CN108610015A - A kind of microwave absorbing material preparation method based on gangue - Google Patents
A kind of microwave absorbing material preparation method based on gangue Download PDFInfo
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- CN108610015A CN108610015A CN201810587005.7A CN201810587005A CN108610015A CN 108610015 A CN108610015 A CN 108610015A CN 201810587005 A CN201810587005 A CN 201810587005A CN 108610015 A CN108610015 A CN 108610015A
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- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/327—Iron group oxides, their mixed metal oxides, or oxide-forming salts thereof
- C04B2235/3279—Nickel oxides, nickalates, or oxide-forming salts thereof
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Abstract
The microwave absorbing material preparation method based on gangue that the present invention provides a kind of carrying out break process to gangue, obtains bastard coal mountain flour；Pickling is carried out to the bastard coal mountain flour, obtains pickling bastard coal mountain flour；By the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；The gangue based ceramic microsphere is impregnated in divalent nickel salt solution, obtains dipping microballoon；It is roasted after the dipping microballoon is dried, obtains the microwave absorbing material based on gangue.Method provided by the invention realizes the recycling of gangue using gangue as raw material, economizes on resources and cost；Meanwhile the method for the invention only needs simple breaker, mixing arrangement and calciner, it is low for equipment requirements, and operating process is easy, it is easy to implement, it can be used in the industrial production of batch.
Description
Technical field
The present invention relates to microwave absorbing material technical field more particularly to a kind of microwave absorbing material systems based on gangue
Preparation Method.
Background technology
With the high speed development of electronic technology, electronics, electrical equipment or other information system is more and more extensive answers
Used in the every field of the daily production and life of people, the thing followed is that electromagnetic radiation is flooded with people’s lives space, is made
At serious electromagnetic pollution, it has become another after noise pollution, atmosphere pollution, water pollution and solid waste pollution
Big public hazards.Therefore, it studies, exploitation causes extensive concern for the absorbing material of electromagnetic radiation pollution.Currently, ensureing to inhale
Under the premise of receiving intensity, microwave absorbing material is just good, inexpensive and preparation process simplification towards lightweight, wideband, stability
Direction is developed, to meet the protection requirements of large-scale electromagnetic equipment.
Traditional microwave absorbing material can be divided into magnetic loss type and dielectric loss type.Magnetic loss type absorbing material is mainly with carbonyl
Iron, Fe3O4、CoFe2O4And FeNi alloys etc. are representative, density height is its common problem, how to realize that lighting causes research
The extensive concern of personnel.Compared with magnetic loss absorbing material, the coating layer thickness of dielectric loss type absorbing material is larger, is suitable for more
Layer structure type design.However, the absorbing material of single form cannot concurrently reach multiband, wide band assimilation effect, such as
Magnetic loss and dielectric loss absorbing material are carried out effective compound to overcome single absorbing material by fruit by various methods
Deficiency helps to increase absorption frequency range, widens absorption band.In addition, only when the impedance of microwave absorbing material and free space
When close, incident electromagnetic wave could more into absorbing material inside and be depleted.Therefore, how to realize lightweight, how
With the effectively compound hot spot for having become the research of magnetic loss absorbing material of dielectric loss absorbing material.As professor Sun Genban will be magnetic golden
Belong to Co, Ni particle by liquid phase synthesis uniform load, being coated on grapheme material, that lightweight, absorbing property is prepared is good
Co/GN and Ni/GN composite materials；Qin Yong researcher then obtains Fe respectively using technique for atomic layer deposition3O4The carbon nanometer spiral shell of cladding
The graphene composite wave-suction material of rotation and Ni uniform loads.In addition, also numerous studies concentrate on preparing with Fe3O4、FeNi、Ni
Equal magnetic-particles are kernel, polypyrrole, SiO2, the dielectric materials such as C be composite material of core-shell structure that shell is constituted.The above thinking
General character be by heavy magnetic loss component by chemical method load, be coated on all kinds of dielectric types using carbon material as representative
On carrier, the composite wave-suction material for having both magnetic loss and dielectric loss effect to electromagnetic wave is formed, magnetic is not only efficiently solved
The high density problem of material is lost, and prepared Radar Absorbing Properties of Composites is excellent.
However, being used to prepare in the prior art in the method for composite microwave absorbing material, big multipair production equipment requires very
Height, complex technical process are only applicable to laboratory research, it is difficult to realize large-scale production and application.
