CN109468468B - Method for comprehensively utilizing and treating molybdenum-copper slag - Google Patents
Method for comprehensively utilizing and treating molybdenum-copper slag Download PDFInfo
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- 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
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- C22B34/30—Obtaining chromium, molybdenum or tungsten
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Abstract
The invention discloses a method for comprehensively utilizing and treating molybdenum-copper slag, which comprises 9 steps of drying, grinding, washing, first pressure filtration, washing liquid treatment, alkaline leaching of filter residue, second pressure filtration, primary absorption of tail gas and secondary absorption of the tail gas. The invention provides an environment-friendly and resource comprehensive utilization method, which realizes tail gas SO by treatment2The absorption rate of the product reaches 99.9 percent, the water is recycled without wastewater discharge, the produced solids are respectively sodium tungsten molybdate products, copper sulfate products and calcium sulfate products, and no solid waste is discharged; the process has the advantages of simple equipment, short flow, no three wastes, tungsten and molybdenum recovery rate of more than 97 percent and Cu recovery rate of more than 98 percent, and realizes the purposes of high efficiency, environmental protection, high added value comprehensive utilization and molybdenum and copper slag treatment.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to a method for comprehensively utilizing and treating molybdenum-copper slag.
Background
The molybdenum-copper slag is obtained from a tungsten smelting production process, and because the properties of tungsten and molybdenum are similar, in order to obtain a high-purity ammonium paratungstate product, namely APT: (NH4)2WO4Most tungsten smelting enterprises adopt a selective precipitation method to separate tungsten from molybdenum, and after tungsten is purified, the separated molybdenum forms a precipitate with a main component of copper thiomolybdate, and the precipitate is called molybdenum copper slag in the industry. Molybdenum copper slag is now listed as a hazardous waste by the state, but molybdenum contained in molybdenum copper slag: 10% -25%, tungsten: 5% -10%, copper: 25% -40%, sulfur: 30 to 50 percent of the molybdenum ore, and the molybdenum ore is recycled along with the vigorous implementation of environmental protection and the gradual exhaustion of molybdenum ore resourcesThe molybdenum-copper slag is treated by an ecological environment-friendly waste recycling method, and main elements in the molybdenum-copper slag are required to be respectively prepared into valuable products, so that the utilization and treatment of comprehensive, efficient, green (environment-friendly) and high-added-value resources are realized.
The existing treatment method for molybdenum-copper slag generally has the defects of long process, incomplete separation of molybdenum, copper and sulfur, low recovery rate and the like; the extraction process produces large amounts of SO2The generation of waste gas, waste water containing acid or alkali, and waste slag containing copper not only corrodes equipment and worsens production environment to influence normal operation of production, but also seriously pollutes atmosphere, water and soil.
It is known from the literature that the ion exchange method adopted in the related patents for enriching tungsten and molybdenum in the leaching solution of molybdenum copper slag produces a large amount of SO4 2-、OH-The wastewater of (4); the related patents adopt the technology of extracting to separate tungsten and molybdenum or extracting copper, wherein a large amount of extracting agent is volatilized into the air, so that the fire risk and the pollution of oil to water and soil exist; in the similar raw materials, after copper and molybdenum are separated in alkaline leaching, alkaline leaching solution is directly precipitated by calcium chloride, the produced calcium molybdate contains a large amount of calcium sulfide, and low-valent sulfur in the calcium sulfide is simultaneously leached when the calcium molybdate is leached, so that the separation of sulfur and molybdenum is incomplete, great trouble is brought to the subsequent purification of molybdenum products, and a large amount of waste acid is generated; the method adopts an ion exchange method, generates a large amount of waste water and easily causes the ammonia nitrogen of the waste water to exceed the standard; the similar raw materials are prepared by enriching tungsten and molybdenum in leachate with macroporous anion exchange resin, separating tungsten and molybdenum by extraction method, extracting copper by extraction method to obtain large amount of SO4 2-、OH-In the process of using the extracting agent, a large amount of highly toxic organic matters are volatilized into the air, so that the leaked oil pollutes water and soil while the fire risk exists.
Disclosure of Invention
The purpose of the invention is as follows: overcomes the defects of the prior art and provides a method for comprehensively utilizing and treating molybdenum-copper slag with environmental protection and high efficiency.
