CN115011006B - L-band wave-absorbing oil-resistant rubber sheet and preparation method thereof - Google Patents
L-band wave-absorbing oil-resistant rubber sheet and preparation method thereof Download PDFInfo
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- CN115011006B CN115011006B CN202210646830.6A CN202210646830A CN115011006B CN 115011006 B CN115011006 B CN 115011006B CN 202210646830 A CN202210646830 A CN 202210646830A CN 115011006 B CN115011006 B CN 115011006B
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- resistant rubber
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- 229920001971 elastomer Polymers 0.000 title claims abstract description 50
- 239000005060 rubber Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 33
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 33
- 238000003490 calendering Methods 0.000 claims abstract description 28
- 229920000459 Nitrile rubber Polymers 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229920000049 Carbon (fiber) Polymers 0.000 claims abstract description 20
- 239000004917 carbon fiber Substances 0.000 claims abstract description 20
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 17
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 17
- 239000000126 substance Substances 0.000 claims abstract description 14
- 238000000034 method Methods 0.000 claims abstract description 9
- 230000008569 process Effects 0.000 claims abstract description 8
- 238000007599 discharging Methods 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 34
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 30
- 239000002245 particle Substances 0.000 claims description 23
- 229910052759 nickel Inorganic materials 0.000 claims description 15
- 238000007747 plating Methods 0.000 claims description 15
- XMNIXWIUMCBBBL-UHFFFAOYSA-N 2-(2-phenylpropan-2-ylperoxy)propan-2-ylbenzene Chemical compound C=1C=CC=CC=1C(C)(C)OOC(C)(C)C1=CC=CC=C1 XMNIXWIUMCBBBL-UHFFFAOYSA-N 0.000 claims description 12
- 239000003431 cross linking reagent Substances 0.000 claims description 11
- 239000000314 lubricant Substances 0.000 claims description 11
- 238000007670 refining Methods 0.000 claims description 9
- 235000021355 Stearic acid Nutrition 0.000 claims description 6
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims description 6
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims description 6
- 239000000843 powder Substances 0.000 claims description 6
- 239000008117 stearic acid Substances 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 5
- 235000019400 benzoyl peroxide Nutrition 0.000 claims description 4
- 239000002530 phenolic antioxidant Substances 0.000 claims description 4
- DMWVYCCGCQPJEA-UHFFFAOYSA-N 2,5-bis(tert-butylperoxy)-2,5-dimethylhexane Chemical compound CC(C)(C)OOC(C)(C)CCC(C)(C)OOC(C)(C)C DMWVYCCGCQPJEA-UHFFFAOYSA-N 0.000 claims description 3
- OMPJBNCRMGITSC-UHFFFAOYSA-N Benzoylperoxide Chemical compound C=1C=CC=CC=1C(=O)OOC(=O)C1=CC=CC=C1 OMPJBNCRMGITSC-UHFFFAOYSA-N 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 3
- 150000001412 amines Chemical group 0.000 claims description 3
- -1 polyethylene Polymers 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 238000003825 pressing Methods 0.000 abstract description 17
- 239000000945 filler Substances 0.000 abstract description 12
- 229910052799 carbon Inorganic materials 0.000 abstract description 8
- 239000011159 matrix material Substances 0.000 abstract description 7
- 230000002195 synergetic effect Effects 0.000 abstract description 5
- 230000032683 aging Effects 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 4
- 239000000696 magnetic material Substances 0.000 abstract description 4
- 238000004132 cross linking Methods 0.000 abstract description 3
- 239000003989 dielectric material Substances 0.000 abstract description 3
- 229910052742 iron Inorganic materials 0.000 abstract description 3
- 239000006057 Non-nutritive feed additive Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 31
- 239000000203 mixture Substances 0.000 description 22
- 238000010521 absorption reaction Methods 0.000 description 14
- 238000012360 testing method Methods 0.000 description 10
- 230000008859 change Effects 0.000 description 8
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical compound C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 8
- 238000009472 formulation Methods 0.000 description 8
- 238000004513 sizing Methods 0.000 description 8
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 7
