CN106433120B - A kind of preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue and its product of preparation - Google Patents
A kind of preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue and its product of preparation Download PDFInfo
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- CN106433120B CN106433120B CN201610682987.9A CN201610682987A CN106433120B CN 106433120 B CN106433120 B CN 106433120B CN 201610682987 A CN201610682987 A CN 201610682987A CN 106433120 B CN106433120 B CN 106433120B
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- 239000000463 material Substances 0.000 title claims abstract description 57
- 230000005855 radiation Effects 0.000 title claims abstract description 49
- 239000003245 coal Substances 0.000 title claims abstract description 41
- 229920000767 polyaniline Polymers 0.000 title claims abstract description 28
- 150000001875 compounds Chemical class 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000002245 particle Substances 0.000 claims abstract description 41
- 229920001940 conductive polymer Polymers 0.000 claims abstract description 28
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000000203 mixture Substances 0.000 claims abstract description 21
- 239000007767 bonding agent Substances 0.000 claims abstract description 15
- 239000002131 composite material Substances 0.000 claims abstract description 11
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 50
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 33
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims description 22
- 238000010521 absorption reaction Methods 0.000 claims description 18
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 239000000047 product Substances 0.000 claims description 15
- 229910002804 graphite Inorganic materials 0.000 claims description 14
- 239000010439 graphite Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 14
- 238000000227 grinding Methods 0.000 claims description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 239000004411 aluminium Substances 0.000 claims description 9
- 229910052782 aluminium Inorganic materials 0.000 claims description 9
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 9
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 8
- 229920001568 phenolic resin Polymers 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000005554 pickling Methods 0.000 claims description 7
- 238000007711 solidification Methods 0.000 claims description 6
- 230000008023 solidification Effects 0.000 claims description 6
- 239000004925 Acrylic resin Substances 0.000 claims description 5
- 229920000178 Acrylic resin Polymers 0.000 claims description 5
- 239000003822 epoxy resin Substances 0.000 claims description 5
- 239000005007 epoxy-phenolic resin Substances 0.000 claims description 5
- 229920000647 polyepoxide Polymers 0.000 claims description 5
- 230000001680 brushing effect Effects 0.000 claims description 4
- 238000005507 spraying Methods 0.000 claims description 4
- 229920000642 polymer Polymers 0.000 claims description 3
- 238000010276 construction Methods 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 150000004968 peroxymonosulfuric acids Chemical class 0.000 claims 1
- 238000000967 suction filtration Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 5
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000002322 conducting polymer Substances 0.000 description 3
- 238000011161 development Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000005011 phenolic resin Substances 0.000 description 3
- 229910000859 α-Fe Inorganic materials 0.000 description 3
- 238000004891 communication Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000007769 metal material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000005984 hydrogenation reaction Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 239000011733 molybdenum Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 229920001197 polyacetylene Polymers 0.000 description 1
- 229920000128 polypyrrole Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000011592 zinc chloride Substances 0.000 description 1
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Macromolecular Compounds Obtained By Forming Nitrogen-Containing Linkages In General (AREA)
- Shielding Devices Or Components To Electric Or Magnetic Fields (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue and its product of preparation, including produce coal liquifaction residue powder, produce conductive polymer polyanilinc particle and by residue powder, conductive polymer polyanilinc particle and bonding agent mix, obtained anti-electromagnetic radiation material is compared with the material of pure polyaniline or one-component, Radar Absorbing Properties of Composites significantly improves, and volume density is low, there is light weight, inhale the advantages of wave frequency section is wide.
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 development of science and technology great-leap-forward development, the electromagnetic technique such as electronic information technology, military equipment technology constantly obtain
Progress is broken through, huge Gospel is brought for human social development, is played in fields such as detection, positioning, communications irreplaceable
Effect.However, with the continuous amplification of electromagnetic wave application field, harm caused by its negative interference also slowly causes people's
Pay attention to.The electromagnetic environment of deterioration can produce electromagnetic interference, influence the systems such as electronics, communication, can also be to the health band of people
To threaten.In military affairs, stealth technology turn into sea, land and sky, day, electromagnetism five in one three-dimensional modernized war in it is most important,
Maximally effective air defense penetration tactics technical measures, it is to improve armament systems existence, prominent anti-and indispensable deep strike ability means.