The technical scheme is as follows: a method for comprehensively utilizing and treating molybdenum-copper slag comprises 9 steps of drying, grinding, washing, primary filter pressing, washing liquor treatment, alkaline leaching of filter residue, secondary filter pressing, primary absorption of tail gas and secondary absorption of tail gas:
1) and (3) drying: drying the molybdenum-copper slag with the water content of 0-40%, and carrying out tail gas absorption treatment on tail gas generated in the drying process in the subsequent step 9) and step 10);
preferably, during drying, the molybdenum-copper slag is flatly paved on a dryer, and the thickness of a material layer is 5-50 cm; the drying and heating temperature is 180-300 ℃, and the drying time is 8-20 hours; the drying heat source adopts high-temperature steam, electric heating or microwave;
2) grinding: and (3) crushing and grinding the dried molybdenum-copper slag by a Raymond mill or a rod mill to ensure that the granularity reaches D97: 50 μm;
3) washing: stirring and washing the finely ground molybdenum-copper slag solid material and industrial water for 1-3 hours at normal temperature according to the solid-liquid ratio of 1: 2-1: 5;
4) primary filter pressing: after washing, carrying out solid-liquid separation by first filter pressing through a filter press to obtain first filter pressing filter residue and first filter pressing washing liquid; the first filter pressing washing liquid can directly enter the subsequent step 5), or can return to the step 3) to participate in washing again, and the washing liquid subjected to 1-6 times of circulating washing and filter pressing enters the subsequent step 5) for washing liquid treatment; carrying out alkaline leaching on the first filter residue in the subsequent step 6);
5) and (3) washing liquid treatment: the first filter pressing washing liquid mainly comprises copper sulfate solution, and Cu enriched by the first filter pressing washing liquid is recycled2+The concentration is more than 10 g/l; cooling and crystallizing the first filter pressing washing liquid and the first-stage absorption filtrate (the main component is also copper sulfate solution) of the tail gas obtained in the step 8) at the temperature of 0-10 ℃, and filtering to obtain CuSO with the mass fraction of more than 99%4.5H2O, wherein the recovery rate of Cu is more than 98 percent; the filtered mother liquor can be cooled and crystallized again;
6) alkaline leaching of filter residue: mixing and size mixing the first filter-pressing filter residue and industrial water according to the solid-liquid weight ratio of 1: 2-1: 4, adding NaOH solution for alkaline leaching reaction, heating to 60-90 ℃, stirring for 1-4 hours until the pH value reaches 10-14 at the end of the reaction;
the main reaction formula is as follows:
MoO3+2NaOH＝Na2MoO4；
WO3+2NaOH＝Na2WO4；
7) and (3) secondary filter pressing: after the alkaline leaching of the filter residue is finished, carrying out secondary filter pressing and solid-liquid separation to obtain secondary filter pressing filter residue and secondary filter pressing filtrate; evaporating the second filter pressing filtrate to dryness to obtain a sodium tungsten molybdate product, namely a mixture of sodium tungstate and sodium molybdate; the purity of the sodium tungsten molybdate can reach more than 98 percent, and the recovery rate of the tungsten and the molybdenum is more than 97 percent; the main component of the secondary filter pressing filter residue is copper oxide, and the secondary filter pressing filter residue enters a subsequent step 8) for primary absorption of tail gas;
8) primary absorption of tail gas:
mixing the secondary filter-pressing filter residue (copper oxide) and industrial water in a solid-to-liquid ratio of 1: 1-1: 4 in a primary absorption tank, and mixing tail gas (the main component is SO) generated in the drying process2) Introducing into a first-stage absorption tank, and stirring by adopting compressed air;
the main reaction formula is as follows: CuO + SO2+O2＝CuSO4；
Sampling and inspecting the concentration of copper ions in the primary absorption tank, when the concentration is more than 10g/l, extracting supernatant and filtering, and then, cooling and crystallizing filtrate copper sulfate solution in the step 5); filter residue (the main component is CuO) can be returned to the step 8) for circulation and first-stage absorption of tail gas;
9) secondary absorption of tail gas:
