CN104946891A - Method for recycling molybdenum by smelting ferro-molybdenum at low temperature - Google Patents
Method for recycling molybdenum by smelting ferro-molybdenum at low temperature Download PDFInfo
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- CN104946891A CN104946891A CN201510427240.4A CN201510427240A CN104946891A CN 104946891 A CN104946891 A CN 104946891A CN 201510427240 A CN201510427240 A CN 201510427240A CN 104946891 A CN104946891 A CN 104946891A
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Abstract
Provided is a method for recycling molybdenum by smelting ferro-molybdenum at a low temperature. The method comprises the following steps that ammonium leaching residues, ammonium molybdate, molybdenum oxide powder, iron oxide powder, iron powder and reducing agents are added and evenly mixed into a cylindrical mixer, and a mixing material is obtained. The obtained mixing material is placed into a furnace lining induction furnace made of carbonic materials to be subjected to warming and heating. Under the condition of the temperature ranging from 1400 DEG C to 1600 DEG C, self-reaction is carried out to form smelting residues and ferro-molybdenum, iron residues separating is carried out on the material, and the ferro-molybdenum is obtained. According to the low-temperature smelting technology, the induction furnace is utilized to carry out heating, carbon powder which is cheaper than the aluminate powder is adopted by the reducing agent, the smelting temperature ranges from 1400 DEG C to 1600 DEG C, saltpeter and calcium fluoride which can generate polluted gas are not adopted by the auxiliaries, and the ferro-molybdenum which is suitable for steel industry using is prepared.
Description
Technical field
The invention belongs to comprehensive utilization of resources and molybdenum-iron preparing technical field, particularly a kind of method utilizing molybdenum industrial residue low temperature smelting molybdenum-iron to reclaim molybdenum.
Background technology
Molybdenum is one of important alloying element of Iron And Steel Industry, the aggregate consumption of World Molybdenum 80% for Iron And Steel Industry alloy addition.Steel grade adds intensity and the toughness (particularly high-temperature behavior) that molybdenum can improve steel, improves hardening capacity and the hardenability of steel part.When molybdenum interpolates iron and steel, usually add with forms such as molybdenum-iron, molybdenum oxide lump, ammonium molybdates, especially common with molybdenum-iron form.The molybdenum content of molybdenum-iron is all between 55% ~ 75% both at home and abroad at present, and the molybdenum-iron product molybdenum content of domestic main flow is all about 60%, and the preparation of these molybdenum-irons all adopts thermite process to prepare.
Tradition aluminothermy legal system is for molybdenum-iron smelting temperature more than 2000 DEG C, and heat is released mainly through metallothermic reduction process, and reductive agent used mainly contains goes back aluminium powder and ferrosilicon, but these two kinds of reductive agent prices are higher.Smelt in formulation auxiliaries at molybdenum-iron simultaneously and add nitre and Calcium Fluoride (Fluorspan), this can produce oxynitride in smelting process and fluoride gas pollutes.Adopt this traditional formula to carry out thermite process when preparing molybdenum-iron, mainly there is following shortcoming: 1) temperature of reaction is high, generally more than 2000 DEG C, and reaction process difficult control of temperature; 2) react the nitre used or fluorite can produce oxynitride or fluorochemical in preparation process, pollute.
For molybdenum-iron product, its fusing point is mainly by the impact of molybdenum content, and molybdenum content is higher, and the fusing point of molybdenum-iron also can be higher, and its fusing point of molybdenum-iron containing molybdenum 60% is 1800 DEG C.When molybdenum content lower than 50% time, the fusing point of molybdenum-iron also can greatly reduce, and corresponding preparation condition also can change, and low temperature molybdenum-iron smelting technology can be adopted to go to prepare molybdenum-iron, also can eliminate the auxiliary material producing exhaust emission simultaneously.Low-grade molybdenum-iron uses in steel mill and does not have any problem, because the element except molybdenum is mainly iron.Therefore study low temperature molybdenum-iron and smelt new technology, decontamination, reducing energy consumption is a significantly job.
Summary of the invention
In order to overcome the shortcoming of above-mentioned prior art, a kind of low temperature smelting molybdenum-iron is the object of the present invention is to provide to reclaim the method for molybdenum, by low temperature smelting technique, the heating of application induction furnace, reductive agent adopts price relative to aluminium powder and the lower carbon dust of ferrosilicon, smelting temperature is at 1400 DEG C ~ 1600 DEG C, and auxiliary material does not re-use the nitre and Calcium Fluoride (Fluorspan) that produce pollution gas, has prepared the molybdenum-iron that applicable Iron And Steel Industry uses.
