CN106583752B - A kind of preparation method of carried magnetic metal sepiolite composite granule or fiber - Google Patents
A kind of preparation method of carried magnetic metal sepiolite composite granule or fiber Download PDFInfo
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- CN106583752B CN106583752B CN201611110090.5A CN201611110090A CN106583752B CN 106583752 B CN106583752 B CN 106583752B CN 201611110090 A CN201611110090 A CN 201611110090A CN 106583752 B CN106583752 B CN 106583752B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/30—Making metallic powder or suspensions thereof using chemical processes with decomposition of metal compounds, e.g. by pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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Abstract
The invention discloses the preparation methods of a kind of carried magnetic metal sepiolite composite granule or fiber, this method is that sepiolite powder or sepiolite fibre are carried out calcination processing, or sepiolite powder or sepiolite fibre are placed in immersion treatment in silane coupler solution, obtain pretreatment sepiolite powder or sepiolite fibre, after the pretreatment sepiolite powder or sepiolite fibre are mixed with magnetic metal organic solution, it is placed in sealing reaction kettle, carry out pyrolytic reaction, to obtain the final product, magnetic metal is uniformly distributed in sepiolite surface or hole in the composite material of preparation, magnetic metal load capacity is high, can its electromagnetic matching performance be adjusted by load capacity and metal proportioning；The preparation method simple process and low cost, is conducive to mass produce.
Description
Technical field
The present invention relates to the preparation processes of a kind of magnetic metal modified meerschaum powder or fibrous material, more particularly to a kind of
The preparation method of carried magnetic metal sepiolite composite powder or fiber is prepared by pyrolysismethod；Belong to electromagnetic-wave absorbent preparation
Technical field.
Background technology
With the development of science and technology and electronics industry, electromagnetic wave is applied to each side of daily life and national defense and military
Face.The popularization and application of broadcast, TV and wireless network etc., greatly facilitates daily life.However, also result in electricity
Magnetic wave is ubiquitous, not only influences the normal operation of various electronic equipments, and human body and natural environment are also resulted in be difficult to it is pre-
The influence estimated, continuous this facilitate electromagnetic-wave absorbent develop and apply；Militarily, infrared, laser, radar etc. detect body
The popularization and application of system has high detection accuracy, in order to fight each side's detection, protects itself strength, and various countries are by electromagnetic wave absorption
Material is widely used in weaponry.Therefore, absorbing material development and application have daily life and national defense and military important
Meaning.
Carbonyl iron has higher magnetic conductivity and thermal stability, and in S-band as typical magnetic loss type absorbing material
(2~4GHz) has certain absorption potentiality, but its density is big, loss mechanisms are single, is increasingly difficult to growing at present to meet
Application requirement.[Li Ze, Xu Baocai, Wang Jianjiang etc., the BaTiO such as Li Ze3Coat preparation and its wave absorbtion of carbonyl iron wave absorbing agent
It can study, artificial lens journal, 2016,45 (9)：2240~2245] it is normal by coating adjusting dielectric material in carbonyl iron surface
The absorbing property of material is counted and improves, but absorption frequency range is narrow, in X-band (8~12GHz) assimilation effect unobvious.Li Xiang into
Deng [Li Xiangcheng, Gong Rongzhou, Lu Pei etc., the fibre structure control of carbonyl Fe-Ni fiber and electromagnetic mechanism research, rare-earth metal material
Scientific and engineering, 2007,36 (23)：222~224] carbonyl iron and carbonyl iron are prepared for using carbonyl iron compound thermal decomposition method
Nickel fiber, reflectance loss is less than -5dB in the range of 8~12GHz, but loss is relatively low, is not enough to input application.
Sepiolite is aqueous chain stratiform magnesium silicate mineral, and structure is made of class talc lamellar band, formation and Hai Pao
The consistent channel of stone radial direction has extremely strong absorption property, good dispersion performance and thermal stability, can 1300~
1500 DEG C of holding structure stability, these features make sepiolite have excellent load performance.For sepiolite and its modified master
It to conduct a research in water pollution to the processing capacity of heavy metal ion for it.Wang Wei waits clearly [Wang Weiqing, Feng Qiming, Dong
Send out a kind of diligent etc., method for preparing magnetic meerschaum, national inventing patent, CN 101569851] using chemical coprecipitation legal system
It is standby to contain ferritic magnetic meerschaum, not only there is good ion exchange to adsorb ability heavy metal ion, but also have to organic matter
Strong absorption property, solve the problems, such as sepiolite processing waste water after long-term suspension in water, be difficult to quickly recycle；Li Shuanshuan etc.