Therefore, the protection of electromagnetic radiation receives the common concern of the whole society with shielding.Electromagnetism good fortune is reduced in life and penetrates pollution and military affairs
On realize that target is stealthy and will use anti-electromagnetic radiation material, so efficiently the research and development of anti-electromagnetic radiation material into
For the focus of industry research.
From the point of view of element composition and physicochemical property, traditional anti-electromagnetic radiation material mainly has ferrite, magnetic metal, carbon
Several classes such as based material, conducting polymer composite.As anti-electromagnetic radiation material, ferrite has resistivity height, absorbs strong, frequency
Band is wider and the features such as cost is low, but the shortcomings of density is big, hot properties is poor be present.Magnetic metal material (such as Fe, Co, Ni
Metal and its alloy) have the advantages that saturation magnetization high, magnetic conductivity and dielectric constant are big, but exist corrosion resistance it is low,
The shortcomings of density is big.Carbon system anti-electromagnetic radiation material mainly has graphite and carbon black, carbon fiber and CNT etc., has raw material
The advantages that wide material sources, preparation technology are simple, density is low, electrical conductivity is high, but be used alone when exist impedance matching property it is 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, there is small density, structure diversification, can be achieved that infrared and microwave is compatible, Yi Fu
Close the machinery of processing and uniqueness, physics and many advantages, such as chemical characteristic, but the suction wave frequency rate of single conduction high polymer compared with
It is narrow.
Excellent anti-electromagnetic radiation material requirements, which has, absorbs small strong, bandwidth, density, thickness of thin, environmental stability
The features such as good, and traditional anti-electromagnetic radiation material is difficult to meet above-mentioned composite request, and it is single, close to be primarily present absorption band
Degree is big, absorbs the problems such as not strong.Therefore, the high-quality anti-electromagnetic radiation material of preparation " thin, light, wide, strong " becomes grinds at present
The focus studied carefully.And compound anti-electromagnetic radiation material can realize the mutual supplement with each other's advantages of various materials, 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 mainly handled by high-temperature hydrogenation,
Inorganic mineral and additional deliquescence accelerant composition.And catalyst for coal liquefaction can be divided into three classes：(1) oil hydrofinishing class
Catalyst, if cobalt (Co), molybdenum (Mo), nickel (Ni) are active metal catalyst；(2) metal halide catalyst, such as ZnCl2、
SnCl2Deng；(3) Fe-series catalyst, the natural crystal of iron content, oxide, sulfide and the hydroxide of iron etc. are included.So coal
Liquefaction residue is mainly made up of rich carbon component, and is a kind of cheap and easy to get containing components such as a small amount of ferrite, magnetic metal materials
Anti-electromagnetic radiation material source.
The content of the invention
An object of the present invention is to provide a kind of preparation of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue
Method.
The second object of the present invention is to provide a kind of compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue.
The these and other objects of the present invention will further be embodied by following detailed description and description.
The preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention, comprises the following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 400-1000 DEG C, constant temperature 0.5-2h, be then down to room temperature, take
Go out grinding, cross 100-500 mesh sieves, it is 0.1-150um residue powder to obtain particle diameter；
B, at room temperature, aniline is added slowly in hydrochloric acid solution, after stirring, (NH is slowly added dropwise4)2S2O8Solution
The molar ratio of reaction, ammonium persulfate and aniline is 1:1-2, product are dried under vacuum to constant weight through filtering, after pickling at 60 DEG C
Produce conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-10：1-10:1-10 ratio
Add in batch mixer, be uniformly mixed, it is last as needed, spraying, brushing or briquetting process are taken, prepares institute
The anti-electromagnetic radiation material needed.
Further, the preparation method of the compound anti-electromagnetic radiation material of polyaniline of the invention/coal liquifaction residue, including
Following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 500-800 DEG C, constant temperature 0.8-1.5h, be then down to room temperature,
Grinding is taken out, crosses 100-300 mesh sieves, it is 0.5-80um residue powder to obtain particle diameter；
B, at room temperature, 15-30 grams of aniline is added slowly to 200-300 milliliters, in 0.5-1.5mol/L hydrochloric acid solutions, stirred
After mixing uniformly, (NH is slowly added dropwise4)2S2O8Solution reaction stir speed (S.S.) at 0 DEG C is 400-600r/min, reacts 4-12h, mistake
The molar ratio of ammonium sulfate and aniline is 1:1-1.5, product, which through filtering, after pickling at 60 DEG C is dried under vacuum to constant weight and produced, leads
Electric polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-5：2-8:1-5 ratio adds
Enter in batch mixer, be uniformly mixed, finally according to construction needs, take spraying, brushing or briquetting process, prepare
Required anti-electromagnetic radiation material.
