CN106433120A - Preparation method for composite anti-electromagnetic wave radiation material of polyaniline/coal-to-oil residues and product prepared by same - Google Patents
Preparation method for composite anti-electromagnetic wave radiation material of polyaniline/coal-to-oil residues and product prepared by same Download PDFInfo
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- CN106433120A CN106433120A CN201610682987.9A CN201610682987A CN106433120A CN 106433120 A CN106433120 A CN 106433120A CN 201610682987 A CN201610682987 A CN 201610682987A CN 106433120 A CN106433120 A CN 106433120A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L79/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen or carbon only, not provided for in groups C08L61/00 - C08L77/00
- C08L79/02—Polyamines
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L61/00—Compositions of condensation polymers of aldehydes or ketones; Compositions of derivatives of such polymers
- C08L61/04—Condensation polymers of aldehydes or ketones with phenols only
- C08L61/06—Condensation polymers of aldehydes or ketones with phenols only of aldehydes with phenols
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
Abstract
The invention discloses a preparation method for a composite anti-electromagnetic wave radiation material of polyaniline/coal-to-oil residues and the composite anti-electromagnetic wave radiation material of polyaniline/coal-to-oil residues. The preparation method comprises the following steps: preparing coal-to-oil residue powder, preparing conductive macromolecule polyaniline particles and mixing the residue powder, the conductive macromolecule polyaniline particles and adhesives, thus obtaining the anti-electromagnetic wave radiation material. Compared with the material comprising pure polyaniline or a single component, the composite material is obviously improved in wave absorbing performances, and further has the advantages of low volume density, light mass and wide wave-absorbing frequency bands.
Description
Technical field
The invention belongs to anti-electromagnetic radiation field of material technology, more particularly to a kind of polyaniline/coal liquifaction residue
The preparation method of compound anti-electromagnetic radiation material and its product of preparation.
Technical background：
With the progress of science and technology, the great-leap-forward development such as electronic information technology, military equipment technology, electromagnetic technique is constantly obtained
Progress is broken through, is that human social development brings huge Gospel, play in fields such as detection, positioning, communications irreplaceable
Effect.However, with the continuous amplification of electromagnetic wave application, the harm that its negative interference is produced also slowly causes people's
Pay attention to.The electromagnetic environment of deterioration can produce electromagnetic interference, affect the systems such as electronics, communication, can also be to the healthy band of people
To threaten.In military affairs, stealth technology become most important in the three-dimensional modernized war of sea, land and sky, day, electromagnetism five in one,
Maximally effective air defense penetration tactics technical measures, are to improve armament systems existence, the indispensable means of anti-and deep strike ability of dashing forward.
Therefore, the protection of electromagnetic radiation receives the common concern of the whole society with shielding.Reduce electromagnetism good fortune in life and penetrate pollution and military affairs
On realize that target is stealthy will to use anti-electromagnetic radiation material, so efficiently the research and development of anti-electromagnetic radiation material become
Focus for industry research.
From the point of view of elementary composition and physicochemical property, traditional anti-electromagnetic radiation material mainly has ferrite, magnetic metal, carbon
A few classes such as based material, conducting polymer composite.Used as anti-electromagnetic radiation material, ferrite has resistivity height, absorbs by force, frequently
The features such as band wider and low cost, but there is the shortcomings of density is big, hot properties is poor.Magnetic metal material (such as Fe, Co, Ni etc.
Metal and its alloy) have the advantages that saturation magnetization is high, pcrmeability and dielectric constant are big, but exist corrosion resistance low,
The shortcomings of density is big.Carbon system anti-electromagnetic radiation material mainly has graphite and white carbon black, carbon fiber and CNT etc., with raw material
The advantages of wide material sources, preparation process is simple, density are low, electrical conductivity is high, but be used alone when exist impedance matching property poor,
The shortcomings of absorption band is narrow, absorbent properties are weak.Conducting polymer composite such as polyacetylene, polypyrrole, polyaniline, polythiophene etc. all belong to
In conducting polymer anti-electromagnetic radiation coating, with density is little, structure diversification, can achieve that infrared and microwave is compatible, Yi Fu
Many advantages, such as machinery of conjunction processing and uniqueness, physics and chemical characteristic, but the suction wave frequency of single conduction high polymer is relatively
Narrow.