Invention content
The microwave absorbing material preparation method based on gangue that the purpose of the present invention is to provide a kind of, this method is to production
Equipment requirement is low, and process is easy, easy to implement, can be used in large-scale industry application.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The microwave absorbing material preparation method based on gangue that the present invention provides a kind of, comprises the following steps：
(1) break process is carried out to gangue, obtains bastard coal mountain flour；
(2) pickling is carried out to the bastard coal mountain flour, obtains pickling bastard coal mountain flour；
(3) by the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；
(4) the gangue based ceramic microsphere is impregnated in divalent nickel salt solution, obtains dipping microballoon；
(5) it is roasted after drying the dipping microballoon, obtains the microwave absorbing material based on gangue.
Preferably, in the step (1) bastard coal mountain flour granularity≤300 mesh.
Preferably, spent pickling acid liquid is oxalic acid in the step (2).
Preferably, a concentration of 0.1~1mol/L of step (2) mesoxalic acid.
Preferably, raw material when step (3) mixing granulation also includes soluble starch；
The mass ratio of the pickling bastard coal mountain flour and soluble starch is 100:(0~40].
Preferably, the grain size of gangue based ceramic microsphere is 0.2~0.8cm in the step (3).
Preferably, in the step (4) divalent nickel salt solution a concentration of 0.05~1g/mL；
The ratio between the quality of the gangue based ceramic microsphere and the volume of divalent nickel salt solution are 1g:(5~15) mL.
Preferably, divalent nickel salt includes inorganic divalent nickel salt in the step (4)；
The inorganic divalent nickel salt is one or more of nickel nitrate, nickel sulfate and nickel chloride.
Preferably, the time impregnated in the step (4) is 18~for 24 hours.
Preferably, the temperature roasted in the step (5) is 400~1000 DEG C；
The time of the roasting is 1~5h.
The microwave absorbing material preparation method based on gangue that the present invention provides a kind of, comprises the following steps：(1) to coal
Spoil carries out break process, obtains bastard coal mountain flour；(2) pickling is carried out to the bastard coal mountain flour, obtains pickling bastard coal mountain flour；(3)
By the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；(4) by the gangue based ceramic microsphere
It is impregnated in divalent nickel salt solution, obtains dipping microballoon；(5) it is roasted after drying the dipping microballoon, obtains Ni-based base
In the microwave absorbing material of gangue.Method provided by the invention, using gangue as raw material, the recycling for realizing gangue is sharp again
With economizing on resources and cost；Meanwhile the method for the invention only needs simple breaker, mixing arrangement and calciner
, it is low for equipment requirements, and operating process is easy, it is easy to implement, it can be used in the industrial production of batch.By embodiment result
It is found that preparation method provided by the present application can obtain the microwave absorbing material based on gangue.
Description of the drawings
Fig. 1 is the microwave absorbing material based on gangue that embodiment 1 loads simple substance Ni in Different matching layer thickness
Electromagnetic wave absorption curve；
Fig. 2 is the X ray diffracting spectrum for the microwave absorbing material based on gangue that embodiment 2 loads simple substance Ni；
Fig. 3 be embodiment 2 load simple substance Ni based on the microwave absorbing material of gangue Different matching layer thickness electricity
Magnetic wave profile.
Fig. 4 be embodiment 3 load simple substance Ni based on the microwave absorbing material of gangue Different matching layer thickness electricity
Magnetic wave profile.
Specific implementation mode
The microwave absorbing material preparation method based on gangue that the present invention provides a kind of, comprises the following steps：
(1) break process is carried out to gangue, obtains bastard coal mountain flour；
(2) pickling is carried out to the bastard coal mountain flour, obtains pickling bastard coal mountain flour；
(3) by the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；
(4) the gangue based ceramic microsphere is impregnated in divalent nickel salt solution, obtains dipping microballoon；
(5) it is roasted after drying the dipping microballoon, obtains the microwave absorbing material based on gangue.
The present invention carries out break process to gangue, obtains bastard coal mountain flour.The present invention does not have the source of the gangue
Any particular/special requirement, using the gangue in source well known to those skilled in the art.
The present invention does not have the break process of the gangue special requirement, use well-known to those skilled in the art
Breaking method carries out, and can obtain the bastard coal mountain flour of target grain size.In the present invention, the bastard coal that the step (1) obtains
The granularity of mountain flour is preferably≤300 mesh, more preferably≤325 mesh.The bastard coal mountain flour is crushed to 300 mesh and following by the present invention
Grain size, convenient for the granulation in subsequent operations；If grain size is too big, the performance for being granulated balling-up is bad.