[Li Shuanshuan, Dai Youzhi, Li Na etc., the development of iron modified meerschaum and absorption antimony characteristic, water technology, 2009,35 (5)：49
~52] sepiolite is modified using iron chloride to obtain ferriferous oxide modified meerschaum (IMS), using antimony as target contaminant,
The processing capacity to stibium-containing wastewater is investigated.Xuization just waits [Xu Huafang, Hu Zhenqi, Gong Bikai etc., composite modified sepiolite physics and chemistry
Specificity analysis, nonmetallic ore, 2011,34 (1):18~21] activation of a kind of compound sepiolite method of modifying of use, i.e. sepiolite-
Hydrochloric acid-manganese chloride is modified, and is obtained sour manganese modified meerschaum, is increased sepiolite specific surface area, enhances absorption property, and investigate
To Cu2+Processing capacity.
Invention content
In view of the defects existing in the prior art, the purpose of the invention is to provide a kind of simple, low cost preparations to bear
The method for carrying magnetic metal sepiolite composite granule or fiber；The composite material magnetic metal good dispersion of preparation, and with magnetic
Property content of metal it is high, and magnetic metal load capacity is controllable, and dielectric loss and the magnetic loss matching that can easily be accommodated composite material are special
Property.
In order to realize above-mentioned technical purpose, the present invention provides a kind of carried magnetic metal sepiolite composite granule or fibers
Preparation method, this method includes the following steps：
1) sepiolite powder or sepiolite fibre are subjected to calcination processing；Alternatively, by sepiolite powder or sepiolite fibre
It is placed in immersion treatment in silane coupler solution；Up to pretreatment sepiolite powder or sepiolite fibre；
2) magnetic metal organic matter is dissolved in organic solvent, obtains magnetic metal organic solution；
3) it after mixing the pretreatment sepiolite powder or sepiolite fibre with the magnetic metal organic solution, puts
In sealing reaction kettle in, carry out pyrolytic reaction to get.
Preferred scheme, the calcination treatment conditions are：Temperature is 105~150 DEG C, and the time is 6~12h, at calcination
Reason, sepiolite powder or fibrous inside fully dried, at the same by sepiolite powder or fibrous inside it is volatile and it is other can
The compound removal of decomposition.
Preferred scheme, the immersion treatment condition are：Temperature is 20~70 DEG C, and the time is 20~60min.
Preferred scheme, during the immersion treatment, sepiolite powder or sepiolite fibre and silane coupler solution
Liquid-solid ratio be (1~10) mL:1g；The silane coupler solution is silane coupled in the range of 0.1~1mmol/L for concentration
Agent ethanol solution, wherein, ethanol solution mass percent concentration is 95%.Sepiolite powder through silane coupling agent surface modification
Or sepiolite fibre, it is remarkably reinforced with the wellability of organic solvent.
More preferably scheme, silane coupling agent is vinyl silanes, amino silane, epoxy radicals silicone hydride, in sulfenyl silane extremely
Few one kind.
Preferred scheme, magnetic metal organic matter is iron, at least one of organic matter of chromium, nickel, Huo Zhetie, chromium, nickel
At least one of organic matter and manganese, vanadium, barium, zinc, aluminium, lanthanum, cerium at least one of organic matter combination.More preferably scheme,
Magnetic metal organic matter is the acetylacetone,2,4-pentanedione salt of magnetic metal, in carbonyl salt, Oxalates or isopropanol salt at least
It is a kind of.
Preferred scheme, organic solvent include dimethylbenzene, ethylene glycol, quinoline, diethylene glycol (DEG), diphenyl ether, tetraethylene glycol diformazan
At least one of ether, triethylene glycol, glycerine.The organic solvent of selection is high boiling organic solvent, and preferably preferably boiling point is high
In the organic solvent of the reaction temperature upper limit.
Preferred scheme, iron in magnetic metal organic matter, chromium, nickel organic matter gross mass degree be not less than
60%.
More preferably scheme, the mass percent concentration of magnetic metal organic matter is in the magnetic metal organic solution
3~60%.
More preferably scheme, the volume that the magnetic metal organic solution loads in reaction kettle are not more than 60%.
More preferably scheme, the pretreatment sepiolite powder or sepiolite fibre and the magnetic metal organic solution
Liquid-solid ratio be (1~10) mL:1g.
