CN109457116B - Financial separation method for neodymium iron boron waste flash roasting supergravity slag - Google Patents
Financial separation method for neodymium iron boron waste flash roasting supergravity slag Download PDFInfo
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
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Abstract
The invention discloses a method for dividing neodymium iron boron waste flash roasting hypergravity slag into money, which is characterized in that neodymium iron boron waste and cosolvent are mixed and then sprayed into a high-temperature vertical reaction tower space together with mixed gas through a nozzle, the material is in a highly dispersed floating state and drifts from the upper end to the lower end of the reaction tower, the rare earth in the material is quickly and fully oxidized by controlling the oxidizing atmosphere in the reaction tower, iron is not oxidized as much as possible, and a small amount of oxidized iron is reduced into metal iron when passing through a red-hot coke layer arranged above a sedimentation tank. After being discharged, the high-temperature mixed melt of the molten iron and the rare earth slag enters the supergravity slag separator through the chute, the molten iron penetrates through the porous ceramic filter membrane under the action of supergravity, and the rare earth slag is retained in the rotary drum, so that the high-efficiency enrichment and separation of the rare earth and the iron in the neodymium iron boron waste are realized, the defects that the traditional neodymium iron boron waste treatment method is long in flow, high in energy consumption, capable of oxidizing the rare earth and the iron simultaneously, incapable of separating the rare earth and the iron before acid dissolution, large in acid leaching slag amount, low in rare earth recovery rate, difficult in iron resource recovery and the like are overcome, and the high-temperature mixed melt has good economic and environmental benefits.
Description
Technical Field
The invention relates to a financial separation method for flash roasting of hypergravity slag by neodymium iron boron waste, and belongs to the technical field of rare earth metallurgy.
Background
Neodymium iron boron is a magnetic material, is the latest result of development of rare earth permanent magnetic materials, is called as 'magical king' due to excellent magnetic performance, and is widely applied to various fields. During the production process of the neodymium iron boron magnetic material, about 20-25% of waste materials are generated, and most of the waste materials belong to neodymium iron boron oil sludge. These wastes contain about 60% iron and around 30% rare earth elements. The recycling of the neodymium iron boron waste material not only reasonably utilizes resources, but also reduces the environmental pollution.
At present, neodymium iron boron oil sludge waste is roasted by adopting a two-section rotary kiln, and then processes of leaching, extraction, precipitation, ignition and the like are carried out to recover rare earth in the neodymium iron boron oil sludge waste. The first stage of rotary kiln roasting mainly removes neodymium and ironThe oil in the boron oil sludge provides a raw material for the second-stage deep oxidation, but due to the inherent defects of the rotary kiln, the temperature and the atmosphere cannot be accurately controlled, the oil removal process is often insufficient in combustion, the energy consumption is high, black smoke is often emitted, and the environment is polluted. The second stage of rotary kiln roasting is used for respectively oxidizing rare earth and iron into RE (rare earth) as much as possible2O3And Fe2O3Because the oxidation reaction rate of the rotary kiln is low, the high oxidation rate can be achieved within 4-8 hours, and because two sections of rotary kilns are adopted, the rotary kiln has large volume, large occupied area and large external heat dissipation area, and simultaneously, a hot-cold alternative link exists, so the energy consumption is high. In addition, because rare earth and iron are simultaneously oxidized and then leached by hydrochloric acid, a large amount of iron in the waste enters acid leaching slag, the amount of slag is large, the total amount of rare earth taken away by the slag is large, the total recovery rate of the rare earth is reduced, the leaching slag is difficult to be comprehensively utilized, and the leaching slag is often stockpiled to cause environmental pollution.
Disclosure of Invention
The invention aims to overcome the defects of a traditional neodymium iron boron waste recovery method and provides a method for separating supergravity slag in a neodymium iron boron waste flash roasting manner.
a. After the powdery neodymium iron boron waste material and the cosolvent are mixed, the mixed gas and the mixed gas are sprayed into a reaction tower (2) with the height of 2.0-25.0 meters and the temperature of 400-1600 ℃ through a nozzle (1), the material is floated from the upper end to the lower end of the reaction tower in a highly dispersed floating state, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-25-10-5atm, the rare earth in the material is rapidly oxidized to form a rare earth slag phase with the added fluxing agent, most of iron is not oxidized, and a small amount of iron is oxidized into ferroferric oxide or ferric oxide. When the roasted product falls into a sedimentation tank (4) below the reaction tower, the roasted product passes through a hot coke layer arranged above the sedimentation tank, the temperature of the coke layer is 1000-1600 ℃, and iron oxide is reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a slag discharge port (5) and enters a supergravity slag financial divider through a chute.
b. The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filter membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device. The rotating speed of the revolving drum speed regulating motor (15) and the melt feeding speed are adjusted, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the revolving drum.