To achieve these goals, the technical solution used in the present invention is:
Low temperature smelting molybdenum-iron reclaims a method for molybdenum, comprises the following steps:
Step one, ammonium soaked slag, ammonium molybdate, molybdenum oxide powder, brown iron oxide, iron powder and reductive agent and add in cylindrical mixer and mix, obtain mixture;
Step 2, to be put into by gained mixture in the furnace lining induction furnace that does by carbonaceous and smelt, starting the heating that heats up, is under the condition of 1400 DEG C ~ 1600 DEG C in temperature, and autoreaction forms smelting slag and molybdenum-iron, then carries out slag sluicing system to product, obtains molybdenum-iron.
Described reductive agent is carbon dust.
In described step one, by massfraction, in mixture, ammonia leaching residue 22.3%, ammonium molybdate 17.2%, molybdenum oxide powder 23.0%, brown iron oxide 20.3%, iron powder 14.2%, reductive agent 3%.
In described step one, by massfraction, in mixture powder, ammonia leaching residue 17.3%, ammonium molybdate 18.5%, molybdenum oxide powder 21.0%, brown iron oxide 19.0%, iron powder 18%, reductive agent 6.2%.
In described step one, in mixture, the weight percent sum of brown iron oxide and iron powder is not less than 27.9%, and the mass content that ammonium soaks molybdenum in slag and ammonium molybdate is 10% ~ 20%.
In described step one, the quality purity of iron powder is not less than 98%, and the quality purity of described brown iron oxide is not less than 98%, and in described step 2, the quality purity of the molybdenum in gained molybdenum-iron is not less than 50%.
In described step one, molybdenum oxide powder is one or both in molybdic oxide powder and titanium dioxide molybdenum powder.
In described step 2, by massfraction, the molybdenum-iron composition of gained is: molybdenum 50.60%, carbon 1.36%, sulphur 0.328%, phosphorus 0.052%, silicon 0.67%, iron 46.99%.
In described step 2, the autoreaction time is no less than 8 minutes.
Compared with prior art, the invention has the beneficial effects as follows:
1, the present invention adopts carbon dust as reductive agent, and after being mixed with reductive agent by mixture powder, roasting is made under not higher than the temperature condition of 1600 DEG C, and in preparation process, the pollutent such as nitrogenfree oxide, fluorochemical produces.
2, composition of raw materials strong adaptability of the present invention, compared with preparing with tradition the thermite process that molybdenum-iron adopts, quality regulate and the amount adjustment of composition of raw materials of the present invention have very good material adaptability, the consumption of molybdenum oxide powder controls in 21.0% ~ 42.9% of mixture powder quality, ratio range is comparatively large, and can select molybdic oxide powder and/or titanium dioxide molybdenum powder.
3, the temperature of reaction of molybdenum-iron preparation method of the present invention is relatively low, and adopt carbon dust relatively low as reductive agent price, adopt ammonium molybdate and industrial residue as fusing assistant, carbon dust and fusing assistant can play to act synergistically and impel the reduction of temperature of reaction, this is mainly because of mixture powder being facilitated to react generation ferro-molybdenum adding of (being less than 1600 DEG C) carbon dust when first showing that temperature is relatively low by analysis molybdenum-iron carbon phase diagram, in addition, the compound containing some low melting points in ammonium molybdate and industrial residue can be used as the generation that initiator causes reduction reaction.
4, do not contain nitre and fluorite in raw material of the present invention, prepare in the reaction process of molybdenum-iron and can not produce oxynitride or fluorochemical, reaction process relative clean compared with traditional method, environmental friendliness.
Embodiment
Embodiments of the present invention are described in detail below in conjunction with embodiment.
Embodiment 1
The molybdenum-iron of the present embodiment is made up of mixture powder and reductive agent, mixture powder is mixed by the raw material of following weight percent: molybdenum oxide powder 21.0%, iron powder 33.2%, ammonia leaching residue 22.3%, ammonium molybdate 23.5%, reductive agent is carbon dust, the consumption of carbon dust is 3% of mixture powder quality, and in ammonia leaching residue, the mass content of molybdenum is 15%; The quality purity of iron powder is not less than 98%, and the quality purity of brown iron oxide is not less than 98%; Molybdenum oxide powder is molybdic oxide powder.
The method that the present embodiment prepares molybdenum-iron is: mixed with reductive agent by mixture powder and be placed in induction furnace, is to obtain product under the condition of 1400 DEG C in temperature, then carries out slag sluicing system to product, obtains molybdenum-iron and slag.
