CN104120288A - Method for continuously preparing metal samarium through direct thermal reduction - Google Patents

Method for continuously preparing metal samarium through direct thermal reduction Download PDF

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CN104120288A
CN104120288A CN201410345625.1A CN201410345625A CN104120288A CN 104120288 A CN104120288 A CN 104120288A CN 201410345625 A CN201410345625 A CN 201410345625A CN 104120288 A CN104120288 A CN 104120288A
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samarium
pelletizing
high temperature
batching
metal
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CN104120288B (en
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张廷安
豆志河
张子木
刘燕
吕国志
赵秋月
牛丽萍
傅大学
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Northeastern University China
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Northeastern University China
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Abstract

The invention discloses a method for continuously preparing metal samarium through direct thermal reduction, and belongs to the technical field of nonferrous metallurgy. The preparation method comprises the following steps: Sm2O3, Al, CaO or MgO are mixed, wherein a reducing agent is Al, and can be replaced by an Si-Fe alloy with 75 mass% of Ca or Si; the batching and the pelletizing are performed; and then, the high-temperature reduction reaction is performed for pellets in flowing inert gas or nitrogen atmosphere; and finally, high-temperature samarium steam carried out by flowing inert carrier gases or nitrogen in a high-temperature reduction furnace is condensed to obtain the metal samarium. The method adopts the relative-vacuum manner, cancels a vacuum system and a vacuum reduction tank, realizes the continuous preparation of the metal samarium, shortens the reduction period, and improves the preparation efficiency; the recovery rate of the metal samarium can reach above 97%; as the energy consumption is obviously reduced, the method is a novel energy-saving green process for preparing the metal samarium with low cost; and the method is simple in operation, is simpler in equipment, is low in requirement, and reduces the equipment investment and the operation cost.

Description

A kind of method of direct heat reduction continuous production samarium metal
Technical field
The invention belongs to non-ferrous metallurgy technology field, particularly a kind of method of direct heat reduction continuous production samarium metal.
Background technology
Samarium metal (Sm) is one of staple product of light rare earth metal, has special physico-chemical property.Its 1074 DEG C of fusing points, 1794 DEG C of boiling points, hardness 45～65HB, density 7.536g/ml, ductility good and be easy to processing become a useful person.Samarium has very strong metallochemistry, under certain ambient conditions effect, easily and the interaction such as oxygen, hydrogen, nitrogen, sulphur, carbon and generate corresponding compound (Sm 2o 3, SmH 3, SmN etc.), can generate alloy (as SmCo etc.) with some metal, can generate different metal salt (SmCl with acid-base function 3, Sm 2(SO 4) 3, SmNO 3deng).As above samarium metal compound, alloy and salt etc. all have good practical technique and economic worth.
In recent years, samarium metal obtains applying more and more widely in the field such as scavenging agent and nuclear power of the alterant of rare earth permanent-magnetic material, alloy, iron and steel.For example, because the orbital moment in samarium atom and spin moment all have desirable influence to magnetic moment, can be made into SmCo 5, Sm 2co 17and Sm 2fe 17n xdeng rare earth samarium permanent magnet material, industrial and commercial bank of the army of being widely used in ripple device and circulator.Because SmCo type energy density is large, can be made into the sealed valve of magnet valve for Nuclear power plants, reduce and reveal.Samarium permanent magnet material is also widely used in the biologic medical fields such as channels magnetotherpay device, instruments and medical magnetic sheet.Also have containing the sparking alloy of samarium and be used for industrial gas lamp, welding gun lighter for ignition and torch portfire etc.; Samarium can deoxidation sulphur removal in steel-making and iron manufacturing process, thus raising steel and ferrum property; Samarium also can be made into the excellent material that heats neutron amount for reactor internal control, absorbs the split speed of thermal neutron with regard to adjustable atom; Sm 2o 3also can be used for the component of the ceramic protective layer on nucleon reaction heap, or for controlling the nuclear reaction of atomic boiler, effect is fine.From the 80-90 age in last century, China produces Sm, and oneself reaches industrialized level, and oneself forms large-scale production, can meet the demand of domestic and international market.Since 2000, the production technology and equipments of China Sm is more perfect, and oneself becomes the big producing country of Sm, and output occupies first of the world.
