CN105779795A - Rare earth alloy refined through waste catalysts reclaimed by high-frequency furnace or medium-frequency furnace and preparation method of rare earth alloy - Google Patents
Rare earth alloy refined through waste catalysts reclaimed by high-frequency furnace or medium-frequency furnace and preparation method of rare earth alloy Download PDFInfo
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- C22C1/00—Making non-ferrous alloys
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Abstract
The invention belongs to the technical field of reclaiming of catalysts, and relates to a rare earth alloy refined through waste catalysts reclaimed by a high-frequency furnace or a medium-frequency furnace and a preparation method of the rare earth alloy. The preparation method comprises the following steps of A, performing crushing: crushing waste catalysts containing TiO2 into small granules so as to obtain powder; B, performing impurity elimination: putting the powder into a sodium hydroxide solution, performing sufficient stirring, filtering filtrate so as to obtain filter residues, rinsing the filter residue with technology water until the pH is neutral, and performing drying; C, performing compounding: adding ferrosilicon powder, iron ore powder, aluminum granules and lime powder to the powder, and performing uniform stirring so as to obtain materials to be refined; and D, performing melting: putting the materials to be refined into the high-frequency furnace or the medium-frequency furnace, performing high-temperature melting, shifting out a melting solution, and performing cooling so as to obtain the rare earth alloy. According to the rare earth alloy and the preparation method thereof disclosed by the invention, the ferrotitanium rare earth alloy is smelted through aluminum and silicon in a hot manner, the preparation method is feasible in economic, physical and chemical principles, and secondary pollution is not generated.
Description
Technical field
The invention belongs to catalyst recovery technology field, relate to a kind of coreless induction furnace or the intermediate frequency furnace rare earth alloy reclaiming dead catalyst refining and preparation method thereof.
Background technology
Coal-burning power plant, steel plant the nitrogen oxides (NOx) of the discharged from coal-fired boiler such as sintering circuit and coking process, glass kiln, chemical plant and cement furnace be one of Air Pollutants.
In numerous denitration technologies, selective catalytic reduction (SCR) is that denitration efficiency is the highest, denitration technology the most ripe.The demonstration project establishing first SCR system in Shimoneski power plant of Japan in 1975, SCR technology is widely applied in Japan thereafter.The successful Application experience of existing 120 multiple stage large-scale plants in Europe, the removal efficiency of its NOx can reach 80～90%.Up to now, nearly 170 covering devices of Japan, close to this equipment of Installation in Plant of 100GW capacity, SCR technology is also controlled the major technique of NOx by U.S. government as main power plant.Relevant report is pointed out, SCR method has become the mainstream technology of current home and abroad power plant denitration comparative maturity.After entering 21 century, face the negative effect that environment is caused by the industrial revolution, through industrial practice for many years and checking, now widely used is for carrier loaded barium oxide as active substance (be aided with tungsten oxide or molybdenum oxide is the metal oxide catalyst of promoter) using anatase titanium dioxide, become the ripe out of stock technology of coal-burning boiler, be widely used among the environment-friendly engineering in each field of China.
But after going into effect " fossil-fuel power plant atmospheric pollutant emission standard " (GB13223 2011) on January 1st, 2012, the each SCR system in the whole nation all reflects because of catalyst inevitably that because various physics chemical action (poisoning, abrasion, thermal sintering, blocking/contamination etc.) lost efficacy, cause that its service life shortens, the serious problems that the replacement cycle of catalyst shortens；This not only denitration effect and Financial cost to SCR system cause tremendous influence；And ecological environment is also resulted in great negative effect.
According to relevant report it can be seen that for coal-burning boiler, the deactivation rate of SCR catalyst is about every 1000h, denitration efficiency reduces by 0.7%, the catalyst change cycle be 3-5/time.For station boiler and the incinerator of burning inferior coal or co-firing of biomass and coal, the speed of catalysqt deactivation is faster；One, the U.S. uses culled wood and the fuel combination power station of PRB (PowderRiverBasin) coal, the deactivation rate of catalyst reduces by 18% up to every 1000h, denitration efficiency, be coal fired power plant application 25.7 times, namely this power station catalyst change cycle less than March/time.