Molybdenum-iron prepared by the present embodiment: molybdenum 50.550%, carbon 1.360%, sulphur 0.319%, phosphorus 0.052%, silicon 0.410%, iron 47.309%.
Embodiment 2
The molybdenum-iron of the present embodiment is made up of mixture powder and reductive agent, and mixture powder is mixed by the raw material of following weight percent: molybdenum oxide powder 42.9%, brown iron oxide 50.3%, ammonium molybdate 3.6%, ammonia leaching residue 3.2%; Reductive agent is carbon dust, and the consumption of carbon dust is 20% of mixture powder quality, and in ammonia leaching residue, the mass content of molybdenum is 15%; The quality purity of iron powder is not less than 98%, and the quality purity of brown iron oxide is not less than 98%; Molybdenum oxide powder is titanium dioxide molybdenum powder.
The method that the present embodiment prepares molybdenum-iron is: mixed with reductive agent by mixture powder and be placed in induction furnace, is to obtain product under the condition of 1600 DEG C in temperature, then carries out slag sluicing system to product, obtains molybdenum-iron and slag.
Molybdenum-iron prepared by the present embodiment: molybdenum 49.590%, carbon 0.430%, sulphur 0.327%, phosphorus 0.048%, silicon 0.415%, iron 49.190%.
Embodiment 3
The molybdenum-iron of the present embodiment is made up of mixture powder and reductive agent, mixture powder is mixed by the raw material of following weight percent: molybdenum oxide powder 29.60%, brown iron oxide 17.7%, iron powder 15.30%, ammonium molybdate 14.80%, ammonia leaching residue 16.60%, carbon dust 6.0%, the method that the present embodiment prepares molybdenum-iron is: mixed with reductive agent by mixture powder and be placed in induction furnace, be under the condition of 1500 DEG C in temperature, obtain product, then slag sluicing system is carried out to product, obtain molybdenum-iron and slag.
Molybdenum-iron prepared by the present embodiment: molybdenum 51.150%, carbon 1.302%, sulphur 0.638%, phosphorus 0.020%, silicon 0.770%, iron 46.120%.
Embodiment 4
The molybdenum-iron of the present embodiment is made up of mixture powder and reductive agent, mixture powder is mixed by the raw material of following weight percent: molybdenum oxide powder 27.13%, brown iron oxide 14.21%, iron powder 22.42%, ammonium molybdate 13.23%, ammonia leaching residue 15.66%, carbon dust 7.35%, in industrial residue, the mass content of molybdenum is 8.0%; The quality purity of iron powder is not less than 98%, and the quality purity of brown iron oxide is not less than 98%; Molybdenum oxide powder is that the molybdic oxide powder of 1:9 and titanium dioxide molybdenum powder mix by mass percent.
The method that the present embodiment prepares molybdenum-iron is: mixed with reductive agent by mixture powder and be placed in induction furnace, the condition being 1500 DEG C in temperature obtains product, then carries out slag sluicing system to product, obtains molybdenum-iron and slag.
Molybdenum-iron prepared by the present embodiment: molybdenum 51.200%, carbon 0.306%, sulphur 0.364%, phosphorus 0.020%, silicon 0.600%, iron 47.510%.
The composition measurement result of molybdenum-iron prepared by the embodiment of the present invention 1 ~ embodiment 4 is as shown in table 1.
Table 1
In the present invention, ammonium molybdate and ammonia leaching residue are the byproducts producing the generation of other product, its composition is as shown in the table, shown composition be to ammonium molybdate and ammonia leaching residue chemical analysis after the content of the element such as molybdenum, and Mu Ye company is all useless for these two kinds of byproducts, in them, the component content of molybdenum is high, the object of the invention is molybdenum wherein to utilize.
Ammonium molybdate, ammonia leaching residue principal element content (mass percent)
Below be only preferred embodiment of the present invention; not the present invention is imposed any restrictions; every above embodiment is done according to the technology of the present invention essence any simple modification, change and equivalent structure change, all still belong in the protection domain of technical solution of the present invention.
Claims (9)
1. low temperature smelting molybdenum-iron reclaims a method for molybdenum, it is characterized in that, comprises the following steps:
Step one, ammonium soaked slag, ammonium molybdate, molybdenum oxide powder, brown iron oxide, iron powder and reductive agent and add in cylindrical mixer and mix, obtain mixture;
Step 2, to be put into by gained mixture in the furnace lining induction furnace that does by carbonaceous and smelt, starting the heating that heats up, is under the condition of 1400 DEG C ~ 1600 DEG C in temperature, and autoreaction forms smelting slag and molybdenum-iron, then carries out slag sluicing system to product, obtains molybdenum-iron.