And further, discharging the roasting flue gas in the step a from a flue (3), and exhausting after dust collection.
Further, in the step b, when the rare earth slag is accumulated to a certain thickness, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Further, the powdery neodymium iron boron waste is a material with or without oil, and the granularity of the powdery neodymium iron boron waste is below 50 meshes.
Further, the mixed gas is a mixture of inert gas and oxygen, the inert gas is nitrogen or argon, and the mass percentage concentration of the oxygen is 30-100%.
Further, the fluxing agent is SiO2、CaO、MgO、Al2O3、B2O3The particle size of the one or more of the above (B) is 50 meshes or less.
Furthermore, the adding amount of the fluxing agent is 1-30% of the weight of the waste material
Compared with the traditional neodymium iron boron waste recovery method, the method for dividing the flash roasting supergravity slag of the neodymium iron boron waste has the following advantages: (1) by adopting a flash oxygen-controlled roasting technology, the powdery neodymium iron boron waste and the mixed gas are sprayed into the space of the high-temperature reaction tower together, so that the material is in a highly dispersed floating state and is fully contacted with the gas, superior reaction kinetic conditions are provided, meanwhile, the rare earth in the material can be rapidly and fully oxidized by accurately controlling the oxygen potential, the oxidation rate is higher than 99.0 percent, and the iron is not oxidized as much as possible. (2) The whole reaction time of flash roasting is only ten seconds short, which is far lower than that of a rotary kiln for several hours, the temperature of a furnace body is accurately controlled, and the energy consumption is greatly reduced; because the furnace body has good sealing performance, the furnace is environment-friendly. (3) The high-temperature incandescent coke layer is arranged above the sedimentation tank, and can fully reduce iron oxides into metallic iron, thereby being beneficial to separating iron and rare earth in the waste in one step without adopting methods such as magnetic separation and the like. (4) The super-gravity slag financial separation is adopted to realize the collection of fine and dispersed iron particles mixed in the rare earth slag phase, and the slag and gold are thoroughly separated. (5) Before acid leaching, the iron and the rare earth in the waste are separated and respectively enriched, so that the consumption of hydrochloric acid is reduced, the acid leaching residue amount is greatly reduced, the total amount of the rare earth taken away by the residue is greatly reduced, and the total recovery rate of the rare earth is improved. In addition, the iron-rich phase after magnetic separation is convenient for comprehensive utilization of iron resources.
The invention can be widely applied to recovering valuable metals from various powdery neodymium iron boron wastes, and has good popularization and application values.
Drawings
FIG. 1: the process flow of the invention is schematically illustrated.
FIG. 2: the structure of the flash roasting equipment adopted by the invention is shown schematically.
In FIG. 2, 1 is a nozzle, 2 is a reaction tower, 3 is a flue, 4 is a sedimentation tank, and 5 is a mixed melt discharge port.
FIG. 3: the invention adopts a structural schematic diagram of the supergravity slag finance branch equipment.
In the figure 3, 6 parts of a feeding pipe, 7 parts of a distributing device speed regulating motor, 8 parts of an exhaust port, 9 parts of a distributing device, 10 parts of a porous ceramic filtering membrane, 11 parts of a rotary drum central column, 12 parts of a molten iron outlet, 13 parts of a scraper hydraulic rod, 14 parts of a scraper, 15 parts of a rotary drum speed regulating motor, 16 parts of a shock absorber and 17 parts of a rare earth slag outlet.
Detailed Description
The invention will now be further described with reference to the following examples, which are intended to illustrate the invention but not to limit it further.