the tail gas (the main component is still SO) remained after the first-stage absorption treatment of the tail gas2) Introducing into NaOH solution in a tail gas secondary absorption tank, keeping the pH value to be more than 9, performing tail gas secondary absorption to generate absorption liquid NaSO3(ii) a The absorption liquid is regenerated with CaO to generate CaSO3And NaOH, and recycling the NaOH to absorb the tail gas SO again2(ii) a Calcium sulfate product is obtained by filtration, and tail gas SO is generated in the process2Has an absorption of 99.9%;
the main reaction formula is as follows:
SO2+2NaOH＝Na2SO3；
Na2SO3+CaO+H2O＝CaSO3↓+2NaOH。
the invention has the beneficial effects that: the invention provides an environment-friendly and resource comprehensive utilization method, which can realize zero emission and prepare high-purity sodium tungsten molybdate, copper sulfate and other products; the treatment process has the advantages that the tail gas generated in the process is treated to realize SO2The absorption rate of the water-based composite material reaches 99.9 percent, the water is recycled, no wastewater is discharged, the produced solids are respectively a sodium tungsten molybdate product, a copper sulfate product and a calcium sulfate product, and no solid waste is discharged; the process has the advantages of simple equipment, short flow, no three wastes, tungsten and molybdenum recovery rate of more than 97 percent, Cu recovery rate of more than 98 percent, high purity of various prepared products and realization of the purposes of high efficiency, environmental protection and high added value comprehensive utilization and treatment.
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FIG. 1 is a schematic flow chart of the method for preparing sodium molybdate by extracting molybdenum from molybdenum-removed slag according to the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in detail with reference to the accompanying drawings and specific embodiments.
As shown in figure 1, the method for comprehensively utilizing and treating the molybdenum-copper slag comprises 9 steps of drying, grinding, washing, first pressure filtration, washing liquid treatment, alkaline leaching of filter residue, second pressure filtration, primary absorption of tail gas and secondary absorption of tail gas:
1) and (3) drying: drying the molybdenum-copper slag with the water content of 0-40%, and carrying out tail gas absorption treatment on tail gas generated in the drying process in the subsequent step 8) and step 9);
preferably, during drying, the molybdenum-copper slag is flatly paved on a dryer, and the thickness of a material layer is 5-50 cm; the drying and heating temperature is 180-300 ℃, and the drying time is 8-20 hours; the drying heat source adopts high-temperature steam, electric heating or microwave;
2) grinding: and (3) crushing and grinding the dried molybdenum-copper slag by a Raymond mill or a rod mill to ensure that the granularity reaches D97: 50 μm;
3) washing: stirring and washing the finely ground molybdenum-copper slag solid material and industrial water for 1-3 hours at normal temperature according to the solid-liquid ratio of 1: 2-1: 5;
4) primary filter pressing: after washing, carrying out solid-liquid separation by first filter pressing through a filter press to obtain first filter pressing filter residue and first filter pressing washing liquid; the first filter pressing washing liquid can directly enter the subsequent step 5), or can return to the step 3) to participate in washing again, and the washing liquid subjected to 1-6 times of circulating washing and filter pressing enters the subsequent step 5) for washing liquid treatment; carrying out alkaline leaching on the first filter residue in the subsequent step 6);
5) and (3) washing liquid treatment: the first filter pressing washing liquid mainly comprises copper sulfate solution, and Cu enriched by the first filter pressing washing liquid is recycled2+The concentration is more than 10 g/l; cooling and crystallizing the first filter pressing washing liquid and the first-stage absorption filtrate (the main component is also copper sulfate solution) of the tail gas obtained in the step 8) at the temperature of 0-10 ℃, and filtering to obtain CuSO with the mass fraction of more than 99%4.5H2O, wherein the recovery rate of Cu is more than 98 percent; the filtered mother liquor can be cooled and crystallized again;
6) alkaline leaching of filter residue: mixing and size mixing the first filter-pressing filter residue and industrial water according to the solid-liquid weight ratio of 1: 2-1: 4, adding NaOH solution for alkaline leaching reaction, heating to 60-90 ℃, stirring for 1-4 hours until the pH value reaches 10-14 at the end of the reaction;