Excellent anti-electromagnetic radiation material requirements has and absorbs that strong, bandwidth, density is little, thickness of thin, environmental stability
Good the features such as, and traditional anti-electromagnetic radiation material is difficult to meet above-mentioned composite request, is primarily present absorption band single, close
Degree is big, the problems such as absorb strong.Therefore, the high-quality anti-electromagnetic radiation material of preparation " thin, light, wide, strong " becomes and grinds at present
The focus that studies carefully.And the mutual supplement with each other's advantages that anti-electromagnetic radiation material can achieve various materials is combined, reach wanting for " thin, light, wide, strong "
Ask.
Coal liquefaction residue is the material of a kind of high-carbon, high ash and high-sulfur, the heavy organics for mainly being processed by high-temperature hydrogenation,
Inorganic mineral and additional deliquescence accelerant composition.And catalyst for coal liquefaction can be divided three classes：(1) oil hydrofinishing class
Catalyst, such as cobalt (Co), molybdenum (Mo), nickel (Ni) are active metal catalyst；(2) metal halide catalyst, such as ZnCl2、
SnCl2Deng；(3) Fe-series catalyst, including the natural crystal of iron content, the oxide of ferrum, sulfide and hydroxide etc..So coal
Liquefaction residue is mainly made up of rich carbon component, and the component containing a small amount of ferrite, magnetic metal material etc., is a kind of cheap and easy to get
Anti-electromagnetic radiation material source.
Content of the invention
An object of the present invention is to provide the preparation that a kind of polyaniline/coal liquifaction residue is combined anti-electromagnetic radiation material
Method.
The second object of the present invention is to provide a kind of polyaniline/coal liquifaction residue to be combined anti-electromagnetic radiation material.
The these and other objects of the present invention will be embodied further by following detailed description and description.
The polyaniline of the present invention/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, comprises the steps：
A, coal liquifaction residue is placed in graphite furnace 400-1000 DEG C is heated to, constant temperature 0.5-2h, is then down to room temperature, takes
Going out grinding, 100-500 mesh sieve is crossed, particle diameter is obtained for 0.1-150um residue powder；
B, at room temperature, aniline is added slowly in hydrochloric acid solution, after stirring, slowly Deca (NH4)2S2O8Solution
Reaction, Ammonium persulfate. is 1 with the molar ratio of aniline:1-2, product is dried under vacuum to constant weight after sucking filtration, pickling at 60 DEG C
Obtain final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-10：1-10:The ratio of 1-10
Add in batch mixer, be uniformly mixed, finally according to needs, take spraying, brush or briquetting process, prepare institute
The anti-electromagnetic radiation material for needing.
Further, the polyaniline of the present invention/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, including
Following steps：
A, coal liquifaction residue is placed in graphite furnace 500-800 DEG C is heated to, constant temperature 0.8-1.5h, then room temperature is down to,
Grinding being taken out, 100-300 mesh sieve is crossed, particle diameter is obtained for 0.5-80um residue powder；
B, at room temperature, 15-30 gram of aniline is added slowly to 200-300 milliliter, in 0.5-1.5mol/L hydrochloric acid solution, is stirred
Mix uniform after, slowly Deca (NH4)2S2O8Solution reaction stir speed (S.S.) at 0 DEG C is 400-600r/min, reacts 4-12h, mistake
Ammonium sulfate is 1 with the molar ratio of aniline:1-1.5, product is dried under vacuum to constant weight at 60 DEG C after sucking filtration, pickling and obtains final product lead
Electric polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-5：2-8:The ratio of 1-5 adds
Enter in batch mixer, be uniformly mixed, need finally according to construction, take spraying, brush or briquetting process, prepare
Required anti-electromagnetic radiation material.
It is an option that the polyaniline of the present invention/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material,
Comprise the steps：
A, coal liquifaction residue is placed in graphite furnace 550-650 DEG C is heated to, constant temperature 0.8-1.2h, then room temperature is down to,
Grinding being taken out, 150-250 mesh sieve is crossed, particle diameter is obtained for 0.5-74um residue powder；
B, at room temperature, 20-28 gram of aniline is added slowly to 250-350 milliliter, in 0.8-1.2mol/L hydrochloric acid solution, is stirred
Mix uniform after, slowly Deca (NH4)2S2O8Solution reaction, Ammonium persulfate. is 1 with the molar ratio of aniline:1-1.2, product is through taking out
Filter, then with 1.0mol/L HCl solution cyclic washing 3 times, till being then washed to filtrate no color, at 60 DEG C, vacuum is done
Dry conductive polymer polyanilinc granule is obtained final product to constant weight；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-3：2-6:The ratio of 1-3 adds
Enter in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 150 DEG C, solidification 1.5h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.