Preferred scheme, the pyrolytic reaction control pyrolysis reaction temperature using three sections of temperature-programmed modes：One section of warm area
Be room temperature to 100 DEG C~150 DEG C, two sections of warm areas are 100 DEG C~150 DEG C to 120 DEG C~200 DEG C, three sections of warm areas for 120 DEG C~
200 DEG C to 135 DEG C~220 DEG C.
More preferably scheme, one section of temperature-raising region temperature raising rate are 0.4~0.8 DEG C/min；The heating rate of two sections of warm areas is
0.03~0.20 DEG C/min；The heating rate of three sections of warm areas is 0.05~0.40 DEG C/min.Be conducive to using three sections of temperature programmings
The in-situ preparation and deposition of magnetic metal enhance the compound ability between magnetic metal and sepiolite, respectively with different rates
It carries out, ensures that each elementary reaction is gentle, be conducive to the uniform load of magnetic metal, Dispersed precipitate.
The carried magnetic metal sepiolite composite granule of the present invention or the preparation method of fiber include step in detail below：
(1) pretreatment of sepiolite powder or fiber
First way：By sepiolite powder or fiber in baking oven or sintering furnace after 105~150 DEG C of 6~12h of calcination,
Cooling, levigate, sieving, obtain pretreatment sepiolite powder or sepiolite fibre；
The second way：Compound concentration is the silane coupler solution of 0.1~1mmol/L, is (1~10) by liquid-solid ratio
mL:1g adds sepiolite powder or fiber into silane coupling agent aqueous solution, 20~60min is stirred at 20~70 DEG C, then
Cleaning filtering, 80~200 DEG C of dryings 1~for 24 hours, cooling, levigate, sieving obtain pretreatment sepiolite powder or fiber；
(2) configuration of organic metal solution
With high boiling organic solvent include dimethylbenzene, ethylene glycol, quinoline, diethylene glycol (DEG), diphenyl ether, tetraethyleneglycol dimethyl ether,
Magnetic metal organic compound with organic solvent is sufficiently mixed, obtains magnetism by least one of triethylene glycol, glycerine in proportion
Metallorganic solution system；Wherein mass percent of the metallorganic in metallorganic solution system is 3~60%,
Magnetic metal organic compound ingredient, mass percentage content based at least one of Fe, Co, Ni organic compound are
60~100%, at least one of manganese, vanadium, barium, zinc, aluminium, lanthanum, cerium organic compound can be adulterated, mass percentage content is
0~40%；
(3) pyrolytic reaction and post processing
Pyrolytic reaction device is reaction kettle, reaction kettle assembling atmosphere device and condensing unit, by metallorganic solution body
System is injected into reaction kettle, then adds in pretreatment sepiolite powder or fiber, and liquid-solid ratio is (1~10) mL:1g is fully stirred
It mixes, sepiolite powder or fiber is made to be sufficiently mixed with organic metal solution；Reaction kettle is closed, is passed through protective gas, excludes reaction
Oxygen in kettle；Temperature program is set according to metal-organic pyrolytic reaction, is heated up by multistage, constant temperature program to pyrolysis
The reaction was complete, is cooled to room temperature, and discharging, resulting material is through the cleaning of at least one of absolute ethyl alcohol, acetone or deionized water, mistake
Reaction product, as carried magnetic metal sepiolite fibre composite granule are obtained after filter, dry, levigate, screening.
Compared with the prior art, the advantageous effects that technical scheme of the present invention is brought：
1) technical scheme of the present invention is former using sepiolite powder or sepiolite fibre as the carrier of magnetic metal and skeleton
Material after being pre-processed to it, has the characteristic of excellent adsorption, can fully absorb magnetic metal organic solution, can make heat point
The magnetic in-situ deposition of solution reaction generation is in the surface of sepiolite or hole, so as to make magnetic metal Dispersed precipitate；And it uses
Sepiolite as raw material, it is cheap and easy to get, environmentally friendly.
2) technical scheme of the present invention prepares carried magnetic metal sepiolite composite granule or fiber composite by pyrolysismethod
On the basis of using sepiolite powder or fibers adsorption magnetic metal organic matter, magnetic can be realized by thermal decomposition method for material
Property in-situ metal is loaded on sepiolite powder or fiber surface and channel, is realized the Dispersed precipitate of magnetic metal, is particularly existed
During pyrolysis, the load capacity of magnetic metal can be regulated and controled by adjusting the concentration of magnetic metal organic solution,
It can realize the composite material of high load amount, and be easy to adjust dielectric loss and magnetic loss matching according to load capacity and metal proportioning
Characteristic.
3) the carried magnetic metal sepiolite composite granule or fibrous composite that prepared by technical scheme of the present invention are having
The characteristic of sepiolite low bulk density can be played, and magnetic metal load capacity and metal can be passed through while standby microwave absorbing property
It matches to adjust electromagnetic matching characteristic.