the main reaction formula is as follows:
MoO3+2NaOH＝Na2MoO4；
WO3+2NaOH＝Na2WO4；
7) and (3) secondary filter pressing: after the alkaline leaching of the filter residue is finished, carrying out secondary filter pressing and solid-liquid separation to obtain secondary filter pressing filter residue and secondary filter pressing filtrate; evaporating the second filter pressing filtrate to dryness to obtain a sodium tungsten molybdate product, namely a mixture of sodium tungstate and sodium molybdate; the purity of the sodium tungsten molybdate can reach more than 98 percent, and the recovery rate of the tungsten and the molybdenum is more than 97 percent; the main component of the secondary filter pressing filter residue is copper oxide, and the secondary filter pressing filter residue enters a subsequent step 8) for primary absorption of tail gas;
8) primary absorption of tail gas:
mixing the secondary filter-pressing filter residue (copper oxide) and industrial water in a solid-to-liquid ratio of 1: 1-1: 4 in a primary absorption tank, and mixing tail gas (the main component is SO) generated in the drying process2) Introducing into a first-stage absorption tank, and stirring by adopting compressed air;
the main reaction formula is as follows: CuO + SO2+O2＝CuSO4；
Sampling and inspecting the concentration of copper ions in the primary absorption tank, when the concentration is more than 10g/l, extracting supernatant and filtering, and then, cooling and crystallizing filtrate copper sulfate solution in the step 5); filter residue (the main component is CuO) can be returned to the step 8) for circulation and first-stage absorption of tail gas;
9) secondary absorption of tail gas:
the tail gas (the main component is still SO) remained after the first-stage absorption treatment of the tail gas2) Introducing into NaOH solution in a tail gas secondary absorption tank, keeping the pH value to be more than 9, performing tail gas secondary absorption to generate absorption liquid NaSO3(ii) a The absorption liquid is regenerated with CaO to generate CaSO3And NaOH, and recycling the NaOH to absorb the tail gas SO again2(ii) a Calcium sulfate product is obtained by filtration, and tail gas SO is generated in the process2Has an absorption of 99.9%;
the main reaction formula is as follows:
SO2+2NaOH＝Na2SO3；
Na2SO3+CaO+H2O＝CaSO3↓+2NaOH。
the foregoing is considered to be merely illustrative of the present invention and is not intended to be limiting thereof, since any modifications, equivalents, improvements and the like which come within the spirit and scope of the invention are intended to be included within the scope of the system architecture and method of the present invention.
Claims (5)
1. The method for comprehensively utilizing and treating the molybdenum-copper slag is characterized by comprising 9 steps of drying, grinding, washing, first pressure filtration, washing liquid treatment, alkaline leaching of filter residue, second pressure filtration, primary absorption of tail gas and secondary absorption of the tail gas:
1) and (3) drying: drying the molybdenum-copper slag with the water content of 0-40%, and flatly paving the molybdenum-copper slag on a dryer when the molybdenum-copper slag is dried, wherein the thickness of a material layer is 5-50 cm; the drying and heating temperature is 180-300 ℃, and the drying time is 8-20 hours; tail gas generated in the drying process enters the subsequent step 8) and step 9) for tail gas absorption treatment;
2) grinding: and (3) crushing and grinding the dried molybdenum-copper slag by a Raymond mill or a rod mill to ensure that the granularity reaches D97: 50 μm;
3) washing: stirring and washing the finely ground molybdenum-copper slag solid material and industrial water for 1-3 hours at normal temperature according to the solid-liquid ratio of 1: 2-1: 5;
4) primary filter pressing: after washing, carrying out solid-liquid separation by first filter pressing through a filter press to obtain first filter pressing filter residue and first filter pressing washing liquid; the first filter pressing washing liquid directly enters the subsequent step 5), or returns to the step 3) to participate in washing again; the washing liquid after 1-6 times of circulating washing and filter pressing enters the subsequent step 5) for washing liquid treatment; carrying out alkaline leaching on the first filter residue in the subsequent step 6);
