CN102230075A - Dephosphorizing process of molybdenum nickel ore - Google Patents
Dephosphorizing process of molybdenum nickel ore Download PDFInfo
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Abstract
The invention relates to a molybdenum nickel ore, in particular to a dephosphorizing process of the molybdenum nickel ore. According to the invention, the method comprises the steps of adopting sulphide ore (containing phosphorus) containing a molybdenum nickel component as a raw material; and oxidizing and roasting the sulphide ore to remove the phosphorus so as to obtain a low-phosphorus molybdenum nickel ore; adding carbon powder to the low-phosphorus molybdenum nickel ore according to the phosphorus content; and then placing the low-phosphorus molybdenum nickel ore in a microwave vacuum furnace to be sintered; adjusting microwave heating frequency and power so as to carry out carbon reduction reaction through microwave in a vacuum state; volatilizing product gaseous elemental phosphorus and the generated CO to enter a gas exhaust passage and recycling the phosphorus and the CO to obtain white phosphorus; and magnetically separating a solid product to obtain the low-phosphorus molybdenum nickel ore.
Description
Technical field
The present invention relates to the molybdenum nickel minerals, refer in particular to a kind of dephosphorizing method of molybdenum nickel minerals.
Background technology
Nickel, molybdenum are the important strategic metals, because its unique physics and chemical property, become matrix, main component or the additive of advanced configuration material and functional materials,, be widely used in fields such as national economy and defence and military as nickel base superalloy, nickel-molybdenum alloy steel etc.; To the large scale mining of Mineral resources, the situation of resource retained reserve shortage has appearred in the global range along with in recent decades, China's rapid economy development in recent years particularly, and imbalance between supply and demand strengthens, and nonferrous metal prices such as nickel, molybdenum rise violently; And the nickel-molybdenum ore distinctive a kind of multi-metal complex mineral wealth that are China, mainly be distributed in ground such as zunyi, guizhou, Xiang Xibei, Hubei Duchang, Fuyang, Zhejiang, the common feature of China's nickel-molybdenum ore be nickel and molybdenum in the nickel-molybdenum ore the occurrence status complexity, grade is not high, mineral are various, foreign matter content is high, makes that the ore dressing difficulty is big, the decomposition of mineral, separate impurities difficulty be big; Existing beneficiation test proves, the effort of selecting qualified concentrated molybdenum ore and nickel ore concentrate with the method for ore dressing from this type of ore is all unsuccessful, very difficult choosing, promptly these mineral do not possess the special property of ore dressing, composition and composition are also relatively unique, and this project is orientated these class mineral as in " the difficult separate complex of low ore grade nickel molybdenum ore deposit "; Occurring in nature molybdenum nickel minerals with sulphur phosphorus association be in the same place, and sulphur phosphorus can cause the hot-short and cold short of steel, is necessary very much to remove in preparation process, perhaps is reduced to tracer level.
Mainly contain in the existing progress in this field before: for the difficult separate complex of the low ore grade nickel molybdenum ore deposit that this project proposes, existing at present two kinds of exploration schemes: the one, nickel-molybdenum ore pyrogenic process-wet method bonded smelting technology; The 2nd, the full wet method smelting process of nickel-molybdenum ore, pyrogenic process-wet method process combined, its principal character is to have applied mechanically processing molybdenum glance smelting technology, adopts the desulfurization with roasting technique of pyrogenic process to adopt the wet method extract technology again, reagent consumption is big, the cost height; More crucial is: when adopting this pyrogenic process-wet method process combined, the nickel in the nickel-molybdenum ore is difficult to efficient recovery, and the leaching yield of molybdenum also is difficult to reach more than 90%; Continue it, have proposition to adopt wet method to extract the molybdenum technology of pyrogenic process extraction nickel again, the difficulty of this route is owing to the molybdenum ore complicated component, and particularly when the nickelous sulfide existence, the leaching yield of molybdenum is low, and remaining impurity will consume a large amount of acid and directly have influence on the rate of recovery of metal; Therefore, find, at present not at the efficient industrialized method of utilizing in the difficult separate complex of low ore grade nickel molybdenum ore deposit from the prior art investigation; Undoubtedly, along with the further exploitation of rich ore, and global tight demand to nickel, molybdenum, reclaiming the nickel molybdenum from the low ore grade nickel molybdenum ore has become the current problem that presses for solution.