At present, China's samarium metal main preparation methods is rare earth metal reduction distillation method, taking Rare Earth Lanthanum (or cerium, praseodymium, neodymium) or lanthanum cerium alloy as reductive agent, and Sm 2o 3for raw material 1200～1250 DEG C of high temperature reduction 90min under the vacuum condition lower than 1Pa, then condensation, fractionation by distillation obtain samarium metal.The Processes and apparatus of the method is more ripe, own industrial applications.But the method exists production capacity is little, samarium product unit output is low, while causing demand to increase soon, must use a lot of platform reduction furnace equipment just can satisfy the demands, cause that facility investment is large, operation is numerous and diverse, productive expense is high and the problem such as management inconvenience.The method, taking rare earth metal as reductive agent, exists the shortcomings such as production cost height simultaneously.For above problem, for improving samarium metal output, reduce its production cost, must fast Development samarium metal novel preparation method.Develop in recent years Sm 2o 3high temperature fused salt electrolysis method, calciothermy are prepared samarium metal or samarium alloy, but above method all exists the problems such as quality product is low, production efficiency is low, production cost is high, and cannot industrial applications.
Summary of the invention
Prepare samarium metal for existing rare earth vacuum reduction-distillation method and produce and study existing shortcoming and defect, the present invention proposes a kind of method of direct heat reduction continuous production samarium metal, in dynamic rare gas element or nitrogen, carry out high temperature reduction, rare gas element or nitrogen that the high temperature samarium steam generating is flowed carry away, and condensation obtains samarium metal.The invention provides a kind of under " relative vacuum " condition, the method that adopts metallothermics to refine continuously samarium, realize the low cost of samarium and produced continuously, solved traditional rare earth vacuum reduction-distillation method and prepare the problems such as the existing energy consumption of samarium metal is high, reduction short and production cost of tank life-span is high; The inventive method speed of response is fast, and reduction efficiency is high, has realized the continuous production of samarium simultaneously.
A kind of method of direct heat reduction continuous production samarium metal comprises in pelletizing group, relative vacuum atmosphere the steps such as pelletizing reduces continuously, the condensation of high temperature samarium steam.Wherein, pelletizing group refers to Sm 2o 3, reductive agent, interpolation reaction promoter CaO or MgO be mixed in proportion, wherein reductive agent is that Al can replace with Ca or 75Si-Fe alloy, adopts roller machine to be pressed into block or spherical pelletizing; Pelletizing continuous reduction in " relative vacuum " atmosphere refers to carries out pelletizing high temperature reduction reaction in mobile inert atmosphere or nitrogen atmosphere, and inert carrier gas or nitrogen that the high temperature samarium steam that reaction generates is flowed immediately carry away.For each reaction interface, because the high temperature samarium steam generating is carried and left reaction interface by inert carrier gas or nitrogen immediately, so for the high temperature samarium steam in reaction interface, its dividing potential drop is always in the negative pressure state lower than 1atm, i.e. so-called " relative vacuum " state.Therefore, for the atmosphere generating on the reduction reaction interface of samarium steam, just look like that an airtight container has been taken out vacuum the same, be referred to as " relative vacuum " or " negative pressure relatively ", this is the thermodynamic and kinetic conditions more fully that provides of reaction; The condensation of samarium steam refers to the high temperature samarium steam cooling process that obtains samarium metal ingot fast of coming being carried by rare gas element in high temperature reduction furnace or nitrogen.
The method of direct heat reduction continuous production samarium metal of the present invention, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: adopt the one in following batching mode (1)～(4):
(1) by Sm 2o 3: Al: CaO in molar ratio 1: (2～2.4): (0～3) batching;
(2) by Sm 2o 3: Al: MgO in molar ratio 1: (2～2.4): 1 batching;
(3) by Al and MgO in the Al in (1) and CaO or (2), with Ca replacement, wherein, the consumption of Ca is definite with Al, and the Al of 1 mass unit can replace with the calcium of 2.2 times of mass units;
(4), by the Al in (1) or (2), with the replacement of 75Si-Fe alloy, wherein, the Si-Fe alloy that the Al of 1 mass unit is 75% with the Si content of 1 mass unit replaces;
Pelletizing: the batch mixing of preparing burden is even, at 100～250kg/cm 2under pressure, be pressed into pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile rare gas element or nitrogen atmosphere, gas flow is 3.0～6.0m 3/ h, adds high temperature reduction furnace continuously by pelletizing, and reduction temperature is 900～1600 DEG C, recovery time is 20～60min, obtains high temperature samarium steam, and mixes with rare gas element or nitrogen, form high-temperature gas mixture, reducing slag is discharged to high temperature reduction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to high temperature reduction furnace by mobile rare gas element or nitrogen, be transported to condenser system by sealing pipeline and carry out condensation, obtain solid metal samarium.