The deactivation cause of catalyst can be summarized as contamination and (4) catalyst poisoning etc. of (1) sintering deactivation, the hole plug of (2) catalyst, (3) catalyst.The inactivation behavior that wherein (2) and (3) reason causes can pass through washing, method of reproduction re-applies in the denitration process of coal-burning boiler after processing.(1) reason causes inactivation behavior, it is impossible to make its activity recovery by washing the mode of regeneration；(4) reason causes inactivation behavior to be not only difficult to make its activity recovery by washing the mode of regeneration, and in denitrification process because of SCR catalyst adsorb alkali metal, alkaline-earth metal, arsenic, hydrogen chloride, the phosphorus in flue gas, lead and other elements occupies active site makes wide variety of vanadium system SCR catalyst lose activity (strong chemisorbed or chemical reaction occur poisoning reactant, product or the impurity of including on catalyst activity position)；Add V on TiO2 carrier, elements such as w content overproof again.Thereby it is assumed that, the TiO2 carrier used in coal-burning boiler SCR denitration technique, it has also become high-risk solid waste (it is reported, inefficacy TiO2 carrier generating capacity in Inner Mongolia Autonomous Region is 1.5 ten thousand t/)！
SCR denitration and TiO2 carrier thereof are generally adopted chemical synthesis to be prepared with raw materials such as sulfide and halogen (chlorine) compounds；High-risk solid waste TiO2 carrier, if recycling by the method, not only process route is difficult to arrange again, and the intractability of secondary pollution bigger (cost, environment and products thereof quality).If being treated as mine, city, by the method for pyrometallurgy using resources such as Ti as valuable metal recovery, microelement fixations such as alkali metal, alkaline-earth metal, arsenic, hydrogen chloride, phosphorus, lead in slag, and it is applied to other field, both do not result in secondary environmental pollution, and can reach effectively to utilize the purpose of (efficiency, Social benefit and economic benefit also open up NPD projects) yet.SCR denitration technique, industrial undertaking will be contributed to friendly environment society etc. and produce long-range, positive positive effect by it.
Summary of the invention
It is an object of the invention to for the problems referred to above, it is provided that the preparation method that a kind of coreless induction furnace or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy.
It is a further object of the present invention to provide rare earth alloy prepared by a kind of dead catalyst.
For reaching above-mentioned purpose, present invention employs following technical proposal: the preparation method that a kind of coreless induction furnace or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, comprise the following steps:
A, pulverizing, will containing TiO2Dead catalyst be ground into little granule, form powder；
B, remove impurity, put into powder in sodium hydroxide solution, be sufficiently stirred for, and obtains filtering residue after filter liquor, rinses filtering residue to pH in neutrality with fresh water (FW), dry；
C, dispensing, add ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone in powder, stir, and is formed and treats refining material；
D, melting, will treat that refining material is put in coreless induction furnace or intermediate frequency furnace, and high temperature melting removes liquation, is rare earth alloy after cooling.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step, described powder particle size is 100-200 order, and described dead catalyst is the SCR catalyst of inactivation；In stepb, the pH of described sodium hydroxide solution is 14.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step C, the weight ratio of described powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone is 100:3.8-6.7:20.7-77:55-67.6:12.2-13.2.
Reclaim in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step, TiO in described powder2Content be not less than 95%, in step C, described treats that refining material is divided into major ingredient and refinery, wherein in major ingredient, the weight ratio of powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone is 100:3.8:20.7:55:12.2, refinery is that the ferrosilicon powder of 2.9:56.3:12.6:1, Iron Ore Powder, aluminum shot and pulverized limestone form by weight ratio, and the weight ratio of major ingredient and refinery is 191.7:72.8.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step D, high temperature melting in coreless induction furnace or intermediate frequency furnace first put into by major ingredient, then puts into refinery high temperature melting in liquation, removes liquation afterwards and cools down.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step C, major ingredient is first put in pretreatment stove, and between 750-850 DEG C roasting preheating, afterwards major ingredient hot charging is entered in coreless induction furnace or the intermediate frequency furnace of step D.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, described major ingredient hot charging between 200-400 DEG C enters in coreless induction furnace or the intermediate frequency furnace of step D.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step D, the temperature of coreless induction furnace or intermediate frequency furnace controls between 1900-2000 DEG C.