It is preferred that the polyaniline of the present invention/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, including
Following steps：
A, coal liquifaction residue is placed in graphite furnace 600 DEG C are heated to, constant temperature 1h, is then down to room temperature, takes out grinding, mistake
200 mesh sieves, obtain particle diameter for 0.5-74um residue powder；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solution, stirring is equal
After even, slowly Deca (NH4)2S2O8Solution reaction, Ammonium persulfate. is 1 with the molar ratio of aniline:1.05, product is through sucking filtration, acid
Constant weight is dried under vacuum to after washing at 60 DEG C obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1：2:1 ratio adds in proportion
Enter in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 150 DEG C, solidification 1.5h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.
It is combined in the preparation method of anti-electromagnetic radiation material in the polyaniline/coal liquifaction residue of the present invention, described is viscous
It is epoxy resin, phenolic resin or acrylic resin to connect agent.
Polyaniline prepared by the method for the present invention/coal liquifaction residue is combined anti-electromagnetic radiation material, the composite
Assume two absorption bands in 2-18GHz frequency range, center is respectively in 7.5GHz and 14.5GHz, and maximum absorption is -17dB
With -10.5dB, a width of 5GHz is carried less than -10dB, composite volume density is 1.39g/cm3.
Description of the drawings
Fig. 1 is Radar Absorbing Properties of Composites curve of the present invention.
Fig. 2 is composite and one-component absorbing property curve.
The polyaniline of the present invention/coal liquifaction residue is combined anti-electromagnetic radiation material, with pure polyaniline or one-component
Material compare, Radar Absorbing Properties of Composites is significantly improved, and composite maximum absorption is up to -10.5dB and -17dB, and pure
Polyaniline and coal liquifaction residue maximum absorption are respectively -4dB and -12dB, and body density is low, with light weight, inhale wave frequency
The wide advantage of section, bandwidth of the absorbtivity less than -10dB is 5GHz.
In the present invention, refer in particular to as non-, all of amount, part, ratio are unit of weight, and all of raw material, equipment are all permissible
Buy from market.
Specific embodiment
Embodiment 1
Polyaniline/coal liquifaction the residue for being prepared as follows the present invention is combined anti-electromagnetic radiation material, including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 600 DEG C are heated to, constant temperature 1h, is then down to room temperature, takes out grinding, mistake
200 mesh sieves, obtain particle diameter for 0.5-74um residue powder；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solution, stirring is equal
After even, slowly Deca (NH4)2S2O8Solution reaction, at 5 DEG C, stir speed (S.S.) is 400r/min, reacts 8h, Ammonium persulfate. and benzene
The molar ratio of amine is 1:1.05, product (with 1.0mol/L HCl solution cyclic washing 3 times, is then washed after sucking filtration, pickling
To filtrate no color) at 60 DEG C, vacuum drying 12h obtains final product conductive polymer polyanilinc granule to constant weight；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1：2:1 ratio adds in proportion
Enter in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 150 DEG C, solidification 1.5h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.There is preferable absorption in 6-18GHz wave band, maximum absorption is up to -17dB.
Embodiment 2
Polyaniline/coal liquifaction the residue for being prepared as follows the present invention is combined anti-electromagnetic radiation material, including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 600 DEG C are heated to, constant temperature 1h, is then down to room temperature, takes out grinding, mistake
200 mesh sieves, obtain particle diameter standby for 0.5-74um residue powder.
B, at 20 ± 5 DEG C, 25 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solution, are stirred
Afterwards, slowly Deca (NH4)2S2O8Solution reaction, at 5 DEG C, stir speed (S.S.) is 300r/min, reacts 12h, Ammonium persulfate. and aniline
Molar ratio be 1:1.1, product (with 1.0mol/L HCl solution cyclic washing 3 times, is then washed to after sucking filtration, pickling
Till filtrate no color) at 60 DEG C, vacuum drying 24h obtains final product conductive polymer polyanilinc granule to constant weight；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 3：2:2 ratio adds in proportion
Enter in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 160 DEG C, solidification 1h is pressed into 180mm
The thin slice of × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, needed for preparing
Anti-electromagnetic radiation material.There is preferable absorption in 6-18GHz wave band, maximum absorption is up to -16.4dB.