Wherein, in step 1, with roll squeezer, batching is pressed into block or spherical pelletizing when pelletizing; Rare gas element in step 2 is that purity is more than or equal to 99.95% high-purity argon gas; Condensation method in step 3 is direct condensation or atomization condensation, and wherein directly condensation method adopts recirculated water cooling condensation; High temperature reduction furnace in step 2 or step 3 is medium-frequency induction furnace or high temperature resistance furnace.
Described 75Si-Fe alloy is the Si-Fe alloy of Si mass content 75%.
In above-mentioned step, work as Sm 2o 3: Al: CaO prepares burden 1: 2 in molar ratio: when (0～3) batching pelletizing, according to reaction formula (1) reaction, stoichiometric ratio is mol ratio;
Sm 2O 3(s)+2Al(l)+xCaO＝2Sm(g)+Al 2O 3·xCaO(s) (1)
Reaction formula (1) can exist the one in following several reaction formation to react:
Sm 2O 3(s)+2Al(l)＝2Sm(g)+Al 2O 3(s) (1-1)
Sm 2 O 3 ( s ) + 2 Al ( l ) + 1 2 CaO ( s ) = 2 Sm ( g ) + 1 2 2 A l 2 O 3 · CaO ( s ) - - - ( 1 - 2 )
Sm 2O 3(s)+2Al(l)+CaO(s)＝2Sm(g)+Al 2O 3·CaO(s) (1-3)
Sm 2 O 3 ( s ) + 2 Al ( l ) + 12 7 CaO ( s ) = 2 Sm ( g ) + 1 7 7 A l 2 O 3 · 12 CaO ( s ) - - - ( 1 - 4 )
Sm 2O 3(s)+2Al(l)+3CaO(s)＝2Sm(g)+Al 2O 3·3CaO(s) (1-5)
Work as Sm 2o 3: when Al: MgO prepares burden 1: 2: 1 batching in molar ratio, according to reaction formula (2) reaction, stoichiometric ratio is mol ratio;
Sm 2O 3(s)+2Al(l)+MgO(s)＝2Sm(g)+MgO·Al 2O 3(s) (2)
In order to ensure Sm 2o 3reduction effect, in batching, the actual dosage of reductive agent Al is than theoretical amount excessive 10%～20%.
Because high temperature reduction reaction is to carry out in mobile inert atmosphere or in nitrogen atmosphere, therefore rare gas element or nitrogen that the high temperature samarium steam generating in pelletizing reaction interface is flowed immediately carry away, therefore in reaction interface to high temperature samarium steam, all the time the negative pressure state far below 1atm in a dividing potential drop, i.e. so-called " relative vacuum " or " negative pressure relatively ".Because the high temperature samarium steam generating is carried by inert carrier gas or nitrogen at any time, the reaction formula (1) or the reaction formula (2) that greatly promote high temperature reduction to generate samarium steam are carried out to the right, greatly improve Sm 2o 3reducing degree and reduction rate.The rate of recovery of samarium metal is greater than 97%.Reducing slag is directly discharged, and has realized the continuous production of samarium metal.