Example 1:
mixing the powdery neodymium iron boron waste with the granularity of 80 meshes and SiO accounting for 5 percent of the weight of the waste2After the powder is mixed evenly, the powder and mixed gas (oxygen content is 50 percent) of nitrogen and oxygen are sprayed into a reaction tower (2) with the height of 2.5 meters and the temperature of 1200 ℃ through a nozzle (1), and the materials are dispersed highly and float from the upper end of the reaction towerFalls to the lower end, during which the oxygen partial pressure in the reaction column is controlled to 10-20atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.24%, 78% of iron in the waste is not oxidized, 15% of iron is oxidized into ferroferric oxide, and 7% of iron is oxidized into ferric oxide. When the roasted product drifts to a sedimentation tank (4) below the reaction tower, the roasted product passes through a hot coke layer which is arranged above the sedimentation tank and has the temperature of 1350 ℃, and ferroferric oxide and ferric oxide are reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a discharge port (5) and enters a supergravity slag financial separator through a chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor from a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 200 r/min. The rotating speed of the rotary drum speed regulating motor (15) is adjusted to 400r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the rotary drum. When the thickness of the rare earth slag is accumulated to 10cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Example 2:
uniformly mixing powdery neodymium iron boron waste with the granularity of 100 meshes with CaO powder accounting for 6 percent of the weight of the waste, spraying the mixture together with mixed gas (oxygen content is 95 percent) of nitrogen and oxygen into a reaction tower (2) with the height of 3.5 meters and the temperature of 1350 ℃ from a nozzle (1), wherein the materials are dispersed highly and float from the upper end to the lower end of the reaction tower, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-15atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.65%, 71% of iron in the waste is not oxidized, 18% of iron is oxidized into ferroferric oxide, and 11% of iron is oxidized into ferric oxide. When the roasted product drifts to a sedimentation tank (3) below the reaction tower, the roasted product passes through a 1450 ℃ incandescent coke layer arranged above the sedimentation tank, and ferroferric oxide and ferric oxide are reduced into metallic iron. Discharging the high-temperature mixed melt of molten iron and rare earth slagThe port (5) is continuously or periodically discharged and enters the hypergravity slag finance separator through the chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 300 r/min. The rotating speed of the rotary drum speed regulating motor (15) is adjusted to 600r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the rotary drum. When the thickness of the rare earth slag is accumulated to 8cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Example 3:
mixing the powdery neodymium iron boron waste material with the granularity of 200 meshes with SiO accounting for 3 percent of the weight of the waste material2After the powder and 2 percent of CaO powder are uniformly mixed, the mixture is sprayed into a reaction tower (2) with the height of 5.5 meters and the temperature of 1500 ℃ together with the mixed gas of argon and oxygen (the oxygen content is 60 percent) through a nozzle (1), the materials are dispersed highly and float from the upper end to the lower end of the reaction tower, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-10atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.86%, 67% of iron in the waste is not oxidized, 21% of iron is oxidized into ferroferric oxide, and 12% of iron is oxidized into ferric oxide. When the roasted product drifts to a sedimentation tank (3) below the reaction tower, the roasted product passes through a 1550 ℃ incandescent coke layer arranged above the sedimentation tank, and ferroferric oxide and ferric oxide are reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a discharge port (5) and enters a supergravity slag financial separator through a chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 500 r/min. The rotating speed of the revolving drum speed regulating motor (15) is adjusted to 800r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the revolving drum. When the thickness of the rare earth slag is accumulated to 15cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Example 4:
mixing the powder neodymium iron boron waste material with the granularity of 300 meshes, 200-mesh MgO powder accounting for 0.5 percent of the weight of the waste material and 200-mesh B accounting for 0.5 percent of the weight of the waste material2O3After the powder is mixed evenly, the powder and mixed gas (oxygen content is 80%) of argon and oxygen are sprayed into a reaction tower (2) with the height of 10.0 m and the temperature of 1600 ℃ through a nozzle (1), the materials are dispersed highly and float from the upper end to the lower end of the reaction tower, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-25atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.97%, 54% of iron in the waste is not oxidized, 32% of iron is oxidized into ferroferric oxide, and 14% of iron is oxidized into ferric oxide. When the roasted product drifts to a sedimentation tank (3) below the reaction tower, the roasted product passes through a hot coke layer at 1200 ℃ arranged above the sedimentation tank, and ferroferric oxide and ferric oxide are reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a discharge port (5) and enters a supergravity slag financial separator through a chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 600 r/min. The rotating speed of the revolving drum speed regulating motor (15) is adjusted to 800r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the revolving drum. When the thickness of the rare earth slag is accumulated to 12cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Example 5:
mixing the powdery neodymium iron boron waste with the granularity of 50 meshes with 100 meshes of SiO accounting for 5 percent of the weight of the waste2Powder, 3% of 100 mesh Al2O3After the powder is mixed evenly, the powder and mixed gas (oxygen content is 100 percent) of argon and oxygen are sprayed into a reaction tower (2) with the height of 2.0 meters and the temperature of 1000 ℃ through a nozzle (1), the materials are dispersed highly and float from the upper end to the lower end of the reaction tower, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-10atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.98%, 51% of iron in the waste is not oxidized, 34% of iron is oxidized into ferroferric oxide, and 15% of iron is oxidized into ferric oxide. When the roasted product drifts to a sedimentation tank (3) below the reaction tower, the roasted product passes through a 1600 ℃ incandescent coke layer arranged above the sedimentation tank, and ferroferric oxide and ferric oxide are reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a discharge port (5) and enters a supergravity slag financial separator through a chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 800 r/min. The rotating speed of the rotary drum speed regulating motor (15) is adjusted to 900r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the rotary drum. When the thickness of the rare earth slag is accumulated to 15cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Example 6:
mixing the powdery neodymium iron boron waste with the granularity of 100 meshes with 50 meshes of SiO accounting for 18 percent of the weight of the waste2After the powder and 12 percent of MgO powder of 50 meshes are mixed uniformly, the mixture is sprayed into a reaction tower (2) with the height of 25.0 meters and the temperature of 400 ℃ together with the mixed gas of argon and oxygen (the oxygen content is 30 percent) through a nozzle (1), the materials are dispersed highly and float from the upper end to the lower end of the reaction tower, and in the process, the oxygen partial pressure in the reaction tower is controlled to be 10-5atm, rare earth in the material is rapidly oxidized by oxygen-enriched air, the oxidation rate is 99.56%, 81% of iron in the waste material is not oxidized, and 14% of iron is oxidized into tri (tetra) oxideIron, 5% of the iron was oxidized to iron sesquioxide. When the roasted product drifts to a sedimentation tank (3) below the reaction tower, the roasted product passes through a 1000 ℃ incandescent coke layer arranged above the sedimentation tank, and ferroferric oxide and ferric oxide are reduced into metallic iron. The molten iron and rare earth slag high-temperature mixed melt is continuously or periodically discharged from a discharge port (5) and enters a supergravity slag financial separator through a chute. The roasting smoke is discharged from the flue (3), and is exhausted after dust collection.
The high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device to 1000 r/min. The rotating speed of the rotary drum speed regulating motor (15) is adjusted to 1000r/min, so that the molten iron flows out from the molten iron outlet (12) through the porous ceramic filtering membrane, and the rare earth slag is trapped in the rotary drum. When the thickness of the rare earth slag is accumulated to 5cm, the feeding is stopped, the rare earth slag is scraped off by a scraper (14) and is discharged from a rare earth slag outlet (17).
Claims (5)
1. The method for financial separation of supergravity slag by flash roasting of neodymium iron boron waste is characterized by comprising the following steps of:
a. after the powdery neodymium iron boron waste material is mixed with the fluxing agent, the powdery neodymium iron boron waste material and the fluxing agent are sprayed into a reaction tower (2) with the height of 2.0-25.0 meters and the temperature of 400--25-10-5atm, the rare earth in the material is rapidly oxidized to form a rare earth slag phase with the added fluxing agent, most of iron is not oxidized, and a small amount of iron is oxidized into ferroferric oxide or ferric oxide; when the roasted product falls into a sedimentation tank (4) below the reaction tower, the roasted product passes through a hot coke layer arranged above the sedimentation tank, the temperature of the coke layer is 1000-1600 ℃, and iron oxide is reduced into metallic iron; the molten iron and the rare earth slag high-temperature mixed melt are continuously or periodically discharged from a discharge port (5); the roasting smoke is discharged from the flue (3), and is exhausted after dust collection;
b. the high-temperature mixed melt of the molten iron and the rare earth slag flows to a distributing device of the supergravity slag financial distributor through a feeding pipe (6), and the mixed melt is uniformly distributed on a porous ceramic filtering membrane (10) on the inner wall of the rotary drum by adjusting the rotating speed of a speed regulating motor (7) of the distributing device; adjusting the rotating speed of a revolving drum speed regulating motor (15) and the melt feeding speed to ensure that the molten iron flows out from a molten iron outlet (12) through a porous ceramic filtering membrane, and the rare earth slag is retained in the revolving drum; when the rare-earth slag is accumulated to a certain thickness, the feeding is stopped, the rare-earth slag is scraped off by a scraper (14) and is discharged from a rare-earth slag outlet (17).
2. The method of claim 1, wherein the powdered neodymium-iron-boron waste is an oily or non-oily material with a particle size of 50 mesh or less.
3. The method according to claim 1, wherein the mixed gas is a mixture of an inert gas and oxygen, the inert gas is nitrogen or argon, and the concentration of oxygen is 30-100% by mass.
4. The method of claim 1, wherein the flux is SiO2、CaO、MgO、Al2O3、B2O3The particle size of the one or more of (a) is 50 meshes or less.
5. A method according to claim 1, characterised in that the fluxing agent is added in an amount of 1-30% by weight of the scrap.
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