Reclaiming in the preparation method of dead catalyst refining rare earth alloy at above-mentioned coreless induction furnace or intermediate frequency furnace, in step C, described ferrosilicon powder is pulverized by 75 ferrosilicon and is made, and the total iron-holder in described Iron Ore Powder is more than 64%.
A kind of rare earth alloy prepared according to above-mentioned preparation method.
Compared with prior art, it is an advantage of the current invention that: adopt aluminum silicon heat to smelt ferrotianium rare earth alloy, not only economically, physical and chemical principle is all feasible, and do not produce secondary pollution, provide process technique practical, eco-friendly for processing high-risk garbage (SCR catalyst).
Detailed description of the invention
Embodiment 1
The preparation method that a kind of coreless induction furnace or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, comprises the following steps:
A, pulverizing, will containing TiO2Dead catalyst be ground into little granule, form powder；Described powder particle size is 100-200 order, and described dead catalyst is the SCR catalyst of inactivation, TiO in powder2Content be not less than 95%；
B, remove impurity, powder is put in sodium hydroxide solution, it is sufficiently stirred for 1-3hr, sodium hydroxide solution can be placed in the reactor with stirring paddle, filter liquor obtains filtering residue after removing sodium hydroxide solution, filtering residue is the powder after remove impurity, and filtering residue fresh water (FW) rinses to pH in neutrality, with dehydrator powder after dry remove impurity at 105-120 DEG C；In the present embodiment, the pH of described sodium hydroxide solution is 14, it is clear that it will be appreciated by those skilled in the art that sodium hydroxide solution described herein also replaceable one-tenth potassium hydroxide solution or other strong base solutions, is used for removing greasy dirt, silicon dioxide etc..
C, dispensing, add ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone in powder, stir with blender, is formed and treats refining material；Wherein, the weight of powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone respectively 100kg, 3.8kg, 20.7kg, 55kg and 12.2kg.Ferrosilicon powder is pulverized by 75 ferrosilicon and is made, and the total iron-holder in Iron Ore Powder is more than 64%.
D, melting, will treat that refining material is put in coreless induction furnace or intermediate frequency furnace, and high temperature melting removes liquation, is rare earth alloy after cooling.The temperature of coreless induction furnace or intermediate frequency furnace controls between 1900-2000 DEG C, and smelting time is 60-90 minute.
After above-mentioned step, obtain a kind of in block rare earth alloy, can be directly deposited on place, environment will not be caused heavy metal pollution, the poisonous and hazardous useless SCR catalyst being put into hazardous chemical is transformed into the rare earth alloy with industrial value, and can be directly deposited on place and can be used for further Extraction of rare earth metal, whole preparation process is simple and reliable, environmental friendliness.
Embodiment 2
The present embodiment is essentially identical with the process of embodiment 1, is different in that, in step C, and the weight of powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone respectively 100kg, 6.7kg, 77kg, 67.6kg and 13.2kg.Thus it is high to prepare a kind of iron-holder, the better rare earth alloy of mobility.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, it is different in that, in step C, it is respectively configured major ingredient and refinery, wherein major ingredient includes 100kg, 3.8kg, 20.7kg, the powder of 55kg and 12.2kg, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone, and refinery is made up of 2.9kg, 56.3kg, the ferrosilicon powder of 12.6kg and 1kg, Iron Ore Powder, aluminum shot and pulverized limestone.
In step D, high temperature melting in coreless induction furnace or intermediate frequency furnace first put into by major ingredient, then puts into refinery high temperature melting in liquation, removes liquation afterwards and cools down, obtaining rare earth alloy.In the present embodiment, the method using fed batch, accelerate fusing speed, improve heat effect.
Embodiment 4
The present embodiment is substantially the same manner as Example 3, it is different in that, in step C, major ingredient is first put in pretreatment stove, and between 750-850 DEG C roasting preheating, afterwards major ingredient hot charging between 200-400 DEG C is entered in coreless induction furnace or intermediate frequency furnace, high temperature melting, add refinery, high temperature melting, after cooling, obtain rare earth alloy.