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- 238000004073 vulcanization Methods 0.000 description 7
- 238000005984 hydrogenation reaction Methods 0.000 description 6
- 229920000181 Ethylene propylene rubber Polymers 0.000 description 5
- 239000011358 absorbing material Substances 0.000 description 5
- 229920002379 silicone rubber Polymers 0.000 description 3
- ZNRLMGFXSPUZNR-UHFFFAOYSA-N 2,2,4-trimethyl-1h-quinoline Chemical compound C1=CC=C2C(C)=CC(C)(C)NC2=C1 ZNRLMGFXSPUZNR-UHFFFAOYSA-N 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 2
- 239000005977 Ethylene Substances 0.000 description 2
- OUBMGJOQLXMSNT-UHFFFAOYSA-N N-isopropyl-N'-phenyl-p-phenylenediamine Chemical compound C1=CC(NC(C)C)=CC=C1NC1=CC=CC=C1 OUBMGJOQLXMSNT-UHFFFAOYSA-N 0.000 description 2
- 239000006096 absorbing agent Substances 0.000 description 2
- KAKZBPTYRLMSJV-UHFFFAOYSA-N butadiene group Chemical group C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 2
- HQQADJVZYDDRJT-UHFFFAOYSA-N ethene;prop-1-ene Chemical group C=C.CC=C HQQADJVZYDDRJT-UHFFFAOYSA-N 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 239000004945 silicone rubber Substances 0.000 description 2
- 229920002725 thermoplastic elastomer Polymers 0.000 description 2
- 239000004636 vulcanized rubber Substances 0.000 description 2
- UJAWGGOCYUPCPS-UHFFFAOYSA-N 4-(2-phenylpropan-2-yl)-n-[4-(2-phenylpropan-2-yl)phenyl]aniline Chemical compound C=1C=C(NC=2C=CC(=CC=2)C(C)(C)C=2C=CC=CC=2)C=CC=1C(C)(C)C1=CC=CC=C1 UJAWGGOCYUPCPS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000012762 magnetic filler Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- HYTJADYUOGDVRL-UHFFFAOYSA-N n-phenyl-n-(2-phenylpropan-2-yl)aniline Chemical compound C=1C=CC=CC=1C(C)(C)N(C=1C=CC=CC=1)C1=CC=CC=C1 HYTJADYUOGDVRL-UHFFFAOYSA-N 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000002310 reflectometry Methods 0.000 description 1
- 230000035882 stress Effects 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/74—Mixing; Kneading using other mixers or combinations of mixers, e.g. of dissimilar mixers ; Plant
- B29B7/7476—Systems, i.e. flow charts or diagrams; Plants
- B29B7/7495—Systems, i.e. flow charts or diagrams; Plants for mixing rubber
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/52—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices with rollers or the like, e.g. calenders
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/34—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices
- B29B7/52—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices with rollers or the like, e.g. calenders
- B29B7/56—Mixing; Kneading continuous, with mechanical mixing or kneading devices with movable mixing or kneading devices with rollers or the like, e.g. calenders with co-operating rollers, e.g. with repeated action, i.e. the material leaving a set of rollers being reconducted to the same set or being conducted to a next set
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/30—Mixing; Kneading continuous, with mechanical mixing or kneading devices
- B29B7/58—Component parts, details or accessories; Auxiliary operations
- B29B7/72—Measuring, controlling or regulating
- B29B7/726—Measuring properties of mixture, e.g. temperature or density
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29B—PREPARATION OR PRETREATMENT OF THE MATERIAL TO BE SHAPED; MAKING GRANULES OR PREFORMS; RECOVERY OF PLASTICS OR OTHER CONSTITUENTS OF WASTE MATERIAL CONTAINING PLASTICS
- B29B7/00—Mixing; Kneading
- B29B7/80—Component parts, details or accessories; Auxiliary operations
- B29B7/82—Heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/02—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/22—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor of articles of indefinite length
- B29C43/24—Calendering
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
- B29D7/00—Producing flat articles, e.g. films or sheets
- B29D7/01—Films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C43/00—Compression moulding, i.e. applying external pressure to flow the moulding material; Apparatus therefor
- B29C43/32—Component parts, details or accessories; Auxiliary operations
- B29C43/58—Measuring, controlling or regulating
- B29C2043/5816—Measuring, controlling or regulating temperature
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2309/00—Characterised by the use of homopolymers or copolymers of conjugated diene hydrocarbons
- C08J2309/02—Copolymers with acrylonitrile