It is an option that the preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention,
Comprise the following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 550-650 DEG C, constant temperature 0.8-1.2h, be then down to room temperature,
Grinding is taken out, crosses 150-250 mesh sieves, it is 0.5-74um residue powder to obtain particle diameter；
B, at room temperature, 20-28 grams of aniline is added slowly to 250-350 milliliters, in 0.8-1.2mol/L hydrochloric acid solutions, stirred
After mixing uniformly, (NH is slowly added dropwise4)2S2O8The molar ratio of solution reaction, ammonium persulfate and aniline is 1:1-1.2, product is through taking out
Filter, is then washed 3 times, untill being then washed to filtrate without color, vacuum is done at 60 DEG C repeatedly with 1.0mol/L HCl solutions
It is dry to produce conductive polymer polyanilinc particle to constant weight；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-3：2-6:1-3 ratio adds
Enter in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidification 1.5h is pressed at 150 DEG C
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.
It is preferred that the preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention, including
Following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 600 DEG C, constant temperature 1h, be then down to room temperature, take out grinding, mistake
200 mesh sieves, it is 0.5-74um residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solutions, stirring is equal
After even, (NH is slowly added dropwise4)2S2O8The molar ratio of solution reaction, ammonium persulfate and aniline is 1:1.05, product is through filtering, acid
Constant weight is dried under vacuum at 60 DEG C produce conductive polymer polyanilinc particle after washing；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1：2:1 ratio adds in proportion
Enter in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidification 1.5h is pressed at 150 DEG C
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.
In the preparation method of the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention, described is viscous
It is epoxy resin, phenolic resin or acrylic resin to connect agent.
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue prepared by the method for the present invention, the composite
Two absorption bands are presented in 2-18GHz frequency ranges, respectively in 7.5GHz and 14.5GHz, maximum absorption is -17dB for center
With -10.5dB, less than -10dB with a width of 5GHz, composite volume density is 1.39g/cm3。
Brief 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 compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention, with pure polyaniline or one-component
Material compare, Radar Absorbing Properties of Composites significantly improves, the reachable -10.5dB of composite maximum absorption and -17dB, and pure
Polyaniline and coal liquifaction residue maximum absorption are respectively -4dB and -12dB, and volume density is low, have light weight, inhale wave frequency
The advantages of section is wide, frequency bandwidth of the uptake less than -10dB is 5GHz.
In the present invention, refer in particular to as non-, all amounts, part, than being unit of weight, all raw materials, equipment can be with
Bought from market.
Embodiment
Embodiment 1
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention is prepared as follows, including it is as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 600 DEG C, constant temperature 1h, be then down to room temperature, take out grinding, mistake
200 mesh sieves, it is 0.5-74um residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solutions, stirring is equal
After even, (NH is slowly added dropwise4)2S2O8Solution reaction, stir speed (S.S.) is 400r/min at 5 DEG C, reacts 8h, ammonium persulfate and benzene
The molar ratio of amine is 1:1.05, product (is washed 3 times, then washed through filtering, after pickling repeatedly with 1.0mol/L HCl solutions
Untill filtrate is without color) it is dried in vacuo 12h at 60 DEG C and produces conductive polymer polyanilinc particle to constant weight；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1：2:1 ratio adds in proportion
Enter in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidification 1.5h is pressed at 150 DEG C
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.There are preferable absorption, the reachable -17dB of maximum absorption in 6-18GHz wave bands.
Embodiment 2
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention is prepared as follows, including it is as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 600 DEG C, constant temperature 1h, be then down to room temperature, take out grinding, mistake
200 mesh sieves, it is standby for 0.5-74um residue powder to obtain particle diameter.
B, at 20 ± 5 DEG C, 25 grams of aniline is added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solutions, stirred
Afterwards, (NH is slowly added dropwise4)2S2O8Solution reaction, stir speed (S.S.) is 300r/min at 5 DEG C, reacts 12h, ammonium persulfate and aniline
Molar ratio be 1:1.1, product (is washed 3 times, is then washed to through filtering, after pickling repeatedly with 1.0mol/L HCl solutions
Untill filtrate is without color) it is dried in vacuo 24h at 60 DEG C and produces conductive polymer polyanilinc particle to constant weight；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 3：2:2 ratio adds in proportion
Enter in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidification 1h is pressed into 180mm at 160 DEG C
× 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, are prepared required
Anti-electromagnetic radiation material.There are preferable absorption, the reachable -16.4dB of maximum absorption in 6-18GHz wave bands.
