CN1718790A - Method of preparing cobalt oxide by microwave calcining cobalt salt and it powder material microwave calcining furnace - Google Patents
Method of preparing cobalt oxide by microwave calcining cobalt salt and it powder material microwave calcining furnace Download PDFInfo
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- CN1718790A CN1718790A CN 200510031904 CN200510031904A CN1718790A CN 1718790 A CN1718790 A CN 1718790A CN 200510031904 CN200510031904 CN 200510031904 CN 200510031904 A CN200510031904 A CN 200510031904A CN 1718790 A CN1718790 A CN 1718790A
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Abstract
A process for preparing cabolt oxide through calcining cabolt salt by microwave includes such steps as adding cabolt oxide into furnace, microwave heating to 400-800 deg.C, quantitatively adding Co salt and air, and calcining at 400-800 deg.C to obtain the cabalt oxide powder with 71-73.8% for Co content. Its microwave sintering furnace is composed of a conic internal cavity, a spiral belt-type conic stirrer, top insulating layer, driver for said conic stirrer, screw feeder, screw-type discharging unit, a microwave source, and several microwave guide sets.
Description
Technical field
The present invention relates to a kind of microwave sintering process method and microwave sintering apparatus, relate in particular to a kind of powder body material microwave agglomerating furnace that utilizes the microwave calcination metal-salt to prepare the method for metal oxide and implement this method.
Background technology
The preparation of existing cobalt oxide normally utilizes electric tube furnace and rotary kiln, cobalt oxalate or cobaltous carbonate calcining are the different cobalt oxide of cobalt contents, need heating element, thermosteresis is big, and thermograde is big, product composition and granularity are inhomogeneous, need in the calcined oxide process to use stainless steel or ceramic boat, make product increase iron, the consumption of boat is also bigger, and dust from flying, the operation labour intensity also big, output depends on every stove batch and the length of sintering period.And microwave sintering mainly is the coupling that utilizes micro-wave energy and material, be transformed into heat energy direct heating material to sintering temperature by the dielectric loss of material and the in-fighting of magnetic dielectric loss consumption generation, being sintered material itself is exactly heating element, thereby thermosteresis is little, and because of the penetration depth of microwave big, thermograde is very little, can heat up apace and lower the temperature, thereby whole sintering process is shortened significantly, there is not shade influence, can high performance sintered products, so microwave technology will obtain using more widely gradually.Intermittent type microwave sintering method and equipment have been had at present both at home and abroad, Chinese patent 03226766.5 also provides a kind of continuous-type microwave agglomerating plant, comprise feed mechanism, microwave source, transition waceguide, body of heater, burner hearth, discharging structure, thermal insulation layer, temperature measurer, the microwave-assisted absorbing material, its feed system, sintering body of heater and discharge system are the vertical layout of upper, middle and lower, can realize stoking, its chain-belt type or rollaway type input and output material transporting mechanism complex structure, the cost of manufacture height, and must use boat, and the easy loss of boat, and manual loading and unloading material, its operation labour intensity height causes certain dust from flying again, does not meet the health environment-friendly requirement.
Summary of the invention
The present invention is directed to the deficiency of aforesaid method, providing a kind of utilizes the microwave calcination Cobalt salts to prepare the method for cobalt metal oxide and implements the used powder body material microwave agglomerating furnace of this method, energy-conservation, efficient, continuous calcining, work simplification, device structure advantages of simple, cost is low, and do not need boat, labour intensity is low, and health environment-friendly.
Microwave calcination cobalt salt of the present invention prepares the method for cobalt oxide, may further comprise the steps successively:
1) closes valve plate between the burner hearth of powder body material microwave agglomerating furnace and its spiral discharging mechanism, start its screw feeder structure, stop the spiral charging after 10%～15% the cobalt oxide that accounts for furnace volume added burner hearth, cobalt salt is added in the feed bin of screw feeder structure;
2) start helix agitator and microwave source in the powder body material microwave agglomerating furnace, the heated oxide cobalt makes temperature reach 400 ℃～800 ℃;
3) open valve plate, start the spiral charging and discharging mechanism of powder body material microwave agglomerating furnace simultaneously, quantitatively in burner hearth, add cobalt salt by the input speed of 1.2～1.5kg/min, in the time of charging by the air inlet port of powder body material microwave agglomerating furnace with (12.5～15) m
3The flow input pressurized air of/h, the controlled microwave source power keeps the interior temperature of charge of stove between 400 ℃～800 ℃, make cobalt salt fully calcined for by mass percentage, cobalt contents is 71.0～73.8% cobalt oxide powder, spiral discharging mechanism is with the speed output cobalt oxide powder of 0.5～0.7kg/min.