4) preparation method of technical scheme of the present invention carried magnetic metal sepiolite composite granule or fibrous composite
Simply, it is at low cost, be conducive to industrialized production.
Description of the drawings
【Fig. 1】For present invention process flow diagram；
【Fig. 2】Sepiolite composite granule scanning electron microscope (SEM) photograph for load iron prepared by embodiment 1；
【Fig. 3】Sepiolite composite granule electronic energy spectrum for load iron prepared by embodiment 1；
【Fig. 4】The hysteresis loop of the sepiolite composite granule vibrating example of load iron and magnetization song prepared for embodiment 1
Line；
【Fig. 5】The magnetic conductivity real part curve of the sepiolite composite granule vibrating example of load iron prepared for example 1；
【Fig. 6】The magnetic conductivity imaginary part curve of the sepiolite composite granule vibrating example of load iron prepared for example 1.
Specific embodiment
Following embodiment is intended to further illustrate the content of present invention rather than limits the protection model of the claims in the present invention
It encloses.
Embodiment 1
After sepiolite powder in an oven 120 DEG C of calcination 12h, cool down, is levigate, crossing 200 mesh sieve, it is extra large after being pre-processed
Afrodite powder.Using dimethylbenzene as organic solvent, by carbonyl iron, that metal is configured is organic for mass percentage 50% in solution system
Solution system is added in 20L reaction kettles, loading 50%, and pretreated sepiolite powder is added in using liquid-solid ratio as 4.
Reaction kettle is closed, is passed through nitrogen, excludes oxygen in reaction kettle.3 sections of temperature programs are set：(1) 100 are warming up to from room temperature 120min
DEG C, (2) are warming up to 120 DEG C from 100 DEG C of 540min, and (3) are warming up to 135 DEG C from 120 DEG C of 240min.Room temperature then is cooled to, is gone out
Material, resulting material obtain reaction product, as carried magnetic metal through washes of absolute alcohol after filtering, dry, levigate, screening
The sepiolite fibre composite granule of iron.
From attached it can be seen from the figure that：
The sepiolite composite granule surface of load iron covers cotton-shaped crystallization as can be seen from Figure 2；It bears as can be seen from Figure 3
It carries and contains a large amount of iron in the sepiolite composite granule surface crystallization of iron；The sepiolite composite granule of load iron as can be seen from Figure 4
With certain coercivity and saturation magnetization, the coercivity for calculating the sepiolite composite granule of load iron is
127.86Gauss saturation magnetization 15.65emu/g；The sepiolite composite granule of load iron has as can be seen from Figure 5
Preferable storage magnetic energy power, the sepiolite composite granule of load iron is with certain magnetic loss ability as can be seen from Figure 6.
Embodiment 2
After sepiolite powder in an oven 120 DEG C of calcination 12h, cool down, is levigate, crossing 200 mesh sieve, it is extra large after being pre-processed
Afrodite powder.Dimethylbenzene is organic solvent, carbonyl iron and carbonyl cobalt by mass percentage 1:1 mixing, iron pentacarbonyl and eight carbonyls
Organic metal solution system is configured by mass percentage 50% in solution system in the mixture of two cobalts, is added to 20L reactions
In kettle, loading 50% adds in pretreated sepiolite powder using liquid-solid ratio as 4.Reaction kettle is closed, is passed through nitrogen, is arranged
Except oxygen in reaction kettle.3 sections of temperature programs are set：(1) 100 DEG C are warming up to from room temperature 120min, (2) are from 100 DEG C of 540min liters
For temperature to 120 DEG C, (3) are warming up to 135 DEG C from 120 DEG C of 240min.Room temperature then is cooled to, is discharged, resulting material is through absolute ethyl alcohol
Cleaning obtains the sepiolite composite granule of reaction product, as carried magnetic metallic iron/cobalt after filtering, dry, levigate, screening.
Embodiment 3
Compound concentration is 95% ethanol solution of silane coupling agent (KH550) of 0.5mmol/L, even to silane by liquid-solid ratio 3
Sepiolite fibre is added in connection 95% ethanol solution of agent, 60min is stirred at 20 DEG C, then cleaning filtering, 120 DEG C of dry 2h are cold
But, levigate, sieving, sepiolite fibre after being pre-processed.Quinoline is organic solvent, and nickel carbonyl and decacarbonyldimanganese press quality
Percentage 2.6:The mixture of 1 mixing, nickel carbonyl and decacarbonyldimanganese mass percentage 30% in solution system is configured
Organic metal solution system is added in 20L reaction kettles, loading 50%, and pretreated Hai Pao is added in using liquid-solid ratio as 8
Mountain flour body.Reaction kettle is closed, is passed through nitrogen, excludes oxygen in reaction kettle.3 sections of temperature programs are set：(1) from room temperature 240min liters
For temperature to 150 DEG C, (2) are warming up to 200 DEG C from 150 DEG C of 480min, and (3) are warming up to 220 DEG C from 200 DEG C of 240min.Then it is cooled to
Room temperature, discharging, resulting material obtain reaction product after filtering, dry, levigate, screening, as load magnetic through washes of absolute alcohol
The sepiolite fibre composite material of property metallic nickel/manganese.