Embodiment 3
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention is prepared as follows, including it is as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 800 DEG C, constant temperature 1h, be then down to room temperature, take out grinding, mistake
200 mesh sieves, it is 0.5-74um residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 20 grams of aniline is added slowly to 200 milliliters, in 1.5mol/L hydrochloric acid solutions, stirred
Afterwards, (NH is slowly added dropwise4)2S2O8Solution, stir speed (S.S.) is 600r/min at 0 DEG C, reacts 6h, and ammonium persulfate and aniline rub
Your ratio is 1:1.5, after product filters, washed repeatedly 3 times with 0.5mol/L HCl solutions, be then washed to filtrate is without color
Only.12h is dried in vacuo at 60 DEG C, produces conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and phenolic resin are pressed into mass parts 2：2:3 ratio is in proportion
Add in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidify 1.5h at 150 DEG C and be pressed into
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.Have two absorption bands in 6-18GHz frequency bands, maximum absorption be respectively -9.4dB and -
16.6dB。
Embodiment 4
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention is prepared as follows, including it is as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 500 DEG C, constant temperature 2h, be then down to room temperature, take out grinding, mistake
200 mesh sieves, it is 0.5-74um (micron) residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 30 grams of aniline is added slowly to 250 milliliters, in 1.5mol/L hydrochloric acid solutions, stirred
Afterwards, (NH is slowly added dropwise4)2S2O8Solution, stir speed (S.S.) is 600r/min at 0 DEG C, reacts 4h, and ammonium persulfate and aniline rub
Your ratio is 1:1.5, after product filters, washed repeatedly 3 times with 0.5mol/L HCl solutions, be then washed to filtrate is without color
Only.12h is dried in vacuo at 60 DEG C, produces conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and phenolic resin are pressed into mass parts 1：1:1 ratio is in proportion
Add in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidify 1.5h at 150 DEG C and be pressed into
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.Have two absorption bands in 6-18GHz frequency bands, maximum absorption be respectively -11.7dB and -
16.8dB。
Embodiment 5
The compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue of the present invention is prepared as follows, including it is as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 500 DEG C, constant temperature 1.5h, be then down to room temperature, take out grinding,
200 mesh sieves are crossed, it is 0.5-74um (micron) residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 26 grams of aniline is added slowly to 260 milliliters, in 1.0mol/L hydrochloric acid solutions, stirred
Afterwards, (NH is slowly added dropwise4)2S2O8Solution, stir speed (S.S.) is 450r/min at 0 DEG C, reacts 4h, and ammonium persulfate and aniline rub
Your ratio is 1:1.5, after product filters, washed repeatedly 3 times with 1.0mol/L HCl solutions, be then washed to filtrate is without color
Only.12h is dried in vacuo at 60 DEG C, produces conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and phenolic resin are pressed into mass parts 3：2:1 ratio is in proportion
Add in batch mixer, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, solidify 1h at 160 DEG C and be pressed into
180mm × 180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare institute
The anti-electromagnetic radiation material needed.Have two absorption bands in 6-18GHz frequency bands, maximum absorption be respectively -9.5dB and -
17.2dB。
Claims (5)
1. the preparation method of the compound anti-electromagnetic radiation material of a kind of polyaniline/coal liquifaction residue, it is characterised in that including as follows
Step：
A, coal liquifaction residue is placed in graphite furnace and is heated to 400-1000 DEG C, constant temperature 0.5-2h, be then down to room temperature, taking-up is ground
Mill, 100-500 mesh sieves are crossed, it is 0.1-150um residue powder to obtain particle diameter；
B, at room temperature, aniline is added slowly in hydrochloric acid solution, after stirring, (NH is slowly added dropwise4)2S2O8Solution reaction,
The molar ratio of ammonium persulfate and aniline is 1:1-2, product, which through filtering, after pickling at 60 DEG C is dried under vacuum to constant weight and produced, leads
Electric polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-10：1-10:1-10 ratio adds
In batch mixer, it is uniformly mixed, it is last as needed, spraying, brushing or briquetting process are taken, is prepared required
Anti-electromagnetic radiation material, described bonding agent are epoxy resin, phenolic resin or acrylic resin.