Implement the powder body material microwave agglomerating furnace that microwave calcination cobalt salt of the present invention prepares the method for cobalt oxide, comprise feed mechanism, the microwave source that places upper furnace, the transition waceguide that is arranged on thermal insulation layer, body of heater, burner hearth, the discharging structure that places lower furnace portion, thermal insulation layer, temperature measurer, be filled with the microwave-assisted absorbing material between thermal insulation layer and the burner hearth, it is characterized in that: described burner hearth is up big and down small awl bucket shape structure, be provided with helical-ribbon type taper agitator in it, the transmission rig outer with the thermal insulation layer that places upper furnace links to each other.
Feed mechanism is the screw feeder structure; Discharging mechanism is a water-cooled spiral discharging mechanism, is connected with burner hearth by valve plate.
Microwave source and transition waceguide are arranged around burner hearth, are a cover microwave source and the combination of many cover transition waceguides.
Be provided with at least one group of inlet mouth around the burner hearth, top is provided with at least one group of venting port, is provided with the stainless steel microporous filter on described inlet mouth, the venting port.
Burner hearth is provided with the observation port of infrared thermometer.
Burner hearth is a ceramic material, and helical-ribbon type taper agitator is steel construction surface lining stupalith or stainless steel.
Microwave calcination cobalt salt of the present invention prepares the method for cobalt oxide, reaches subsequently constantly the cobalt salt of adding with cobalt oxide and makes full use of micro-wave energy as heating element, and heat is imitated height, and method is simple and practical, and the product grains structure that obtains is trickle, density is high, stable performance.Present method adopts the spiral charging and discharging mechanism of powder body material microwave agglomerating furnace, realize that the continuous calcining cobalt salt prepares cobalt oxide, need not boat, and preliminary thermal source---the cobalt oxide that adds, except that granularity is slightly grown slightly, composition, organize no change, can be used as product output equally, or again as quantity-produced thermal source next time.
The awl bucket shape burner hearth of powder body material microwave agglomerating furnace of the present invention, in establish helical-ribbon type taper agitator, its center convolution and ribbon material is upwards promoted by the bottom and or along burner hearth taper barrel spiral lifting, throw, material and temperature field are even, have accelerated the sintering of powdered material.Spiral charging and discharging mechanism has guaranteed the homogeneity and the continuity of inlet amount, input speed, and burner hearth and extraneous sealing during work, has realized the continuous-type microwave sintering of powder body material under microwave action; After for some time, the powder of part flows downward around center convolution by deadweight, forces cooling through water-cooled spiral discharging mechanism, and entering feed bin under totally enclosed state becomes product.This microwave agglomerating furnace is simple in structure, and cost of manufacture is low, and charging, sintering, discharging are carried out continuously, does not need manually to load and unload boat, the production efficiency height, and do not have dust from flying, health environment-friendly.
One cover microwave source makes up with the transition waceguide that many covers pass through thermal insulation layer, around the sintering burner hearth, arrange, space between thermal insulation layer and the sintering burner hearth is filled and is sintered the close microwave-assisted absorbing material of powder body material microwave absorption coefficient, guarantee homogeneity, the continuity of microwave field strength, reduce the thermograde that is sintered the zone to greatest extent, make micro-wave energy effective rate of utilization optimization, but according to output, temperature, rate request also reasonable Arrangement overlap microwave source and transition waceguide simultaneously more.
The helical-ribbon type taper agitator of the sintering burner hearth of ceramic material, steel construction surface lining stupalith or stainless steel is suitable for microwave sintering and contaminated material not.
At least being provided with one group of inlet mouth around the sintering burner hearth feeds in the burner hearth; input top is provided with one group of venting port at least, is provided with the stainless steel microporous filter on the gas port like this, both has been convenient to input, has got rid of protection or reaction atmosphere; prevented that dust from raising outward, covered microwave leakage again effectively frequently.
Be provided with the observation port that supplies infrared thermometry in the sintering upper furnace, also can pass the microwave-assisted absorbing material around the sintering burner hearth, thermal insulation layer is provided with the observation port for infrared thermometry, can monitor sintering temperature easily like this, sintering temperature is regulated and control.
Description of drawings
Fig. 1 implements the main sectional view of powder body material microwave agglomerating furnace that microwave calcination cobalt salt of the present invention prepares the method for cobalt oxide;
Fig. 2 is the vertical view of Fig. 1.