Claims (9)
1. a kind of preparation method of carried magnetic metal sepiolite composite granule or fiber, it is characterised in that：Include the following steps：
1) sepiolite powder or sepiolite fibre are subjected to calcination processing, alternatively, sepiolite powder or sepiolite fibre are placed in
Immersion treatment in silane coupler solution；Up to pretreatment sepiolite powder or sepiolite fibre；
2) magnetic metal organic matter is dissolved in organic solvent, obtains magnetic metal organic solution；
3) it after mixing the pretreatment sepiolite powder or sepiolite fibre with the magnetic metal organic solution, is placed in close
Seal reaction kettle in, carry out pyrolytic reaction to get；
The pyrolytic reaction controls pyrolysis reaction temperature using three sections of temperature-programmed modes：One section of warm area for room temperature to 100 DEG C~
150 DEG C, two sections of warm areas are 100 DEG C~150 DEG C to 120 DEG C~200 DEG C, and three sections of warm areas are 120 DEG C~200 DEG C to 135 DEG C~220
℃。
2. the preparation method of carried magnetic metal sepiolite composite granule according to claim 1 or fiber, feature exist
In：The calcination treatment conditions are：Temperature is 105~150 DEG C, and the time is 6~12h.
3. the preparation method of carried magnetic metal sepiolite composite granule according to claim 1 or fiber, feature exist
In：The immersion treatment condition is：Temperature is 20~70 DEG C, and the time is 20~60min.
4. the preparation method of the carried magnetic metal sepiolite composite granule or fiber according to claim 1 or 3, feature
It is：During the immersion treatment, sepiolite powder or the liquid-solid ratio of sepiolite fibre and silane coupler solution for (1~
10)mL:1g；The silane coupler solution is silane coupling agent ethanol solution of the concentration in the range of 0.1~1mmol/L,
In, ethanol solution mass percent concentration is 95%；
The silane coupling agent is at least one of vinyl silanes, amino silane, epoxy radicals silicone hydride, sulfenyl silane.
5. the preparation method of carried magnetic metal sepiolite composite granule according to claim 1 or fiber, feature exist
In：The magnetic metal organic matter is iron, at least one of organic matter of chromium, nickel, Huo Zhetie, chromium, nickel organic matter in extremely
Lack a kind of combination of at least one of the organic matter of and manganese, vanadium, barium, zinc, aluminium, lanthanum, cerium；The organic solvent includes diformazan
At least one of benzene, ethylene glycol, quinoline, diethylene glycol (DEG), diphenyl ether, tetraethyleneglycol dimethyl ether, triethylene glycol, glycerine.
6. the preparation method of carried magnetic metal sepiolite composite granule according to claim 5 or fiber, feature exist
In：The organic matter gross mass degree of iron, chromium, nickel is not less than 60% in the magnetic metal organic matter.
7. the preparation method of the carried magnetic metal sepiolite composite granule or fiber according to claim 1,5 or 6, special
Sign is：The mass percent concentration of magnetic metal organic matter is 3~60% in the magnetic metal organic solution.
8. the preparation method of carried magnetic metal sepiolite composite granule according to claim 1 or fiber, feature exist
In：The volume that the magnetic metal organic solution loads in reaction kettle is not more than 60%, the pretreatment sepiolite powder
The liquid-solid ratio of body or sepiolite fibre and the magnetic metal organic solution is (1~10) mL:1g.
9. the preparation method of carried magnetic metal sepiolite composite granule according to claim 1 or fiber, feature exist
In：One section of temperature-raising region temperature raising rate is 0.4~0.8 DEG C/min；The heating rate of two sections of warm areas is 0.03~0.20 DEG C/min；Three sections
The heating rate of warm area is 0.05~0.40 DEG C/min.
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| CN108525668B (en) * | 2018-04-20 | 2021-03-12 | 河北工业大学 | Preparation method of sepiolite nanofiber loaded cobalt-aluminum composite oxide |
| CN108912402A (en) * | 2018-05-28 | 2018-11-30 | 中南大学 | A kind of sepiolite composite absorber and the preparation method and application thereof |
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