The method tool of direct heat reduction continuous production samarium metal of the present invention has the following advantages:
(1) compared with refining samarium technology with traditional rare earth thermal reduction-distillation method, the inventive method has adopted " relative vacuum " (also can be " negative pressure relatively ") means, cancel vacuum system and vacuum reducing tank, realized the continuous production of samarium metal;
(2) because restoring operation is to carry out under " relative vacuum " condition, the energy consumption of technical solution of the present invention significantly reduces, the inert carrier gas or the nitrogen that are flowed immediately due to the hot metal samarium steam generating carry away, will greatly promote reaction (1) and move to positive dirction, significantly having strengthened Sm 2o 3reduction generates the dynamic conditions of samarium metal, has realized continuous production, has shortened reduction cycle; speed of response is fast, and the reduction reaction time, lower than 1h, has been improved production efficiency; the rate of recovery of samarium metal can reach more than 97%, inertia protection carrier gas simultaneously or nitrogen reusable edible.Therefore, the technology of the present invention is the energy-saving novel environment-friendly process that a kind of low cost is prepared samarium metal.
(3) the technology of the present invention is compared with traditional vacuum reduction-distillation method, and the present invention adopts and uses Al, Ca or Si-Fe alloy as reductive agent simultaneously, and selectivity is added CaO and regulated Sm 2o 3the thermodynamic and kinetic conditions of reduction, then pelletizing, has greatly improved the controllability that samarium metal generates.Use Al, Ca or Si-Fe alloy as reductive agent simultaneously, replace rare earth reductive agent, greatly reduced the raw materials cost of the production of samarium metal.
(4) simple to operate, equipment more simply requires low, has reduced facility investment and running cost.
Embodiment
The Sm that following examples adopt 2o 3purity (massfraction) is greater than 99.0%, CaO and MgO purity (massfraction) is greater than 99.0%, and reductive agent Al and Ca purity are greater than 99.0%, the high-purity argon gas that argon gas is 99.95%.Medium-frequency induction furnace ruhmkorff coil diameter used is 220mm.
Embodiment 1
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al is 1: 2.2 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 100kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas atmosphere, argon flow amount is 6.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1400 DEG C, and the recovery time is 60mins, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 97% of samarium metal.
Embodiment 2
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al is 1: 2.0 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1500 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 97.2% of samarium metal.
Embodiment 3
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al is 1: 2.2 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 30min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal ingot casting, the rate of recovery 97.3% of samarium metal.
Embodiment 4
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.2: 0.5 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile high pure nitrogen gas stream atmosphere, high pure nitrogen flow is 6.0m 3/ h, adds vertical medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 900 DEG C, and the recovery time is 60min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to vertical medium-frequency induction furnace by the High Purity Nitrogen air-flow that flows, be delivered directly to jet atomization device by sealed can road, carry out atomization condensation and obtain samarium metal, the rate of recovery 97.1% of samarium metal.
Embodiment 5
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.2: 0.5 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 100kg/cm 2pressure under be pressed into block pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1400 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 98.5% of samarium metal.
Embodiment 6
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 0.5 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 30min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.2% of samarium metal.
Embodiment 7
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 6.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 900 DEG C, and the recovery time is 60min, obtains high temperature samarium steam;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.0% of samarium metal.
Embodiment 8
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1200 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.1% of samarium metal.
Embodiment 9
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 20min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.3% of samarium metal.
Embodiment 10
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 12/7 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 6.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 900 DEG C, and the recovery time is 60min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 98.9% of samarium metal.
Embodiment 11
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 12/7 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into block pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas atmosphere, argon flow amount is 4.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1200 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.3% of samarium metal.
Embodiment 12
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 12/7 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas atmosphere, argon flow amount is 3.5m 3/ h, adds high temperature resistance furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 30min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to high temperature resistance furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to high temperature resistance furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.0% of samarium metal.
Embodiment 13
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 3 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 950 DEG C, and the recovery time is 60min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to jet atomization device by sealed can road, carry out atomization condensation and obtain samarium metal, the rate of recovery 99.3% of samarium metal.
Embodiment 14
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 3 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1250 DEG C, and the recovery time is 30min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.5% of samarium metal.
Embodiment 15
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: CaO is 1: 2.4: 3 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 25min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.6% of samarium metal.
Embodiment 16
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: MgO is 1: 2.2: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 6.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1000 DEG C, and the recovery time is 50min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.2% of samarium metal.
Embodiment 17
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: MgO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1400 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the rate of recovery 99.5% of samarium metal.
Embodiment 18
The method of direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Al: MgO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 20min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal ingot casting, the rate of recovery 99.5% of samarium metal.