1-feed mechanism 2-microwave source 3-transition waceguide 4-body of heater 5-burner hearth 6-discharging mechanism
7,8-thermal insulation layer 9-temperature measurer 10-microwave-assisted absorbing material 11-helical-ribbon type taper agitator
12-transmission rig 13-inlet mouth 14-air outlet 15-observation port 16-valve plate
1a-feed mechanism spiral 6a-discharging mechanism spiral 6b-discharging mechanism watercooling jacket
Embodiment
Below in conjunction with implementing powder body material microwave agglomerating furnace of the present invention, the method that microwave calcination cobalt salt of the present invention is prepared cobalt oxide is further described.
As shown in Figure 1, 2, powder body material microwave agglomerating furnace of the present invention comprises feed mechanism 1, microwave source 2, transition waceguide 3, body of heater 4, burner hearth 5, discharging mechanism 6, thermal insulation layer 7,8, temperature measurer 9.Burner hearth 5 places in the body of heater 4, and thermal insulation layer 8 is arranged between body of heater 4, burner hearth 5 and around burner hearth 5, fills microwave-assisted absorbing material 10 between thermal insulation layer 8 and the burner hearth 5.Feed mechanism 1, discharge system 6 are screw mechanism, 1a, 6a are respectively the charging and discharging spiral, and discharging mechanism 6 is the water-cooled spiral discharging mechanism of tyre watercooling jacket 6b, the thermal insulation layer 7 that feed mechanism 1 passes burner hearth 5 tops is connected with burner hearth 5, discharge system 6 pass burner hearth 5 bottoms thermal insulation layer 7, be connected with burner hearth 5 by valve plate 16, promptly feed system 1, burner hearth 5 and discharge system 6 are the vertical layout in upper, middle and lower.Burner hearth 5 is designed to up big and down small awl bucket shape structure, is provided with helical-ribbon type taper agitator 11 in it, links to each other with thermal insulation layer 7 transmission rig 12 outward that places burner hearth 5 tops; Burner hearth 5 is a ceramic material, and helical-ribbon type taper agitator 11 is steel construction surface lining stupalith or stainless steel.One cover microwave source 2 and 3 combinations of six cover transition waceguides arrange that around burner hearth 5 microwave imports burner hearth 5 by the transition waceguide 3 that places thermal insulation layer 8.The setting of microwave source 2, transition waceguide 3 and microwave-assisted absorbing material 10 makes the micro-wave energy effective rate of utilization realize optimization.
The center convolution of helical-ribbon type taper agitator 11 can upwards promote powder by the bottom, ribbon then with the part powder from bottom to top along the lifting of spiraling of burner hearth taper barrel, and powder in the cutting burner hearth 5, make it not lump, because the linear velocity of top ribbon is bigger, ribbon is also thrown powder on top, and material and temperature field are more even like this, has accelerated the sintering of powdered material.Spiral charging and discharging mechanism, homogeneity and the continuity of inlet amount, input speed have been guaranteed, and when work burner hearth 5 with extraneous sealing, feed mechanism 1 is controlled with helical-ribbon type taper agitator 11,6 interlocks of water-cooled discharging mechanism, has realized the continuous-type microwave sintering of powder body material under microwave action; After for some time, the powder of part flows downward around center convolution by deadweight, forces cooling through water-cooled spiral discharging mechanism 6, and entering feed bin under totally enclosed state becomes product.The utility model is simple in structure, does not need manually to load and unload boat, no dust from flying, and health environment-friendly, labour intensity is low, the production efficiency height.
Be provided with one group of inlet mouth 12 around the burner hearth 5, feed in the burner hearth 5, import protection or reaction atmosphere, top is provided with one group of venting port 13, and inlet, outlet also can be provided with many groups around burner hearth 5; The stainless steel microporous filter all is set on inlet mouth and venting port, prevents that dust from raising outward, cover microwave leakage frequently.
Monitoring and regulation and control sintering temperature are convenient in burner hearth 5 tops or be provided with the observation port 14 of infrared thermometer all around.
Embodiment 1: 6 valve plates 16 of burner hearth 5 and its spiral discharging mechanism of closing continuous powdery material microwave sintering oven, start its screw feeder structure 1, stop the spiral charging after the cobalt oxide that accounts for burner hearth 5 volumetrical 10% added burner hearth 5, cobalt oxalate is added in the feed bin of screw feeder structure 1; Start helix agitator 11 and microwave source 2 in the continuous powdery material microwave sintering oven, the heated oxide cobalt, by being arranged at the infrared thermometer of upper furnace, after detection cobalt oxide temperature reaches 400 ℃, open valve plate 16, start the spiral charging and discharging mechanism 1,6 of continuous powdery material microwave sintering oven simultaneously, the input speed of pressing 1.5kg/min adds cobalt oxalate in burner hearth 5, in the time of charging by the air inlet port 13 of continuous powdery material microwave sintering oven with 15m
3The flow input pressurized air of/h, controlled microwave source 2 power keep the interior temperature of charge of stove between 420 ℃ ± 20 ℃, making cobalt oxalate fully calcined is cobalt oxide powder, speed output through water-cooled spiral discharging 6 mechanisms with 0.5kg/min, its cobalt contents is 71.4% by mass percentage, granularity fsss:1.21.