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/02—Elements
- C08K3/04—Carbon
- C08K3/041—Carbon nanotubes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
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- C08K7/06—Elements
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
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Abstract
The invention discloses an L-band wave-absorbing oil-resistant rubber sheet and a preparation method thereof. The invention takes hydrogenated nitrile rubber as a matrix, takes flaky carbonyl iron, nickel-plated carbon fiber and nickel-plated carbon nano tube as composite wave-absorbing filler, and simultaneously optimizes a processing aid, a crosslinking system and an aging antioxidant system, thereby obtaining a low-frequency wave-absorbing and oil-resistant rubber product. The invention introduces the hydrogenated nitrile rubber as a rubber matrix, and has the advantages of oil resistance, chemical medium resistance, excellent bonding performance, excellent physical and mechanical properties and better low-frequency wave absorbing performance. According to the invention, the magnetic material flaky carbonyl iron is compounded with the dielectric material nickel-plated carbon fiber and nickel-plated carbon nano tube, and the thickness of the prepared rubber wave absorbing plate is 1.5mm through the synergistic effect of the iron-based wave absorbing filler and the carbon-based wave absorbing filler, so that the maximum wave absorbing rate in an L wave band can reach-20 dB. Compared with the process of directly discharging the sheet by an open mill, the rubber wave absorbing plate after the mold pressing has smooth appearance and better dimensional stability by adopting the preparation process of mixing, calendaring and mold pressing.
Description
Technical Field
The invention belongs to the technical field of functional polymer composite materials, and particularly relates to an L-band (1-2 GHz) wave-absorbing and oil-resistant rubber sheet and a preparation method thereof.
Background
The rubber wave absorbing material is a functional material capable of converting electromagnetic waves into heat energy or other forms of energy through electric loss or magnetic loss so as to absorb most or even all electromagnetic waves. The wave-absorbing material can be used as an effective radar stealth medium and high-sensitivity anti-electromagnetic interference, and has wide application in the aspects of military stealth, wave absorption of microwave devices, electromagnetic interference resistance of electronic communication and the like.
The reflection loss of a wave-absorbing material is directly related to the electromagnetic parameters of the material and the thickness of the wave-absorbing agent. At present, the rubber wave-absorbing material can have better wave-absorbing characteristics in a specific wave band. However, in the low frequency band (L band 1-2 GHz), the conventional iron-based rubber wave absorbing plate is difficult to realize effective wave absorption, and a large thickness is required to be prepared to realize effective wave absorption of the L band.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides an L-band wave-absorbing oil-resistant rubber sheet and a preparation method thereof. The invention takes Hydrogenated Nitrile Butadiene Rubber (HNBR) as a matrix, takes flaky carbonyl iron, nickel-plated carbon fiber and nickel-plated carbon nano tube as composite wave-absorbing filler, and simultaneously optimizes a processing aid, a crosslinking system and an aging antioxidant system, thereby obtaining a low-frequency wave-absorbing and oil-resistant rubber product.
The L-band wave-absorbing oil-resistant rubber sheet comprises the following components in parts by mass: 100 parts by mass of hydrogenated nitrile rubber; 400-650 parts by mass, preferably 450-600 parts by mass, of carbonyl iron; 30-120 parts by mass, preferably 50-100 parts by mass, of nickel-plated carbon fiber; 30-80 parts by mass, preferably 40-60 parts by mass, of nickel-plated carbon nanotubes; 1-5 parts by mass of a crosslinking agent, preferably 2-4 parts by mass; 1.5 to 7 parts by mass of an antioxidant, preferably 2 to 5 parts by mass.
The L-band wave-absorbing oil-resistant rubber sheet also comprises 1-5 parts by mass, preferably 1-4 parts by mass, of lubricant.
The hydrogenated nitrile rubber is a hydrogenated butadiene-acrylonitrile copolymer.