Chinese patent 99114736.7 provides a kind of processing method that molybdenum-nickel paragenetic raw ore is directly leached preparation molybdenum nickel salt with weak base and oxygenant, with the molybdenum-nickel paragenetic green ore through broken ball milling, use weak base and oxygenant leaching, filtration, ammonia still process then, solution extraction is produced ammonium molybdate, and raffinate solution obtains single nickel salt through operations such as evaporation concentration again; This method equipment is simple, easy to operate, does not produce the three wastes, belongs to hydrometallurgy, and weak point is the process more complicated, and reagent consumption is big, the cost height; Chinese patent 200810132538.2 provides a kind of method for extracting molybdenum and nickel by molybdenum nickel ore whole wet method, the full wet method that is black series of rocks molybdenum nickel minerals is extracted molybdenum nickel method, it is characterized in that its leaching process carries out pressure oxidation with levigated molybdenum nickel minerals and leaches, obtain the nickel leach liquor of nickeliferous and molybdenum and the leached mud of molybdenum-containing oxide; Again leach liquor is carried out extracting and separating molybdenum nickel, output nickel salt and ammonium molybdate or molybdic oxide; Molybdenum in the leached mud carried out normal pressure alkali soaks, purifies, the heavy ammonium molybdate of acid is reclaimed again, weak point is the hydrometallurgy process complexity, and reagent consumption is big, the cost height, and molybdenum nickel recovery rate still has room for promotion.
Mention in the document " manganese ore powder microwave heating dephosphorization under reducing atmosphere " (Chen Jin of Institutes Of Technology Of Taiyuan): microwave heats the carbon containing manganese ore in closed system, the solid state reduction dephosphorization can reach 40%-60%, dephosphorization efficient is lower, do not reach the high dephosphorization rate requirement that requires in the present dephosphorization metallurgy, remain further to be adjusted the metallurgical process parameter and realize high dephosphorization effect; Document " technology of slag dephosphorization under reducing atmosphere in microwave field " (Lv Yan of Institutes Of Technology Of Hebei) is mentioned: in 1100-1400 ℃, utilize microwave heating that the carbothermic reduction behavior of bessemer furnace slag is studied.But without any processing, if directly emptying, gaseous state phosphorus can polluted air to product phosphorus, so the recovery measure that should be necessary gaseous product behind the dephosphorization under reducing atmosphere.
Summary of the invention
This patent proposes to place vacuum atmosphere to carry out microwave heating dephosphorization system, can play the promotion dephosphorisation reaction, improves the purpose of dephosphorization rate; And proposition is provided with proprietary product gas recovery approach in heating unit; gaseous state phosphorus in the energy efficient recovery dephosphorization product; both protected environment; have and to reclaim useful matter; comprehensively think: method provided by the invention be based on pyrometallurgy and, physical field metallurgy and vacuum metallurgy principle, purpose is high-level efficiency, high quality, low cost, the low low-phosphorous Mo-Ni alloy of preparation that pollutes.
The objective of the invention is to be achieved through the following technical solutions:
The first step is that raw material is prepared: choose the molybdenum nickel ores, grind powder process, carry out the oxidizing roasting desulfurization; Maturing temperature is lower than 600 ℃, fully oxygen supply, and control roasting terminal point sulphur content is less than 2.0%.
Second the step be the batching: in low-sulfur molybdenum nickel minerals powder with addition of a certain amount of coke powder, according to phosphorus pentoxide content, according to reaction equation 2Ca
3(PO
4)
2+ 10C=6CaO+P
4↑+10CO ↑, according to calculating, need be 96.8% of phosphorus content with addition of effective carbon amount, for promote that the dephosphorization under reducing atmosphere sufficient reacting carries out, the loss of carbon, the reduction consumption of molybdenum nickel oxide, need the carbon surplus,, determine that the carbon coefficient of excess is 1.5 ~ 2.0 according to experiment, promptly on phosphorus content 96.8% basis, increase by 50% ~ 100% with addition of amount, join behind the carbon mixing in addition.
The 3rd step was to vacuumize: off-response stove, vacuum tightness are set in the rough vacuum scope of 100 ~ 200Pa, stop vacuum pumping after vacuum reaches, and close the valve of body of heater and vacuum tunnel; And open top generation air seal passage simultaneously, see Fig. 1 for details.