After obtaining bastard coal mountain flour, the present invention carries out pickling to the bastard coal mountain flour, obtains pickling bastard coal mountain flour.In the present invention
In, spent pickling acid liquid is preferably oxalic acid in the step (2), and the concentration of the oxalic acid is preferably 0.1~1mol/L, more preferably
0.3~0.8mol/L, most preferably 0.5~0.6mol/L.The present invention selects oxalic acid to carry out pickling to bastard coal mountain flour, is on the one hand
Due to the faintly acid of oxalic acid, other components in gangue will not be dissolved when removing the iron oxide in coal gangue component；Another party
Face not will produce any residual since oxalic acid is organic acid after subsequent roasting.
The present invention does not have particular/special requirement to the embodiment of the pickling, is well known side using those skilled in the art
Method carries out pickling.The present invention does not have particular/special requirement to the dosage of the acid solution, can infiltrate bastard coal mountain flour to be washed.
After the pickling, processing is dried in the bastard coal mountain flour after the preferred pickling of the present invention, to obtain dry pickling
Bastard coal mountain flour.In the present invention, the temperature of the drying process is preferably 100~110 DEG C, more preferably 104~106 DEG C；Institute
The time for stating drying process is preferably 5~6h.In the present invention, the drying process can avoid the moisture in acid solution to follow-up
Step has an adverse effect.
After obtaining pickling bastard coal mountain flour, the pickling bastard coal mountain flour and water mixing granulation are obtained bastard coal ground mass by the present invention
Ceramic microsphere.
In the present invention, raw material when step (3) mixing granulation preferably also includes soluble starch.In the present invention
In, when adding soluble starch granulation, the mass ratio of the pickling bastard coal mountain flour and soluble starch is preferably 100:(0~
40], more preferably 100:[10~30], most preferably 100:[20~25]；The pickling bastard coal mountain flour and soluble starch
The mass ratio of gross mass and water is preferably 5~10:1, more preferably 6~9:1, most preferably (7~8):1.The present invention is preferably first
Pickling bastard coal mountain flour and soluble starch are subjected to level-one mixing, obtain primary mixes；Then again by the primary mixes
With water mixing granulation, gangue based ceramic microsphere is obtained.In the present invention, the soluble starch has the function of pore creating material, energy
The porosity of product is enough improved, specifically soluble starch decomposes in postorder roasting process, leaves hole knot in the product
Structure.
In the present invention, the level-one mixing preferably carries out in the vertical intensive mixer perhaps of love, and the level-one mixing is stirred
It is preferably 800~1000r/min to mix rate, more preferably 850~950r/min, most preferably 900~920r/min；Described one
The time of grade mixing is preferably 3~5min.
In the present invention, the mixing granulation preferably carries out in the vertical intensive mixer perhaps of love, more preferably carries out on one side
The granulation, is slowly added water on one side；The stir speed (S.S.) of the mixing granulation is preferably 400~1200r/min, more preferably
600~1000r/min, most preferably 800~900r/min；The mixing granulation adds the water time to be preferably 2~4min, more excellent
It is selected as 3min；After adding all water, the duration of the mixing granulation is preferably 10~15min, more preferably 12~
13min.During the mixing granulation, the addition of water can make primary mixes bond balling-up.
In the present invention, when not adding soluble starch granulation, the mass ratio of the pickling bastard coal mountain flour and water is preferred
It is 5~10:1, more preferably 6~9:1, most preferably 7~8:1.The present invention directly mixes the pickling bastard coal mountain flour and water
It is granulated, obtains gangue based ceramic microsphere.In the present invention, mixing granulation described herein is consistent with mixing granulation described above,
It is no longer repeated herein.
Processing is dried in the substance that the present invention preferably obtains the mixing granulation, to remove Free water.In the present invention
In, the temperature of the drying process is preferably 90~110 DEG C, more preferably 104~105 DEG C；The time of the drying process with
It removes subject to all Free waters.
In the present invention, the grain size of gangue based ceramic microsphere is preferably 0.2~0.8cm in the step (3)；When described
When the grain size that mixing granulation process obtains product does not meet technology requirement, obtained product is screened, grain is screened out
The too big and too small product of diameter, obtains satisfactory gangue based ceramic microsphere.In the present invention, the gangue of the grain size
Based ceramic microsphere has best impregnation performance.