Example 2: 6 valve plates 16 of burner hearth 5 and its spiral discharging mechanism of closing continuous powdery material microwave sintering oven, start its screw feeder structure 1, stop the spiral charging after the cobalt oxide that accounts for burner hearth 5 volumetrical 15% added burner hearth 5, cobaltous carbonate is added in the feed bin of screw feeder structure 1; Start helix agitator 11 and microwave source 2 in the continuous powdery material microwave sintering oven, the heated oxide cobalt, by being arranged at the infrared thermometer of upper furnace, after detection cobalt oxide temperature reaches 600 ℃, open valve plate 16, start the spiral charging and discharging mechanism 1,6 of continuous powdery material microwave sintering oven simultaneously, the input speed of pressing 1.2kg/min adds cobalt oxalate in burner hearth 5, in the time of charging by the air inlet port 13 of continuous powdery material microwave sintering oven with 12.5m
3The flow input pressurized air of/h, controlled microwave source 2 power keep the interior temperature of charge of stove between 620 ℃ ± 20 ℃, making cobaltous carbonate fully calcined is cobalt oxide powder, the nearly ball-type of powder morphology, speed output through water-cooled spiral discharging 6 mechanisms with 0.6kg/min, its cobalt contents is 72.6% by mass percentage, granularity fsss:1.81.
Example 3: 6 valve plates 16 of burner hearth 5 and its spiral discharging mechanism of closing continuous powdery material microwave sintering oven, start its screw feeder structure 1, stop the spiral charging after the cobalt oxide that accounts for burner hearth 5 volumetrical 12.5% added burner hearth 5, cobaltous carbonate is added in the feed bin of screw feeder structure 1; Start helix agitator 11 and microwave source 2 in the continuous powdery material microwave sintering oven, the heated oxide cobalt, by being arranged at the infrared thermometer of upper furnace, after detection cobalt oxide temperature reaches 800 ℃, open valve plate 16, start the spiral charging and discharging mechanism 1,6 of continuous powdery material microwave sintering oven simultaneously, the input speed of pressing 1.5kg/min adds cobalt oxalate in burner hearth 5, in the time of charging by the air inlet port 13 of continuous powdery material microwave sintering oven with 15m
3The flow input pressurized air of/h, controlled microwave source 2 power keep the interior temperature of charge of stove between 620 ℃ ± 20 ℃, making cobaltous carbonate fully calcined is cobalt oxide powder, particle is very even, speed output through water-cooled spiral discharging 6 mechanisms with 0.7kg/min, its cobalt contents is 73.9% by mass percentage, granularity fsss:1.93.
Continuous powdery material microwave burning stove of the present invention not only is suitable for the microwave calcination cobalt salt and prepares cobalt oxide, is applicable to the microwave sintering of various polarity powder particle materials such as cemented carbide industry, electron trade, ceramic industry too.
Claims (7)
1, a kind of microwave calcination cobalt salt prepares the method for cobalt oxide, may further comprise the steps successively:
1) closes valve plate (16) between the burner hearth (5) of powder body material microwave agglomerating furnace and its spiral discharging mechanism (6), start its screw feeder structure (1), stop the spiral charging after the cobalt oxide that will account for burner hearth (5) volumetrical 10%～15% adds burner hearth (5), cobalt salt is added in the feed bin of screw feeder structure;
2) start helix agitator (11) and microwave source (2) in the powder body material microwave agglomerating furnace, the heated oxide cobalt makes temperature reach 400 ℃～800 ℃;
3) open valve plate (16), start the spiral charging and discharging mechanism (1,6) of powder body material microwave agglomerating furnace simultaneously, by the quantitative adding cobalt salt to burner hearth (5) in of the input speed of 1.2～1.5kg/min, in the time of charging by the air inlet port (13) of powder body material microwave agglomerating furnace with (12.5～15) m
3The flow input pressurized air of/h, controlled microwave source (2) power keeps the interior temperature of charge of stove between 400 ℃～800 ℃, make cobalt salt fully calcined for by mass percentage, cobalt contents is 71.0～73.8% cobalt oxide powder, spiral discharging (6) mechanism is with the speed output cobalt oxide powder of 0.5～0.7kg/min.