The 4th step was to carry out the microwave vacuum thermal reduction in the microwave vacuum stove, main control parameters has: microwave frequency 2.45GHz, it is conventional industrial microwave frequency, adjustable power, frequency setting is at 2.45GHz, and when phosphorus content was lower than 5%, microwave power was between 50 ~ 300kW, when phosphorus content was higher than 5%, microwave power was set between 300 ~ 500kW.In setting range, phosphorus content is high more, and selected microwave power is big more; Be controlled at 20 ~ 40min heat-up time, increase along with the increase of handling the fine ore amount, reduction temperature is controlled at 1000 ~ 1150 ℃; In addition, the P that in this process, generates
4With CO gas evolution access to plant top gas barrier, obtain solid-state white phosphorus through after the water cooling; Solid product promptly is molybdenum nickel powder, excess carbon and Calucium Silicate powder and calcium oxide, and magnetic separation promptly obtains low-phosphorous molybdenum nickel powder after separating.
Compare with other documents, advantage of the present invention be mainly reflected in following some:
(1) compare with hydrometallurgy, operating process is short greatly, and master operation has " oxidation sweetening ", " joining the carbon mixing ", " microwave vacuum thermal reduction " and " solid product separates ", compares with hydrometallurgical extraction molybdenum nickel, and operating process shortens greatly;
(2) dephosphorization efficient height.Compare with traditional simple closed system, under the rough vacuum condition, more help the carrying out of dephosphorisation reaction, dephosphorization rate significantly improves, and 90% dephosphorization rate is brought up to more than 99% under the simple closed system;
(3) rate of recovery height of product phosphorus under the vacuum condition.Because the gas recovery passage is arranged, the effusion and the recovery of gas become possibility.Because the vacuum setting is arranged, promoted dephosphorisation reaction to carry out, the product gas growing amount is big, and the rate of recovery brings up to 74 ~ 76% by 60% under antivacuum;
(4) production cost is low, compares with hydrometallurgy, and reagent consumption and devices consume are few, and what need has only carbon dust with addition of composition, and equipment mainly is the microwave vacuum stove, has been sophisticated industrialization equipment now; Energy conservation and consumption reduction effects is obvious, has given full play to the advantages such as " globality, high efficiency, less energy-consumption " of microwave heating;
(5) simple to operate, grasp easily, compare, the pure fire metallurgy process mechanization degree height that the present invention adopts with hydrometallurgy, pyrogenic process/wet-mixed metallurgy, the mixing and the microwave vacuum thermal reduction of joining behind the carbon can realize mechanized operation, and process control is easy.
Description of drawings
Fig. 1 is a vacuum microwave heating dephosphorization device synoptic diagram, every representative respectively among the figure: 1 vacuum pump; 2 vacuum pipes; 3 vacuum valves; 4 gas recovery passages; 5 liquid waters; 6 gas recovery bottles; 7 materials; 8 magnetrons.
Embodiment
The invention will be further elaborated below in conjunction with embodiment, and embodiment only is used to illustrate the present invention, rather than limit the present invention by any way.
Embodiment one: the preparation method and the metallurgical effect of the low-phosphorous molybdenum nickel minerals of 10kg molybdenum nickel raw ore, 4.23% phosphorus content
Batching in the coke effectively carbon content be 6.26%, i.e. 0.626 kg;
Microwave parameters is provided with: vacuum tightness 110Pa in the stove, frequency 2.45GHz, power 200kW, 1020 ℃ of reduction temperatures, recovery time 25min;
Reclaim solid white phosphorus amount: 0.323 kg, the white phosphorus rate of recovery 76%;
Table 1 has been listed [P]=4.23% o'clock microwave vacuum thermal reduction and has been handled principal element content in the molybdenum nickel minerals of front and back;
Principal element content correlation data in the molybdenum nickel minerals before and after table 1 [P]=4.23% o'clock microwave vacuum thermal reduction is handled
| ? | Ni | Mo | S | P | Fe | C | V |
| After original 120 ℃ of oven dry | 8.79 | 12.81 | 42.24 | 4.23 | 16.95 | 13.09 | 1.23 |
| Behind the microwave vacuum dephosphorization | 14.87 | 22.05 | 1.02 | 0.04 | 54.23 | 3.56 | 4.23 |
Test result shows: behind the microwave vacuum dephosphorization, end phosphorus content reaches required low-phosphorous requirement, dephosphorization rate 99.1%.