After obtaining gangue based ceramic microsphere, the present invention soaks the gangue based ceramic microsphere in divalent nickel salt solution
Stain obtains dipping microballoon.
In the present invention, the concentration of divalent nickel salt solution is preferably 0.05~1g/mL in the step (4), more preferably
0.067~0.6g/mL, most preferably 0.1~0.4g/mL；The quality and divalent nickel salt solution of the gangue based ceramic microsphere
The ratio between volume preferably 1g:5~15mL, more preferably 1g:8~13mL, most preferably 1g:10~12mL.
In the present invention, divalent nickel salt preferably comprises inorganic divalent nickel salt in the step (4)；The inorganic divalent nickel salt
Preferably one or more of nickel nitrate, nickel sulfate and nickel chloride；Since the nickel chloride and nickel sulfate can introduce sulfate radical
Ion and chlorion influence the performance of final products, therefore the present invention further preferably inorganic divalent nickel salt is nickel nitrate.
In the present invention, the dipping process carries out at room temperature, additional operation is heated or cooled without any；
The time of the dipping is preferably 18~for 24 hours, more preferably 20-22h.In dipping process of the present invention, divalent nickel salt solution
In bivalent nickel ion can diffuse to inside gangue based ceramic microsphere.
After obtaining dipping microballoon, the present invention roasts after drying the dipping microballoon, obtains Ni-based based on gangue
Microwave absorbing material.In the present invention, the temperature of the drying is preferably 50~70 DEG C, more preferably 55~65 DEG C, optimal
It is selected as 60~62 DEG C；The time of the drying is preferably 10~15h, more preferably 12~13h.In the present invention, the drying
The moisture removal that dipping process can be introduced, prevents the presence due to water from roasting process microballoon being caused to burst.
In the present invention, the roasting is lower preferably under inert atmosphere or vacuumized conditions carries out, the inert atmosphere
Preferably nitrogen or argon gas, the vacuum degree vacuumized are controlled i.e. according to condition well-known to those skilled in the art
It can；The temperature of the roasting is preferably 400~1000 DEG C；The time of the roasting is preferably 1~5h, more preferably 2~3h.
In the present invention, divalent nickel salt is reduced to elemental nickel by the C inside gangue in the roasting process.Meanwhile
In the roasting process, the fixed carbon inside gangue is understood some and is remained, and is dispersed in final product.This hair
In the bright roasting process, microballoon shape invariance is impregnated, only size can be shunk, and grain size is 0.1~0.7cm；The list
The fractional load of matter nickel partly enters inside microballoon and is uniformly mixed with microsphere component in microsphere surface.
The microwave absorbing material preparation method provided by the invention based on gangue is carried out with reference to embodiment detailed
Explanation, but they cannot be interpreted as limiting the scope of the present invention.
Embodiment 1
Break process is carried out to coal shale in brick making, the gangue of the mesh of grain size≤325 is obtained after the screening of 325 mesh standard sieves
Powder；
Pickling is carried out with the oxalic acid of a concentration of 0.5mol/L infiltration bastard coal mountain flour and removes iron, and permanent under the conditions of 110 DEG C
The dry 5h of temperature；
The bastard coal mountain flour after pickling is weighed to set with soluble starch (the 20% of the Coal gangue powder that mass ratio accounts for after pickling)
The rate stirring 5min that Yu Aili is permitted in intensive mixer with 900r/min is uniformly mixed, and mixed raw material powder is made；
In mass ratio 1：7 weigh deionized water and mixed raw material powder, are placed in love power and are permitted in intensive mixer (to add the water time
3min, rate 1000r/min, duration 12min) it is processed into ceramic green pellet, then by ceramic green pellet under the conditions of 100 DEG C
Drying, by being sieved into the gangue based ceramic microsphere that grain size is 0.2~0.8cm；
Nickel nitrate is dissolved in deionized water, is made containing metal ion Ni2+Precursor solution, the quality of nickel nitrate
Volume ratio with deionized water is 5g：20mL；
It weighs 1g gangue based ceramic microspheres and is placed in 10mL precursor solutions and impregnate 18h, obtain dipping microballoon；
Dipping microballoon taking-up is placed in baking oven dry 12h under the conditions of 60 DEG C, then in an inert atmosphere through 400 DEG C of perseverances
Room temperature is cooled to the furnace after temperature sintering 2h, obtains the microwave absorbing material based on gangue of load simple substance Ni.