5) and (3) washing liquid treatment: the main component of the first filter pressing washing liquid is copper sulfate solution, and Cu enriched in the first filter pressing washing liquid2+The concentration is more than 10 g/l; cooling and crystallizing the first filter pressing washing liquid and the tail gas first-stage absorption filtrate copper sulfate solution obtained in the step 8) at the temperature of 0-10 ℃, and filtering to obtain CuSO with the mass fraction of more than 99%4.5H2O, wherein the recovery rate of Cu is more than 98 percent; the filtered mother liquor is cooled and crystallized again;
6) alkaline leaching of filter residue: mixing and size mixing the first filter-pressing filter residue and industrial water according to the solid-liquid weight ratio of 1: 2-1: 4, adding NaOH solution for alkaline leaching reaction, heating to 60-90 ℃, stirring for 1-4 hours until the pH value reaches 10-14 at the end of the reaction;
7) and (3) secondary filter pressing: after the alkaline leaching of the filter residue is finished, carrying out secondary filter pressing and solid-liquid separation to obtain secondary filter pressing filter residue and secondary filter pressing filtrate; evaporating the second filter pressing filtrate to dryness to obtain a sodium tungsten molybdate product, namely a mixture of sodium tungstate and sodium molybdate; the purity of the sodium tungsten molybdate reaches more than 98 percent, and the recovery rate of the tungsten and the molybdenum is more than 97 percent; the main component of the secondary filter pressing filter residue is copper oxide, and the secondary filter pressing filter residue enters a subsequent step 8) for primary absorption of tail gas;
8) primary absorption of tail gas:
mixing the secondary filter-pressing filter residue copper oxide and industrial water in a solid-to-liquid ratio of 1: 1-1: 4 in a primary absorption tank, and carrying out size mixing on tail gas SO generated in the drying process2Introducing into a first-stage absorption tank, and stirring by adopting compressed air;
sampling and inspecting the concentration of copper ions in the primary absorption tank, when the concentration is more than 10g/l, extracting supernatant and filtering, and then, cooling and crystallizing filtrate copper sulfate solution in the step 5); returning filter residue CuO to the step 8) for primary absorption of tail gas in a circulating way;
9) secondary absorption of tail gas:
the residual tail gas SO after the primary absorption treatment of the tail gas2Introducing into NaOH solution in tail gas secondary absorption tank, maintaining pH value greater than 9, performing tail gas secondary absorption to generate absorption liquid Na2SO3(ii) a The absorption liquid is regenerated with CaO to generate CaSO3And NaOH, and recycling the NaOH to absorb the tail gas SO again2(ii) a Calcium sulfate product is obtained by filtration, and tail gas SO is generated in the process2The absorption rate of (a) was 99.9%.
2. The method for comprehensively utilizing and treating molybdenum-copper slag according to claim 1, wherein a drying heat source adopts high-temperature steam, electric heating or microwaves.
3. The method for comprehensively utilizing and treating the molybdenum-copper slag according to claim 1, wherein in the step 6), the main reaction formula is as follows:
MoO3+2NaOH＝Na2MoO4；
WO3+2NaOH＝Na2WO4。
4. the method for comprehensively utilizing and treating the molybdenum-copper slag according to claim 1, wherein in the step 8), the main reaction formula is as follows:
CuO+SO2+O2＝CuSO4。
5. the method for comprehensively utilizing and treating the molybdenum-copper slag according to claim 1, wherein in the step 9), the main reaction formula is as follows:
SO2+2NaOH＝Na2SO3；
Na2SO3+CaO+H2O＝CaSO3↓+2NaOH。
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| CN109971969A (en) * | 2019-04-17 | 2019-07-05 | 成都虹波钼业有限责任公司 | A kind of method of environmentally protective processing molybdenum copper ashes |
| CN111807411A (en) * | 2020-08-10 | 2020-10-23 | 成都虹波钼业有限责任公司 | Method for removing and recycling vanadium in molybdate by using copper salt |
| CN112831660B (en) * | 2020-12-30 | 2022-09-13 | 成都虹波钼业有限责任公司 | Process for comprehensively utilizing molybdenum ore leaching slag |
| CN115010167B (en) * | 2022-05-10 | 2023-07-04 | 成都虹波钼业有限责任公司 | Novel process for recycling calcium silicate slag containing copper and molybdenum |
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| CN109468468A (en) | 2019-03-15 |
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