Embodiment two: the preparation method and the metallurgical effect of the low-phosphorous molybdenum nickel minerals of 20kg molybdenum nickel raw ore, 5.01 % phosphorus contents
Batching in the coke effectively carbon content be 7.42%, i.e. 0.742kg;
Microwave parameters is provided with: vacuum tightness 100Pa in the stove, microwave frequency 2.45GHz, power 450kW, 1150 ℃ of reduction temperatures, recovery time 38min;
Reclaim solid white phosphorus amount: 0.755 kg, the rate of recovery is 75%;
Table 2 has been listed [P]=5.01% o'clock microwave vacuum thermal reduction and has been handled principal element content in the molybdenum nickel minerals of front and back;
Principal element content correlation data in the molybdenum nickel minerals before and after table 2 [P]=5.01% o'clock microwave vacuum thermal reduction is handled
| ? | Ni | Mo | S | P | Fe | C | V |
| After original 120 ℃ of oven dry | 9.79 | 11.94 | 42.23 | 5.01 | 16.85 | 12.51 | 1.68 |
| Behind the microwave vacuum dephosphorization | 15.34 | 22.05 | 0.98 | 0.04 | 53.54 | 4.16 | 3.89 |
Test result shows: behind the microwave vacuum dephosphorization under reducing atmosphere, end phosphorus content reaches required low-phosphorous requirement, dephosphorization rate 99.2%.
Embodiment three: the preparation technology and the metallurgical effect of the low-phosphorous molybdenum nickel minerals of 30kg molybdenum nickel raw ore, 8.75 % phosphorus contents
Batching in the coke effectively carbon content be 7.42%, i.e. 0.742kg;
Microwave parameters is provided with: vacuum tightness 95Pa in the stove, microwave frequency 2.45GHz, power 300kW, 1100 ℃ of reduction temperatures, recovery time 30min;
Reclaim solid white phosphorus amount: 1.943 kg, the rate of recovery is 74%;
Table 3 has been listed [P]=8.75% o'clock microwave vacuum thermal reduction and has been handled principal element content in the molybdenum nickel minerals of front and back;
Principal element content in the molybdenum nickel minerals before and after table 3 [P]=8.75% o'clock microwave vacuum thermal reduction is handled
| ? | Ni | Mo | S | P | Fe | C | V |
| After original 120 ℃ of oven dry | 8.92 | 12.18 | 40.35 | 8.75 | 17.35 | 11.68 | 0.77 |
| Behind the microwave vacuum dephosphorization | 15.23 | 24.24 | 1.01 | 0.04 | 52.98 | 3.44 | 3.06 |
Test result shows: behind the microwave vacuum dephosphorization under reducing atmosphere, end phosphorus content reaches required low-phosphorous requirement, and dephosphorization rate is 99.5%.
Embodiment four: the sealing but under the non-vacuum condition, the preparation method and the metallurgical effect of the low-phosphorous molybdenum nickel minerals of 20kg molybdenum nickel raw ore, 5.01 % phosphorus contents
Batching in the coke effectively carbon content be 7.42%, i.e. 0.742kg;
Microwave parameters is provided with: system in the closed furnace, but antivacuum.Microwave frequency 2.45GHz, power 450kW, 1150 ℃ of reduction temperatures, recovery time 38min;
Reclaim solid white phosphorus amount: 0.618kg, the rate of recovery is 60.5%;
Table 4 has been listed [P]=5.01% o'clock microwave vacuum thermal reduction and has been handled principal element content in the molybdenum nickel minerals of front and back;
Principal element content correlation data in the molybdenum nickel minerals before and after table 4 [P]=5.01% o'clock microwave vacuum thermal reduction is handled
| ? | Ni | Mo | S | P | Fe | C | V |
| After original 120 ℃ of oven dry | 9.79 | 11.94 | 42.23 | 5.01 | 16.85 | 12.51 | 1.68 |
| Behind the microwave sealing dephosphorization | 15.34 | 22.05 | 0.98 | 0.5 | 53.52 | 4.16 | 3.89 |
Test result shows: in antivacuum closed system, behind the microwave reduction dephosphorization, even end phosphorus content does not reach the requirement of required low-phosphorous (500ppm, 0.05%).Dephosphorization rate 90%.
Claims (5)
1. the dephosphorizing method of a molybdenum nickel minerals, to obtain low-sulfur molybdenum nickel minerals after the molybdenum nickel minerals process oxidizing roasting desulfurization, in low-sulfur molybdenum nickel minerals according to phosphorus content with addition of carbon dust, to with addition of the low-sulfur molybdenum nickel minerals of carbon dust in microwave heating installation, adopt the microwave thermal reduction method, adjust microwave power at reduction phase, promote the dephosphorization under reducing atmosphere reaction, when producing low-phosphorous Mo-Ni alloy, reclaim elemental phosphorously, it is characterized in that: the vacuum tightness of microwave heating installation is in the rough vacuum scope of 100 ~ 200Pa.
