like, and has good popularization and application prospect.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention will be further described with reference to the drawings and detailed description.
Example 1
Coupling treatment is carried out by adopting electroplating sludge from a certain electroplating plant and waste cathode carbon from a certain electrolytic aluminum plant, wherein the contents of copper, nickel and chromium in the electroplating sludge are respectively 6.51%, 7.27% and 4.22%, and the carbon in the waste cathode carbon containsThe amount was 73.24% and the fluorine content was 9.49%. Electroplating sludge, waste cathode carbon and calcium oxide are mixed according to the mass ratio of the waste cathode carbon: electroplating sludge = 1:0.5, calcium oxide: electroplating sludge = 0.1:1, after being uniformly mixed, the mixture is sent into a roasting furnace for roasting, wherein the roasting temperature is controlled to be 600 ℃ and the roasting time is controlled to be 2 hours in the process, the oxygen flux is 3 times of the oxygen demand required by the complete combustion of cathode carbon, after the roasting process is finished, the roasting slag is soaked in water, the soaking temperature is controlled to be 30 ℃, the soaking time is controlled to be 90 minutes, and the water-solid ratio is 3:1, a step of; and then the leaching solution is frozen and crystallized to obtain a sodium chromate product, the leaching slag is dried and then is transferred into a smelting furnace, the waste cathode carbon is used as a reducing agent to carry out high-temperature fusion reduction, and the adding amount of the slag former silicon dioxide is controlled to be CaO/SiO in the process 2 The ratio of the waste cathode carbon to the leaching residue is 1:1, the adding amount of the waste cathode carbon is 5% of the leaching residue mass, the smelting reduction temperature is 1250 ℃, the smelting reduction time is 2 hours, after the reduction process is finished, the copper-nickel alloy is discharged from a metal liquid outlet at the lower part of the smelting furnace, the smelting residue is discharged from a slag outlet, and the smelting flue gas is discharged into the atmosphere after the waste heat recovery and the flue gas treatment reach the standards. After the treatment is finished, the contents of copper, nickel and chromium in waste slag can be reduced to 0.55%, 0.62% and 0.33% respectively, so that the high-efficiency recovery of copper, nickel and chromium in electroplating sludge is realized, the sealing efficiency of fluorine in waste cathode carbon is up to 97%, the leaching toxicity value of fluorine in national standard slag is 5mg/l and is far lower than the leaching toxicity identification standard (100 mg/l) of fluorine, the leaching toxicity value of cyanogen in national standard slag is 0.006mg/l and is far lower than the leaching toxicity identification standard (5 mg/l) of cyanogen, and the harmless treatment of fluorine and cyanogen in waste cathode carbon is realized by the preparation method.
Example 2
The electroplating sludge of a certain electroplating plant and the waste cathode carbon of a certain electrolytic aluminum plant are adopted for coupling treatment, wherein the contents of copper, nickel and chromium in the electroplating sludge are respectively 7.23%, 5.66% and 4.28%, and the carbon content in the waste cathode carbon is 74.18% and the fluorine content is 8.49%. Electroplating sludge, waste cathode carbon and calcium oxide are mixed according to the mass ratio of the waste cathode carbon: electroplating sludge = 1:0.8, calcium oxide: electroplating sludge = 0.15:1, after being mixed evenly, the mixture is sent into a roasting furnace for roasting, the roasting temperature is controlled to be 650 ℃ and the roasting time is controlled to be 1.5 hours, the oxygen introducing amount is 2.5 times of the oxygen demand required by the complete combustion of cathode carbon, and after the roasting process is finished, the mixture is added into the mixtureLeaching the roasting slag, controlling the leaching temperature to be 40 ℃, leaching time to be 80min, and water-solid ratio to be 4:1, a step of; then freezing and crystallizing the leaching solution to obtain sodium chromate product, drying the leaching slag, transferring the leaching slag into a smelting furnace, and carrying out high-temperature fusion reduction on the leaching slag by taking waste cathode carbon as a reducing agent, wherein the adding amount of slag former silicon dioxide is controlled to be CaO/SiO in the process 2 The ratio of the waste cathode carbon to the leaching slag is 1:1.5, the adding amount of the waste cathode carbon is 7% of the mass of the leaching slag, the smelting reduction temperature is 1180 ℃, the smelting reduction time is 2.5h, after the reduction process is finished, the copper-nickel alloy is discharged from a metal liquid outlet at the lower part of the smelting furnace, the smelting slag is discharged from a slag outlet, and the smelting flue gas is discharged into the atmosphere after the waste heat recovery and the flue gas treatment reach the standards. After the treatment is finished, the contents of copper, nickel and chromium in waste slag can be reduced to 0.42%, 0.72% and 0.28% respectively, so that the high-efficiency recovery of copper, nickel and chromium in electroplating sludge is realized, the sealing efficiency of fluorine in the waste slag is up to 95%, the leaching toxicity value of fluorine in national standard slag is 8mg/l, which is far lower than the leaching toxicity identification standard (100 mg/l) of fluorine, the leaching toxicity value of cyanide in national standard slag is 0.002mg/l, which is far lower than the leaching toxicity identification standard (5 mg/l) of cyanide, and the harmless treatment of fluorine and cyanide in waste cathode carbon is realized by the preparation method of the invention.