Embodiment 5
The present embodiment is substantially the same manner as Example 3, is different in that, in step C, major ingredient is first put in pretreatment stove, and between 750-850 DEG C roasting preheating, pretreatment stove is rotary kiln or mineral hot furnace, roasting preheating in rotary kiln or mineral hot furnace, ore particle structure is made to change, it is beneficial to reduction, afterwards major ingredient hot charging between 200-400 DEG C is entered in coreless induction furnace or intermediate frequency furnace, add refinery, high temperature melting together, obtains rare earth alloy.
After testing, in embodiment 5, in raw material, the percent reduction of each oxide is: TiO2→ Ti77%；TiO2→ TiO23%；Fe2O3→ Fe99%；Fe2O3→ FeO10%；FeO → Fe99%；SiO2→ Si90%.The content of the rare earth alloy in embodiment 5 is as follows: Ti31%, Al7.0%, Si4.3%.
Table 1 is the material composition table in embodiment 1-5.
Table 1 material chemical component (%)
Specific embodiment described herein is only to present invention spirit explanation for example.Described specific embodiment can be made various amendment or supplements or adopt similar mode to substitute by those skilled in the art, but without departing from the spirit of the present invention or surmount the scope that appended claims is defined.
Claims (10)
1. the preparation method that a coreless induction furnace or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that comprise the following steps:
A, pulverizing, will containing TiO2Dead catalyst be ground into little granule, form powder；
B, remove impurity, put into powder in sodium hydroxide solution, be sufficiently stirred for, and obtains filtering residue after filter liquor, rinses filtering residue to pH in neutrality with fresh water (FW), dry；
C, dispensing, add ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone in powder, stir, and is formed and treats refining material；
D, melting, will treat that refining material is put in coreless induction furnace or intermediate frequency furnace, and high temperature melting removes liquation, is rare earth alloy after cooling.
2. the preparation method that coreless induction furnace according to claim 1 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that in step, described powder particle size is 100-200 order, described dead catalyst is the SCR catalyst of inactivation；In stepb, the pH of described sodium hydroxide solution is 14.
3. the preparation method that coreless induction furnace according to claim 1 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterized in that, in step C, the weight ratio of described powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone is 100:3.8-6.7:20.7-77:55-67.6:12.2-13.2.
4. the preparation method that coreless induction furnace according to claim 3 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that in step, TiO in described powder2Content be not less than 95%, in step C, described treats that refining material is divided into major ingredient and refinery, wherein in major ingredient, the weight ratio of powder, ferrosilicon powder, Iron Ore Powder, aluminum shot and pulverized limestone is 100:3.8:20.7:55:12.2, refinery is that the ferrosilicon powder of 2.9:56.3:12.6:1, Iron Ore Powder, aluminum shot and pulverized limestone form by weight ratio, and the weight ratio of major ingredient and refinery is 191.7:72.8.
5. the preparation method that coreless induction furnace according to claim 4 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterized in that, in step D, high temperature melting in coreless induction furnace or intermediate frequency furnace first put into by major ingredient, in liquation, put into refinery high temperature melting again, remove liquation afterwards and cool down.
6. the preparation method that coreless induction furnace according to claim 4 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterized in that, in step C, major ingredient is first put in pretreatment stove, and between 750-850 DEG C roasting preheating, afterwards major ingredient hot charging is entered in coreless induction furnace or the intermediate frequency furnace of step D.
7. the preparation method that coreless induction furnace according to claim 6 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that described major ingredient hot charging between 200-400 DEG C enters in coreless induction furnace or the intermediate frequency furnace of step D.
8. the preparation method that coreless induction furnace according to claim 1 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that in step D, the temperature of coreless induction furnace or intermediate frequency furnace controls between 1900-2000 DEG C.
9. the preparation method that coreless induction furnace according to claim 1 or intermediate frequency furnace reclaim dead catalyst refining rare earth alloy, it is characterised in that in step C, described ferrosilicon powder is pulverized by 75 ferrosilicon and is made, and the total iron-holder in described Iron Ore Powder is more than 64%.
10. the rare earth alloy that the preparation method according to claim 1-9 any one prepares.
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