2. the dephosphorizing method of a kind of molybdenum nickel minerals as claimed in claim 1 is characterized in that: carbon dust is to increase by 50% ~ 100%, 96.8% of the quality that described balance carbon amount is a phosphorus in the molybdenum nickel minerals on the basis of balance carbon amount quality with addition of amount.
3. the dephosphorizing method of a kind of molybdenum nickel minerals as claimed in claim 1, it is characterized in that: microwave frequency is set in 2.45GHz, and when phosphorus content was lower than 5%, microwave power was between 50 ~ 300kW, when phosphorus content was higher than 5%, microwave power was set between 300 ~ 500kW; In setting range, phosphorus content is high more, and selected microwave power is big more; Be controlled at 20 ~ 40min heat-up time, increase along with the increase of handling the fine ore amount, reduction temperature is controlled at 1000 ~ 1150 ℃.
4. the dephosphorizing method of a kind of molybdenum nickel minerals as claimed in claim 1, it is characterized in that: have the exhaust-duct to link to each other at the microwave heating installation top with the extraneous gas retrieving arrangement, elemental phosphorous steam that reduction is produced and CO mixed gas feed in the cold water and cool off, obtain the solid white phosphorus, the white phosphorus rate of recovery is 74 ~ 76%.
5. the dephosphorizing method of a kind of molybdenum nickel minerals as claimed in claim 1 is characterized in that: with the concrete grammar that obtains low-sulfur molybdenum nickel minerals after the molybdenum nickel minerals process oxidizing roasting desulfurization be: choose the molybdenum nickel ores, grind powder process, carry out the oxidizing roasting desulfurization; Maturing temperature is lower than 600 ℃, fully oxygen supply, and control roasting terminal point sulphur content is less than 2.0%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534200A (en) * | 2012-03-30 | 2012-07-04 | 湖南航天工业总公司 | Method using microwave sintering to extract molybdenum in nickel molybdenum ore |
| CN105803189A (en) * | 2016-05-16 | 2016-07-27 | 贵州大学 | Method for efficiently removing phosphorus from high-phosphorus oolitic hematite |
| CN107312915A (en) * | 2017-08-30 | 2017-11-03 | 安徽省含山县潮林铸管厂（普通合伙） | A kind of method of iron casting dephosphorization |
| CN110396593A (en) * | 2019-09-05 | 2019-11-01 | 东北大学 | A kind of method of high phosphorus iron ore concentrate high-temperature vapor roasting-acidleach dephosphorization |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101259450A (en) * | 2008-03-12 | 2008-09-10 | 中南大学 | High-efficiency ore sorting technique for nickel-molybdenum mineral |
| CN101302586A (en) * | 2008-07-03 | 2008-11-12 | 太原理工大学 | Microwave heating, solid state reduction and gaseous dephosphorization method for manganese ore powder |
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2011
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101259450A (en) * | 2008-03-12 | 2008-09-10 | 中南大学 | High-efficiency ore sorting technique for nickel-molybdenum mineral |
| CN101302586A (en) * | 2008-07-03 | 2008-11-12 | 太原理工大学 | Microwave heating, solid state reduction and gaseous dephosphorization method for manganese ore powder |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534200A (en) * | 2012-03-30 | 2012-07-04 | 湖南航天工业总公司 | Method using microwave sintering to extract molybdenum in nickel molybdenum ore |
| CN105803189A (en) * | 2016-05-16 | 2016-07-27 | 贵州大学 | Method for efficiently removing phosphorus from high-phosphorus oolitic hematite |
| CN105803189B (en) * | 2016-05-16 | 2018-06-29 | 贵州大学 | A kind of method of phosphorus in efficient removal high-phosphor oolitic hematite |
| CN107312915A (en) * | 2017-08-30 | 2017-11-03 | 安徽省含山县潮林铸管厂（普通合伙） | A kind of method of iron casting dephosphorization |
| CN110396593A (en) * | 2019-09-05 | 2019-11-01 | 东北大学 | A kind of method of high phosphorus iron ore concentrate high-temperature vapor roasting-acidleach dephosphorization |
| CN110396593B (en) * | 2019-09-05 | 2020-10-23 | 东北大学 | Method for high-temperature steam roasting-acid leaching dephosphorization of high-phosphorus iron concentrate |
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