2. the preparation method of the compound anti-electromagnetic radiation material of polyaniline according to claim 1/coal liquifaction residue, it is special
Sign is to comprise the following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 500-800 DEG C, constant temperature 0.8-1.5h, be then down to room temperature, taken out
Grinding, 100-300 mesh sieves are crossed, it is 0.5-80um residue powder to obtain particle diameter；
B, at room temperature, 15-30 grams of aniline is added slowly to 200-400 milliliters, in 0.5-1.5mol/L hydrochloric acid solutions, stirring is equal
After even, (NH is slowly added dropwise4)2S2O8Solution reaction stir speed (S.S.) at 0 DEG C is 200-600r/min, reacts 4-12h, persulfuric acid
The molar ratio of ammonium and aniline is 1:1-1.5, product are dried under vacuum to constant weight at 60 DEG C after suction filtration, pickling and produce conductive height
Molecule polyaniline particles；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-5：2-8:1-5 ratio adds mixed
In material machine, it is uniformly mixed, finally according to construction needs, takes spraying, brushing or briquetting process, prepare required
Anti-electromagnetic radiation material, described bonding agent is epoxy resin, phenolic resin or acrylic resin.
3. the preparation method of the compound anti-electromagnetic radiation material of polyaniline according to claim 1/coal liquifaction residue, it is special
Sign is to comprise the following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 550-650 DEG C, constant temperature 0.8-1.2h, be then down to room temperature, taken out
Grinding, 150-250 mesh sieves are crossed, it is 0.5-74um residue powder to obtain particle diameter；
B, at room temperature, 20-28 grams of aniline is added slowly to 250-350 milliliters, in 0.8-1.2mol/L hydrochloric acid solutions, stirring is equal
After even, (NH is slowly added dropwise4)2S2O8The molar ratio of solution reaction, ammonium persulfate and aniline is 1:1-1.2, product through filter,
Then washed 3 times with 1.0mol/L HCl solutions, untill being then washed to filtrate without color, be dried under vacuum at 60 DEG C repeatedly
Constant weight produces conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1-3：2-6:1-3 ratio adds mixed
In material machine, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, at 150 DEG C solidification 1.5h be pressed into 180mm ×
180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare required anti-
Electromagenetic wave radiation material, described bonding agent are epoxy resin, phenolic resin or acrylic resin.
4. the preparation method of the compound anti-electromagnetic radiation material of polyaniline according to claim 1/coal liquifaction residue, it is special
Sign is to comprise the following steps：
A, coal liquifaction residue is placed in graphite furnace and is heated to 600 DEG C, constant temperature 1h, be then down to room temperature, take out grinding, cross 200
Mesh sieve, it is 0.5-74um residue powder to obtain particle diameter；
B, at 20 ± 5 DEG C, 25.62 grams of aniline are added slowly to 250 milliliters, in 1.0mol/L hydrochloric acid solutions, after stirring,
(NH is slowly added dropwise4)2S2O8The molar ratio of solution reaction, ammonium persulfate and aniline is 1:1.05, product is through filtering, after pickling
Constant weight is dried under vacuum at 60 DEG C and produces conductive polymer polyanilinc particle；
C, residue powder, conductive polymer polyanilinc particle and bonding agent are pressed into mass parts 1：2:1 ratio is proportionally added into mixed
In material machine, be uniformly mixed to obtain mixture, in pressure be 5Mpa by mixture, at 150 DEG C solidification 1.5h be pressed into 180mm ×
180mm × 2mm thin slice or the thin slice that 180mm × 180mm × 2mm is brushed or be sprayed on aluminium sheet, prepare required anti-
Electromagenetic wave radiation material, described bonding agent are epoxy resin, phenolic resin or acrylic resin.
5. the compound anti-electromagnetic radiation material of polyaniline/coal liquifaction residue according to prepared by claim any one of 1-4, it is special
Sign is that the composite is presented two absorption bands in 2-18GHz frequency ranges, center respectively in 7.5GHz and 14.5GHz,
Maximum absorption is respectively -10.5dB and -17dB, less than -10dB with a width of 5GHz, bulk density 1.39g/cm3。
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| CN111777391B (en) * | 2020-06-11 | 2022-06-14 | 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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