By Fig. 1 and Fig. 2 it is found that the object phase composition that the embodiment obtains loaded article is Ni, the object of ceramic monolith is mainly mutually
AlNi, C and SiO2；On reflection loss curve (2-18GHz), with the variation (1.5-5.5mm) of absorbing material coating layer thickness,
Minimum reflection loss value of the frequency within the scope of 4-18GHz is below -10dB, and minimum reflection when coating layer thickness is 3.5mm
Loss value is -30dB.
Embodiment 2
Break process is carried out to coal shale in brick making, the gangue of the mesh of grain size≤325 is obtained after the screening of 325 mesh standard sieves
Powder；
Pickling is carried out with the oxalic acid of a concentration of 0.8mol/L infiltration bastard coal mountain flour and removes iron, and permanent under the conditions of 100 DEG C
The dry 6h of temperature；
The bastard coal mountain flour after pickling is weighed to set with soluble starch (the 20% of the Coal gangue powder that mass ratio accounts for after pickling)
The rate stirring 3min that Yu Aili is permitted in intensive mixer with 900r/min is uniformly mixed, and mixed raw material powder is made；
In mass ratio 1：8 weigh deionized water and mixed raw material powder, are placed in and like that power is permitted intensive mixer and (adds the water time
3min, rate 1200r/min, duration 10min) in be processed into ceramic green pellet, then by ceramic green pellet in 110 DEG C of conditions
Lower drying, by being sieved into the gangue based ceramic microsphere that grain size is 0.2~0.8cm；
Nickel nitrate is dissolved in deionized water, is made containing metal ion Ni2+Precursor solution, the quality of nickel nitrate
Volume ratio with deionized water is 4g：15mL；
It weighs 1g gangue based ceramic microspheres and is placed in 10mL precursor solutions and impregnate 20h, obtain dipping microballoon；
Dipping microballoon taking-up is placed in baking oven dry 10h under the conditions of 70 DEG C, then in an inert atmosphere through 700 DEG C of perseverances
Room temperature is cooled to the furnace after temperature sintering 2h, obtains the microwave absorbing material based on gangue of load simple substance Ni.
From the figure 3, it may be seen that the embodiment obtains the object phase composition of loaded article based on simple substance Ni, the object of ceramic monolith is mutually main
For AlNi, C and SiO2；When microwave absorbing coating thickness is more than 4mm, there is biabsorption peak in (2-18GHz) on reflection loss curve,
Minimum reflection loss value when coating layer thickness is 2.5mm is -22dB.
Embodiment 3
Break process is carried out to coal shale in brick making, the gangue of the mesh of grain size≤325 is obtained after the screening of 325 mesh standard sieves
Powder；
Pickling is carried out with the oxalic acid of a concentration of 0.3mol/L infiltration bastard coal mountain flour and removes iron, and permanent under the conditions of 110 DEG C
The dry 5h of temperature；
The bastard coal mountain flour after pickling is weighed to set with soluble starch (the 30% of the Coal gangue powder that mass ratio accounts for after pickling)
The rate stirring 5min that Yu Aili is permitted in intensive mixer with 900r/min is uniformly mixed, and mixed raw material powder is made；
In mass ratio 1：9 weigh deionized water and mixed raw material powder, are placed in and like that power is permitted intensive mixer and (adds the water time
3min, rate 600r/min, duration 15min) in be processed into ceramic green pellet, then by ceramic green pellet under the conditions of 90 DEG C
Drying, by being sieved into the gangue based ceramic microsphere that grain size is 0.2~0.8cm；
Nickel nitrate is dissolved in deionized water, is made containing metal ion Ni2+Precursor solution, the quality of nickel nitrate
Volume ratio with deionized water is 5g：25mL；
It weighs 1g gangue based ceramic microspheres and is placed in 10mL precursor solutions and impregnate 18h, obtain dipping microballoon；
Dipping microballoon taking-up is placed in baking oven dry 12h under the conditions of 60 DEG C, then in an inert atmosphere through 900 DEG C of perseverances
Room temperature is cooled to the furnace after temperature sintering 2h, obtains the microwave absorbing material based on gangue of load simple substance Ni.