The acrylonitrile content in the hydrogenated nitrile rubber is 17-44%, the hydrogenation degree is 85.0-99.5%, and the Mooney viscosity is 50-90.
The cross-linking agent is one or more of dicumyl peroxide, dibenzoyl peroxide and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane.
The carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 2-8 mu m.
The nickel-plated carbon fiber is a carbon fiber with the surface chemically nickel-plated modified, the nickel plating amount is 60-80%, and the D50 particle size is 60-100 mu m.
The nickel-plated carbon nanotube is a carbon nanotube with a surface chemically nickel-plated modified, the nickel plating amount is 60-80%, and the D50 particle size is 60-100 mu m.
The antioxidant consists of a main antioxidant and an auxiliary antioxidant with the mass ratio of 1-5:1, preferably 1.5-3:1.
The main antioxidant is an amine antioxidant; the auxiliary antioxidant is a phenolic antioxidant.
The amine antioxidant is one or more of 4, 4 '-bis (alpha, alpha-dimethylbenzyl) diphenylamine, N-isopropyl-N' -phenyl p-phenylenediamine and 2, 4-trimethyl-1, 2-dihydroquinoline polymer.
The phenolic antioxidant is a quaternary phenolic antioxidant.
The lubricant is one or more of stearic acid, zinc stearate, polyethylene wax, rhin wax 654, rhin powder 16, rhin powder 25 and Rhin powder 54.
The preparation method of the L-band wave-absorbing oil-resistant rubber sheet comprises the following steps: and weighing the raw materials according to the proportion, and then mixing by an open mill, discharging by a calendaring process, and vulcanizing by a flat vulcanizing machine to obtain the L-band wave-absorbing oil-resistant rubber sheet.
The mixing temperature of the open mill is 50-60 ℃ and the mixing time is 25-35min; standing at room temperature for more than 8 hours after mixing, and reversely refining for 5-8 times by an open mill.
The temperature of the sheet produced by the calendaring process is 60-70 ℃.
The vulcanizing temperature of the press vulcanizer is 150-180 ℃, the time is 10-30min, and the pressure is 7-15MPa.
The acrylonitrile chain segment in the hydrogenated nitrile rubber molecular chain adopted by the invention can provide excellent oil resistance, chemical medium resistance and excellent physical and mechanical properties; the hydrogenated butadiene chain segment can provide good heat resistance, ageing resistance and low temperature performance; residual small amounts of butadiene units containing double bonds can provide the unsaturated bonds necessary for crosslinking. The lamellar carbonyl iron wave absorber has the characteristics of high dielectric constant and high magnetic loss, and can effectively absorb electromagnetic waves at low frequency compared with the traditional magnetic filler spherical carbonyl iron. The nickel-plated carbon fiber has low volume resistivity, is favorable for electromagnetic wave reflection and is unfavorable for electromagnetic wave absorption, and the electromagnetic loss mechanism of the nickel-plated carbon fiber is derived from dielectric loss and conductive loss caused by polarization. The dielectric material nickel-plated carbon fiber and the magnetic material flaky carbonyl iron are compounded for use, so that a synergistic effect can be generated, and wave absorption is effective at low frequency. The nickel-plated carbon nanotube has low volume resistivity, and similar to the action of nickel-plated carbon fiber, consumes electromagnetic waves through dielectric loss and has synergistic action with magnetic material flaky carbonyl iron. The ageing resistance of the composite material can be improved through the matched use of the main antioxidant and the auxiliary antioxidant.
Compared with the prior art, the invention has the beneficial effects that:
(1) According to the invention, hydrogenated nitrile rubber (HNBR) is introduced as a rubber matrix to replace the traditional nonpolar ethylene propylene rubber and silicone rubber base materials, so that the rubber has oil resistance, chemical medium resistance, excellent bonding performance and excellent physical and mechanical properties, and the problems of low mechanical strength, low elongation at break, sheet intolerance to bending and poor sheet bonding capability of the ethylene-propylene material and the silicone rubber base materials are solved; meanwhile, the polar hydrogenated nitrile rubber has better low-frequency wave absorbing performance than the nonpolar ethylene propylene rubber and the silicon rubber.