2, a kind ofly implement the powder body material microwave agglomerating furnace that the described microwave calcination cobalt salt of claim 1 prepares the method for cobalt oxide, comprise the feed mechanism (1) that places burner hearth (5) top, microwave source (2), be arranged on the transition waceguide (3) in the thermal insulation layer (8), body of heater (4), burner hearth (5), place the discharging mechanism (6) of burner hearth (5) bottom, thermal insulation layer (7,8), temperature measurer (9), be filled with microwave-assisted absorbing material (10) between thermal insulation layer (8) and the burner hearth (5), it is characterized in that: described burner hearth (5) is up big and down small awl bucket shape structure, be provided with helical-ribbon type taper agitator (11) in it, the transmission rig (12) outer with the thermal insulation layer (7) that places burner hearth (5) top links to each other.
3, a kind of powder body material microwave agglomerating furnace as claimed in claim 2 is characterized in that: described feed mechanism (1) is the screw feeder structure; Described discharging mechanism (6) is a water-cooled spiral discharging mechanism, is connected with burner hearth (5) by valve plate (16).
4, a kind of powder body material microwave agglomerating furnace as claimed in claim 2 is characterized in that: described microwave source (2) and transition waceguide (3) are arranged all around along burner hearth (5), are a cover microwave source (2) and many cover transition waceguides (3) combination.
5, a kind of powder body material microwave agglomerating furnace as claimed in claim 2, it is characterized in that: described burner hearth (5) is provided with at least one group of inlet mouth (13) all around, top is provided with at least one group of venting port (14), is provided with the stainless steel microporous filter on described inlet mouth, the venting port.
6, a kind of powder body material microwave agglomerating furnace as claimed in claim 2 is characterized in that: described burner hearth (5) is provided with the observation port (15) of infrared thermometer.
7, a kind of powder body material microwave agglomerating furnace as claimed in claim 2 is characterized in that: described burner hearth (5) is a ceramic material, and helical-ribbon type taper agitator (11) is steel construction surface lining stupalith or stainless steel.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901343A (en) * | 2012-11-12 | 2013-01-30 | 湖南山联新材科技有限公司 | Industrial microwave sintering hard alloy equipment |
| CN103822464A (en) * | 2012-11-19 | 2014-05-28 | 黄旭鹏 | Industrial continuous high-temperature microwave calcining furnace for mineral granules and powder |
| CN109896529A (en) * | 2019-03-20 | 2019-06-18 | 唐山顺浩环保科技有限公司 | A kind of production method and microwave equipment of microwave fusing aluminum silicate minerals |
| CN110396631A (en) * | 2019-08-02 | 2019-11-01 | 昆明理工大学 | A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy |
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| CN2250945Y (en) * | 1995-12-05 | 1997-04-02 | 陈恺瑞 | Water purifier with front-located filtering back-flushing and residual water draining device |
| US6066290A (en) * | 1996-07-26 | 2000-05-23 | The Pennsylvania State Research Foundation | Method and apparatus for transporting green work pieces through a microwave sintering system |
| CN100417904C (en) * | 2003-01-15 | 2008-09-10 | 长沙隆泰科技有限公司 | Solid material sintering furnace |
| CN2604444Y (en) * | 2003-02-28 | 2004-02-25 | 贾成会 | Ferrous refined powder nodule fritting shaft furnace |
| CN2807171Y (en) * | 2005-07-22 | 2006-08-16 | 株洲硬质合金集团有限公司 | Microwave sintering furnace for powder material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102901343A (en) * | 2012-11-12 | 2013-01-30 | 湖南山联新材科技有限公司 | Industrial microwave sintering hard alloy equipment |
| CN103822464A (en) * | 2012-11-19 | 2014-05-28 | 黄旭鹏 | Industrial continuous high-temperature microwave calcining furnace for mineral granules and powder |
| CN109896529A (en) * | 2019-03-20 | 2019-06-18 | 唐山顺浩环保科技有限公司 | A kind of production method and microwave equipment of microwave fusing aluminum silicate minerals |
| CN110396631A (en) * | 2019-08-02 | 2019-11-01 | 昆明理工大学 | A kind of continuous method and device for preparing WC-10Ni-ZrO2 hard alloy |
| CN110396631B (en) * | 2019-08-02 | 2021-04-23 | 昆明理工大学 | Method and device for continuously preparing WC-10Ni-ZrO2 hard alloy |
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