Embodiment 19
The method that adopts direct heat reduction continuous production samarium metal, specifically comprises the following steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Ca is 1: 3.3 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 250kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 5.0m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1450 DEG C, and the recovery time is 40min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the samarium metal rate of recovery 99.7%.
Embodiment 20
The method that adopts direct heat reduction continuous production samarium metal, specifically comprises the following steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: Ca is 1: 3.6 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 200kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 2.5m 3/ h, adds medium-frequency induction furnace continuously by pelletizing, and reduction temperature is 1600 DEG C, and the recovery time is 35min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to medium-frequency induction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to medium-frequency induction furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the samarium metal rate of recovery 99.8%.
Embodiment 21
The method that adopts direct heat reduction continuous production samarium metal, specifically comprises the following steps:
Step 1, batching pelletizing:
Batching: by Sm 2o 3: 75Si-Fe alloy: CaO is 1: 2.4: 1 batching according to mol ratio;
Pelletizing: the batch mixing of preparing burden is even, adopts roll squeezer at 150kg/cm 2pressure under be pressed into spherical pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile argon gas gas atmosphere, argon flow amount is 4.5m 3/ h, adds high temperature resistance furnace continuously by pelletizing, and reduction temperature is 1550 DEG C, and the recovery time is 50min, obtains high temperature samarium steam, and mixes with argon gas, forms high-temperature gas mixture, reducing slag is discharged to high temperature resistance furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to high temperature resistance furnace by the argon gas that flows, be delivered directly to samarium drainer by sealed can road, carry out recirculated water cooling condensation and obtain samarium metal, the samarium metal rate of recovery 99.2%.

Claims (6)

1. a method for direct heat reduction continuous production samarium metal, specifically comprises the steps:
Step 1, batching pelletizing:
Batching: adopt the one in following batching mode (1)～(4):
(1) by Sm 2o 3: Al: CaO in molar ratio 1: (2～2.4): (0～3) batching;
(2) by Sm 2o 3: Al: MgO in molar ratio 1: (2～2.4): 1 batching;
(3) by Al and MgO in the Al in (1) and CaO or (2), with Ca replacement, wherein, the consumption of Ca is definite with Al, and the Al of 1 mass unit can replace with the calcium of 2.2 times of mass units;
(4), by the Al in (1) or (2), with the replacement of 75Si-Fe alloy, wherein, the Si-Fe alloy that the Al of 1 mass unit is 75% with the Si content of 1 mass unit replaces;
Pelletizing: the batch mixing of preparing burden is even, at 100～250kg/cm 2under pressure, be pressed into pelletizing;
Step 2, pelletizing high temperature reduces continuously:
In mobile rare gas element or nitrogen atmosphere, gas flow is 3.0～6.0m 3/ h, adds high temperature reduction furnace continuously by pelletizing, and reduction temperature is 900～1600 DEG C, recovery time is 20～60min, obtains high temperature samarium steam, and mixes with rare gas element or nitrogen, form high-temperature gas mixture, reducing slag is discharged to high temperature reduction furnace continuously simultaneously;
Step 3, the condensation of high temperature samarium steam:
High temperature samarium steam is carried out to high temperature reduction furnace by mobile rare gas element or nitrogen, be transported to condenser system by sealing pipeline and carry out condensation, obtain solid metal samarium.
2. the method for direct heat as claimed in claim 1 reduction continuous production samarium metal, is characterized in that, in described step 1, with roll squeezer, batching is pressed into block or spherical pelletizing when pelletizing.
3. the method for direct heat reduction continuous production samarium metal as claimed in claim 1, is characterized in that, the rare gas element in described step 2 is that purity is more than or equal to 99.95% high-purity argon gas.
4. the method for direct heat reduction continuous production samarium metal as claimed in claim 1, is characterized in that, the high temperature reduction furnace in described step 2 or step 3 is medium-frequency induction furnace or high temperature resistance furnace.
5. the method for direct heat reduction continuous production samarium metal as claimed in claim 1, is characterized in that, the condensation method in described step 3 is direct condensation or atomization condensation.
6. the method for direct heat reduction continuous production samarium metal as claimed in claim 5, is characterized in that, described direct condensation method is recirculated water cooling condensation.
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