2. low temperature smelting molybdenum-iron reclaims the method for molybdenum according to claim 1, and it is characterized in that, described reductive agent is carbon dust.
3. according to claim 1 or 2, low temperature smelting molybdenum-iron reclaims the method for molybdenum, it is characterized in that, in described step one, by massfraction, in mixture, ammonia leaching residue 22.3%, ammonium molybdate 17.2%, molybdenum oxide powder 23.0%, brown iron oxide 20.3%, iron powder 14.2%, reductive agent 3%.
4. according to claim 1 or 2, low temperature smelting molybdenum-iron reclaims the method for molybdenum, it is characterized in that, in described step one, by massfraction, in mixture powder, ammonia leaching residue 17.3%, ammonium molybdate 18.5%, molybdenum oxide powder 21.0%, brown iron oxide 19.0%, iron powder 18%, reductive agent 6.2%.
5. according to claim 1 or 2, low temperature smelting molybdenum-iron reclaims the method for molybdenum, it is characterized in that, in described step one, in mixture, the weight percent sum of brown iron oxide and iron powder is not less than 27.9%, and the mass content that ammonium soaks molybdenum in slag and ammonium molybdate is 10% ~ 20%.
6. low temperature smelting molybdenum-iron reclaims the method for molybdenum according to claim 1, it is characterized in that, in described step one, the quality purity of iron powder is not less than 98%, the quality purity of described brown iron oxide is not less than 98%, and in described step 2, the quality purity of the molybdenum in gained molybdenum-iron is not less than 50%.
7. low temperature smelting molybdenum-iron reclaims the method for molybdenum according to claim 1, it is characterized in that, in described step one, molybdenum oxide powder is one or both in molybdic oxide powder and titanium dioxide molybdenum powder.
8. low temperature smelting molybdenum-iron reclaims the method for molybdenum according to claim 1, it is characterized in that, in described step 2, by massfraction, the molybdenum-iron composition of gained is: molybdenum 50.600%, carbon 1.360%, sulphur 0.328%, phosphorus 0.052%, silicon 0.670%, iron 46.990%.
9. low temperature smelting molybdenum-iron reclaims the method for molybdenum according to claim 1, and it is characterized in that, in described step 2, the autoreaction time is no less than 8 minutes.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948123A (en) * | 2016-04-28 | 2016-09-21 | 西安建筑科技大学 | High-efficiency method for preparing low-sulfur molybdenum trioxide from molybdenite by roasting |
| CN110331329A (en) * | 2019-06-26 | 2019-10-15 | 金堆城钼业股份有限公司 | A kind of preparation method of Smelting High Speed Steel ferro-molybdenum |
| CN111763835A (en) * | 2020-09-03 | 2020-10-13 | 北京利尔高温材料股份有限公司 | Fluorine-free low-nitrogen-sulfur ferromolybdenum smelting raw material, ferromolybdenum green smelting system and ferromolybdenum green smelting method |
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| CN104152707A (en) * | 2014-08-28 | 2014-11-19 | 金堆城钼业股份有限公司 | Method for smelting ferro-molybdenum from ammonia leaching residue to recover molybdenum |
| CN104762544A (en) * | 2015-04-24 | 2015-07-08 | 金堆城钼业股份有限公司 | Ferro-molybdenum and preparation method thereof |
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- 2015-07-20 CN CN201510427240.4A patent/CN104946891A/en active Pending
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| CN104152707A (en) * | 2014-08-28 | 2014-11-19 | 金堆城钼业股份有限公司 | Method for smelting ferro-molybdenum from ammonia leaching residue to recover molybdenum |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105948123A (en) * | 2016-04-28 | 2016-09-21 | 西安建筑科技大学 | High-efficiency method for preparing low-sulfur molybdenum trioxide from molybdenite by roasting |
| CN105948123B (en) * | 2016-04-28 | 2017-08-01 | 西安建筑科技大学 | A kind of method that high-efficient roasting molybdenite prepares low-sulfur molybdenum trioxide |
| CN110331329A (en) * | 2019-06-26 | 2019-10-15 | 金堆城钼业股份有限公司 | A kind of preparation method of Smelting High Speed Steel ferro-molybdenum |
| CN111763835A (en) * | 2020-09-03 | 2020-10-13 | 北京利尔高温材料股份有限公司 | Fluorine-free low-nitrogen-sulfur ferromolybdenum smelting raw material, ferromolybdenum green smelting system and ferromolybdenum green smelting method |
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