Example 3
The method adopts the electroplating sludge of a certain electroplating plant and the waste cathode carbon of a certain electrolytic aluminum plant for coupling treatment, wherein the copper, nickel and chromium contents in the electroplating sludge are respectively 6.51%, 7.27% and 4.22%, and the carbon content in the waste cathode carbon is 71.78% and the fluorine content is 9.43%. Electroplating sludge, waste cathode carbon and calcium oxide are mixed according to the mass ratio of the waste cathode carbon: electroplating sludge = 1:1. calcium oxide: electroplating sludge = 0.3:1, after being uniformly mixed, the mixture is sent into a roasting furnace for roasting, wherein the roasting temperature is controlled to be 700 ℃ and the roasting time is controlled to be 2 hours in the process, the oxygen flux is 3.5 times of the oxygen demand required by the complete combustion of cathode carbon, after the roasting process is finished, the roasting slag is soaked in water, the soaking temperature is controlled to be 45 ℃, the soaking time is controlled to be 90 minutes, and the water-solid ratio is 3.5:1, a step of; then freezing and crystallizing the leaching solution to obtain sodium chromate product, drying the leaching slag, transferring the leaching slag into a smelting furnace, and carrying out high-temperature fusion reduction on the leaching slag by taking waste cathode carbon as a reducing agent, wherein the adding amount of slag former silicon dioxide is controlled to be CaO/SiO in the process 2 The adding amount of the waste cathode carbon is 8 of the mass of the leaching slag according to the ratio of 1:2The melting reduction temperature is 1300 ℃, the melting reduction time is 3h, after the reduction process is finished, the copper-nickel alloy is discharged from a metal liquid outlet at the lower part of the smelting furnace, smelting slag is discharged from a slag outlet, and smelting flue gas is discharged into the atmosphere after waste heat recovery and flue gas treatment reach the standards. After the treatment is finished, the contents of copper, nickel and chromium in waste slag can be reduced to 0.42%, 0.33% and 0.12% respectively, so that the high-efficiency recovery of copper, nickel and chromium in electroplating sludge is realized, the sealing efficiency of fluorine in the waste slag is 98%, the leaching toxicity value of fluorine in national standard method slag is 4mg/l and is far lower than the leaching toxicity identification standard (100 mg/l) of fluorine, the leaching toxicity value of cyanide in national standard method slag is 0.01mg/l and is far lower than the leaching toxicity identification standard (5 mg/l) of cyanide, and the harmless treatment of fluorine and cyanide in waste cathode carbon is realized by the preparation method.
Claims (1)
1. A method for recovering copper, nickel and chromium in electroplating sludge by using waste cathode carbon as an additive through an oxidation-reduction two-step method is characterized by comprising the following specific steps:
(1) Firstly, uniformly mixing electroplating sludge, waste cathode carbon and calcium oxide according to a certain proportion; wherein the addition amount of the waste cathode carbon is as follows: electroplating sludge = 1:0.5 to 2.5, the addition amount of the calcium oxide is calcium oxide: electroplating sludge = 0.09-0.2:1, a step of;
(2) Sending the mixture into a roasting furnace for roasting, and controlling related parameters such as roasting temperature, roasting time, oxygen introducing amount and the like in the process to finish the directional conversion of chromium and the primary fixation of fluorine; wherein the roasting temperature is 400-800 ℃; roasting for 1-3h; the oxygen quantity is 1.5-3.5 times of the oxygen quantity required by the complete combustion of cathode carbon in the mixed material;
(3) Leaching the roasting slag, and controlling the leaching temperature, time and water-solid ratio to realize leaching separation of sodium chromate; wherein the water immersion temperature is 20-50 ℃; the water immersion time is 30-100min; the water-solid ratio is (3-7): 1, a step of;
(4) The leaching solution is frozen and crystallized to obtain sodium chromate product, the leaching slag is dried and transferred into a smelting furnace, the waste cathode carbon is used as a reducing agent to carry out high-temperature melting reduction, and the adding amount of the waste cathode carbon, the adding amount of a slag forming agent, the melting reduction temperature and time, and copper and nickel are controlled in the processCarrying out sedimentation enrichment in a copper-nickel alloy form after the phase is fully reduced; wherein the precipitation mode of sodium chromate is freezing crystallization; the leaching slag melting reducing agent is waste cathode carbon, and the addition amount is 4-10% of the leaching slag mass; the precipitation mode of sodium chromate in the leaching solution is freezing crystallization; the slag former is silicon dioxide, and the addition amount is controlled to be CaO/SiO 2 The ratio of the slag to the calcium slag is 1:1-2, and the slag is a silicon-calcium slag system; smelting at 1150-1300 deg.c for 1-3 hr;
(5) After the reduction process is finished, the copper-nickel alloy is discharged from a molten metal outlet at the lower part of the smelting furnace, smelting slag is discharged from a slag outlet, and smelting flue gas is discharged into the atmosphere after waste heat recovery and flue gas treatment reach standards.
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2021
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