As shown in Figure 4, the object phase composition which obtains loaded article is Ni, and the object of ceramic monolith is mainly mutually AlNi, C
And SiO2；On reflection loss curve (2-18GHz), with the variation (1.5-5.5mm) of absorbing material coating layer thickness, frequency exists
Minimum reflection loss value within the scope of 3-18GHz is below -10dB.
As seen from the above embodiment, the microwave absorbing material preparation method based on gangue that the present invention provides a kind of, packet
Containing following steps：(1) break process is carried out to gangue, obtains bastard coal mountain flour；(2) pickling is carried out to the bastard coal mountain flour, obtained
To pickling bastard coal mountain flour；(3) by the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；(4) by institute
It states gangue based ceramic microsphere to impregnate in divalent nickel salt solution, obtains dipping microballoon；(5) the dipping microballoon is dried laggard
Row roasting, obtains the microwave absorbing material based on gangue.Method provided by the invention realizes coal using gangue as raw material
The recycling of spoil, economizes on resources and cost；Meanwhile the method for the invention only needs simple breaker, mixing
Device and calciner, it is low for equipment requirements, and operating process is easy, easy to implement, the industry that can be used in batch is raw
Production.By embodiment result it is found that preparation method provided by the present application can obtain the microwave absorbing material based on gangue.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of microwave absorbing material preparation method based on gangue, comprises the following steps：
(1) break process is carried out to gangue, obtains bastard coal mountain flour；
(2) pickling is carried out to the bastard coal mountain flour, obtains pickling bastard coal mountain flour；
(3) by the pickling bastard coal mountain flour and water mixing granulation, gangue based ceramic microsphere is obtained；
(4) the gangue based ceramic microsphere is impregnated in divalent nickel salt solution, obtains dipping microballoon；
(5) it is roasted after drying the dipping microballoon, obtains the microwave absorbing material based on gangue.
2. preparation method according to claim 1, which is characterized in that granularity≤300 of bastard coal mountain flour in the step (1)
Mesh.
3. preparation method according to claim 1 or 2, which is characterized in that spent pickling acid liquid is grass in the step (2)
Acid.
4. preparation method according to claim 3, which is characterized in that a concentration of the 0.1 of step (2) mesoxalic acid~
1mol/L。
5. preparation method according to claim 1, which is characterized in that raw material when step (3) mixing granulation also wraps
Soluble-containing starch；
The mass ratio of the pickling bastard coal mountain flour and soluble starch is 100:(0~40].
6. preparation method according to claim 1 or 5, which is characterized in that gangue based ceramic microsphere in the step (3)
Grain size be 0.2~0.8cm.
7. preparation method according to claim 1, which is characterized in that the concentration of divalent nickel salt solution in the step (4)
For 0.05~1g/mL；
The ratio between the quality of the gangue based ceramic microsphere and the volume of divalent nickel salt solution are 1g:(5~15) mL.
8. preparation method according to claim 1 or claim 7, which is characterized in that divalent nickel salt includes inorganic in the step (4)
Divalent nickel salt；
The inorganic divalent nickel salt is one or more of nickel nitrate, nickel sulfate and nickel chloride.
9. preparation method according to claim 8, which is characterized in that the time impregnated in the step (4) is 18~
24h。
10. preparation method according to claim 1, which is characterized in that the temperature roasted in the step (5) is 400~
1000℃；
The time of the roasting is 1~5h.
Priority Applications (1)
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| CN110699040A (en) * | 2019-10-11 | 2020-01-17 | 太原科技大学 | Method for preparing composite microwave absorbing material by using coal gangue |
| CN110759711A (en) * | 2019-10-11 | 2020-02-07 | 太原科技大学 | Method for preparing spherical ceramic composite microwave absorbing material by utilizing coal gangue |
| CN111807856A (en) * | 2020-06-30 | 2020-10-23 | 太原科技大学 | Preparation method of porous ceramic composite wave-absorbing material loaded with magnetic metal cobalt or nickel |
| CN112341153A (en) * | 2020-10-20 | 2021-02-09 | 上海航翼高新技术发展研究院有限公司 | Waste porous magnetic ceramic system based on 3D printing technology and preparation method thereof |
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| CN110759711A (en) * | 2019-10-11 | 2020-02-07 | 太原科技大学 | Method for preparing spherical ceramic composite microwave absorbing material by utilizing coal gangue |
| CN111807856A (en) * | 2020-06-30 | 2020-10-23 | 太原科技大学 | Preparation method of porous ceramic composite wave-absorbing material loaded with magnetic metal cobalt or nickel |
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