Embodiment 3
Polyaniline/coal liquifaction the residue for being prepared as follows the present invention is combined anti-electromagnetic radiation material, including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 800 DEG C are heated to, constant temperature 1h, is then down to room temperature, takes out grinding, mistake
200 mesh sieves, obtain particle diameter for 0.5-74um residue powder；
B, at 20 ± 5 DEG C, 20 grams of aniline are added slowly to 200 milliliters, in 1.5mol/L hydrochloric acid solution, are stirred
Afterwards, slowly Deca (NH4)2S2O8Solution, at 0 DEG C, stir speed (S.S.) is 600r/min, reacts 6h, and Ammonium persulfate. is rubbed with aniline
Your ratio is 1:1.5, after product sucking filtration, with 0.5mol/L HCl solution cyclic washing 3 times, being then washed to filtrate no color is
Only.12h is vacuum dried at 60 DEG C, obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and phenolic resin press mass parts 2：2:3 ratio is in proportion
Add in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 150 DEG C, solidification 1.5h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.Have two absorption bands in 6-18GHz frequency band, maximum absorption be respectively -9.4dB and -
16.6dB.
Embodiment 4
Polyaniline/coal liquifaction the residue for being prepared as follows the present invention is combined anti-electromagnetic radiation material, including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 500 DEG C are heated to, constant temperature 2h, is then down to room temperature, takes out grinding, mistake
200 mesh sieves, obtain particle diameter for 0.5-74um (micron) residue powder；
B, at 20 ± 5 DEG C, 30 grams of aniline are added slowly to 250 milliliters, in 1.5mol/L hydrochloric acid solution, are stirred
Afterwards, slowly Deca (NH4)2S2O8Solution, at 0 DEG C, stir speed (S.S.) is 600r/min, reacts 4h, and Ammonium persulfate. is rubbed with aniline
Your ratio is 1:1.5, after product sucking filtration, with 0.5mol/L HCl solution cyclic washing 3 times, being then washed to filtrate no color is
Only.12h is vacuum dried at 60 DEG C, obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and phenolic resin press mass parts 1：1:1 ratio is in proportion
Add in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 150 DEG C, solidification 1.5h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.Have two absorption bands in 6-18GHz frequency band, maximum absorption be respectively -11.7dB and -
16.8dB.
Embodiment 5
Polyaniline/coal liquifaction the residue for being prepared as follows the present invention is combined anti-electromagnetic radiation material, including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 500 DEG C are heated to, constant temperature 1.5h, room temperature is then down to, grinding is taken out,
200 mesh sieves are crossed, and particle diameter are obtained for 0.5-74um (micron) residue powder；
B, at 20 ± 5 DEG C, 26 grams of aniline are added slowly to 260 milliliters, in 1.0mol/L hydrochloric acid solution, are stirred
Afterwards, slowly Deca (NH4)2S2O8Solution, at 0 DEG C, stir speed (S.S.) is 450r/min, reacts 4h, and Ammonium persulfate. is rubbed with aniline
Your ratio is 1:1.5, after product sucking filtration, with 1.0mol/L HCl solution cyclic washing 3 times, being then washed to filtrate no color is
Only.12h is vacuum dried at 60 DEG C, obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and phenolic resin press mass parts 3：2:1 ratio is in proportion
Add in batch mixer, mixture is uniformly mixed to obtain, mixture is 5Mpa in pressure, at 160 DEG C, solidification 1h is pressed into
The thin slice of 180mm × 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, prepare institute
The anti-electromagnetic radiation material for needing.Have two absorption bands in 6-18GHz frequency band, maximum absorption be respectively -9.5dB and -
17.2dB.
Claims (6)
1. a kind of polyaniline/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, it is characterised in that including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace 400-1000 DEG C is heated to, constant temperature 0.5-2h, room temperature is then down to, taking-up is ground
Mill, crosses 100-500 mesh sieve, obtains particle diameter for 0.1-150um residue powder；
B, at room temperature, aniline is added slowly in hydrochloric acid solution, after stirring, slowly Deca (NH4)2S2O8Solution reaction,
Ammonium persulfate. is 1 with the molar ratio of aniline:1-2, product is dried under vacuum to constant weight at 60 DEG C after sucking filtration, pickling and obtains final product lead
Electric polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-10：1-10:The ratio of 1-10 is added
In batch mixer, it is uniformly mixed, finally according to needs, takes spraying, brushes or briquetting process, needed for preparing
Anti-electromagnetic radiation material.
2. polyaniline according to claim 1/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, and which is special
Levy and be to comprise the steps：
A, coal liquifaction residue is placed in graphite furnace 500-800 DEG C is heated to, constant temperature 0.8-1.5h, is then down to room temperature, takes out
Grinding, crosses 100-300 mesh sieve, obtains particle diameter for 0.5-80um residue powder；
B, at room temperature, 15-30 gram of aniline is added slowly to 200-400 milliliter, and in 0.5-1.5mol/L hydrochloric acid solution, stirring is equal
After even, slowly Deca (NH4)2S2O8Solution reaction stir speed (S.S.) at 0 DEG C is 200-600r/min, reacts 4-12h, persulfuric acid
Ammonium is 1 with the molar ratio of aniline:1-1.5, product is dried under vacuum to constant weight after sucking filtration, pickling at 60 DEG C and obtains final product conductive height
Molecule polyaniline particles；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-5：2-8:The ratio of 1-5 adds mixed
In material machine, it is uniformly mixed, needs finally according to construction, takes spraying, brushes or briquetting process, needed for preparing
Anti-electromagnetic radiation material.
3. polyaniline according to claim 1/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, and which is special
Levy and be to comprise the steps：
A, coal liquifaction residue is placed in graphite furnace 550-650 DEG C is heated to, constant temperature 0.8-1.2h, is then down to room temperature, takes out
Grinding, crosses 150-250 mesh sieve, obtains particle diameter for 0.5-74um residue powder；
B, at room temperature, 20-28 gram of aniline is added slowly to 250-350 milliliter, and in 0.8-1.2mol/L hydrochloric acid solution, stirring is equal
After even, slowly Deca (NH4)2S2O8Solution reaction, Ammonium persulfate. is 1 with the molar ratio of aniline:1-1.2, product through sucking filtration,
Then with 1.0mol/L HCl solution cyclic washing 3 times, till being then washed to filtrate no color, it is dried under vacuum at 60 DEG C
Constant weight obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1-3：2-6:The ratio of 1-3 adds mixed
In material machine, be uniformly mixed to obtain mixture, mixture be 5Mpa in pressure, at 150 DEG C solidification 1.5h be pressed into 180mm ×
The thin slice of 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, anti-needed for preparing
Electromagenetic wave radiation material.
4. polyaniline according to claim 1/coal liquifaction residue is combined the preparation method of anti-electromagnetic radiation material, and which is special
Levy and be to comprise the steps：
A, coal liquifaction residue is placed in graphite furnace 600 DEG C are heated to, constant temperature 1h, is then down to room temperature, takes out grinding, cross 200
Mesh sieve, obtains particle diameter for 0.5-74um residue powder；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solution, after stirring,
Slowly Deca (NH4)2S2O8Solution reaction, Ammonium persulfate. is 1 with the molar ratio of aniline:1.05, product is after sucking filtration, pickling
Constant weight is dried under vacuum at 60 DEG C obtains final product conductive polymer polyanilinc granule；
C, by residue powder, conductive polymer polyanilinc granule and bonding agent press mass parts 1：2:1 ratio is proportionally added into mixing
In material machine, be uniformly mixed to obtain mixture, mixture be 5Mpa in pressure, at 150 DEG C solidification 1.5h be pressed into 180mm ×
The thin slice of 180mm × 2mm or brush or be sprayed into the thin slice of 180mm × 180mm × 2mm on aluminium sheet, anti-needed for preparing
Electromagenetic wave radiation material.
5. the polyaniline according to one of claim 1-4/coal liquifaction residue is combined the preparation side of anti-electromagnetic radiation material
Method, it is characterised in that described bonding agent is epoxy resin, phenolic resin or acrylic resin.
6. the polyaniline according to prepared by any one of claim 1-5/coal liquifaction residue is combined anti-electromagnetic radiation material, and which is special
Levy and be that the composite assumes two absorption bands in 2-18GHz frequency range, center respectively in 7.5GHz and 14.5GHz,
Maximum absorption is respectively -10.5dB and -17dB, carries a width of 5GHz less than -10dB, and bulk density is 1.39g/cm3.
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| CN201610682987.9A CN106433120B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue and its product of preparation |
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| CN201610682987.9A CN106433120B (en) | 2016-08-17 | 2016-08-17 | A kind of preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue and its product of preparation |
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Cited By (2)
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| CN111777391A (en) * | 2020-06-11 | 2020-10-16 | 中建西部建设建材科学研究院有限公司 | Whole-body moisture-proof and water-resistant gypsum wallboard with electromagnetic shielding function and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109550932A (en) * | 2017-09-27 | 2019-04-02 | 北京碳极极电科技有限公司 | A kind of composite wave-suction material preparation method based on coal oil residue |
| CN111777391A (en) * | 2020-06-11 | 2020-10-16 | 中建西部建设建材科学研究院有限公司 | Whole-body moisture-proof and water-resistant gypsum wallboard with electromagnetic shielding function and preparation method thereof |
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| CN106433120B (en) | 2018-02-02 |
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