(2) According to the invention, the magnetic material flaky carbonyl iron is compounded with the dielectric material nickel-plated carbon fiber and nickel-plated carbon nano tube, and the problem of poor low-frequency wave absorption performance of the rubber wave absorption plate in the L wave band is solved through the synergistic effect of the iron-based wave absorption filler and the carbon-based wave absorption filler, so that the maximum wave absorption rate of the prepared rubber wave absorption plate (with the thickness of 1.5 mm) in the L wave band (1-2 GHz) can reach-20 dB.
(3) The problems of stickiness, appearance bulge and air bubbles of the hydrogenated nitrile rubber in the processing process are solved through the preparation process of mixing, calendaring and mould pressing. By introducing the calendaring process, compared with the process that an open mill directly produces the sheet, the molded rubber wave absorbing sheet has smooth appearance and better dimensional stability.
Detailed Description
The present invention is described in detail below with reference to specific embodiments, and it should be noted that the following embodiments are only for further description of the present invention and should not be construed as limiting the scope of the present invention, and some insubstantial modifications and adjustments of the present invention by those skilled in the art from the present disclosure are still within the scope of the present invention.
The raw materials used in examples and comparative examples were conventional commercially available raw materials.
The amounts of the respective raw materials in the examples and comparative examples were in parts by mass.
Reference standard for performance test:
rubber test: GB/T6038-2006 rubber test sizing material compounding, mixing and vulcanizing equipment and operation procedure.
Mechanical properties: measurement of tensile stress Strain Properties of GB/T528-2009 vulcanized rubber or thermoplastic rubber.
Oil resistance: GB/T1690-2010 test method for liquid resistance of vulcanized rubber or thermoplastic rubber.
Wave absorbing performance: a GJB 2038A-2011 radar absorbing material reflectivity testing method.
Table 1 formulations (in parts by mass) of examples 1 to 4 and comparative examples
Example 1
The formulation is shown in Table 1.
The hydrogenated nitrile rubber (HNBR) used had an acrylonitrile content of 17%, a hydrogenation rate of 95% and a Mooney viscosity of 62; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 2 mu m; the D50 particle diameter of the nickel-plated carbon fiber is 60 mu m, and the content of surface chemical nickel plating is 60%; the D50 particle diameter of the nickel-plated carbon nano tube is 80 mu m, and the content of surface chemical nickel plating is 80%; the cross-linking agent is dibenzoyl peroxide (BPO), the lubricant is zinc stearate, the main antioxidant is 4.4' -bis (alpha, alpha-dimethylbenzyl) diphenylamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components according to the mass ratios of example 1 in Table 1 were precisely weighed and mechanically mixed in an open mill for 25 minutes at a roll temperature of 50℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 60 ℃ to obtain a calendered sheet. And transferring the pressed rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 170 ℃, the time is 15min, and the pressure is 10MPa, so that the L-band wave-absorbing oil-resistant rubber sheet is obtained.
Example 2
The formulation is shown in Table 1.
The hydrogenated nitrile rubber (HNBR) used had an acrylonitrile content of 25%, a hydrogenation rate of 95% and a Mooney viscosity of 80; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 6 mu m; the D50 particle diameter of the nickel-plated carbon fiber is 80 mu m, and the content of surface chemical nickel plating is 60%; the D50 particle diameter of the nickel-plated carbon nano tube is 100 mu m, and the content of surface chemical nickel plating is 60%; the cross-linking agent is dicumyl peroxide (DCP), the lubricant is stearic acid, the main antioxidant is 4.4' -bis (alpha-dimethylbenzyl) diphenylamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components according to the mass ratios of example 2 in Table 1 were precisely weighed and mechanically mixed in an open mill for 35 minutes at a roll temperature of 50℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 60 ℃ to obtain a calendered sheet. And transferring the rolled rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 160 ℃, the time is 25min, and the pressure is 15MPa, so that the L-band wave-absorbing oil-resistant rubber sheet is obtained.
Example 3
The formulation is shown in Table 1.
The acrylonitrile content of the hydrogenated nitrile rubber (HNBR) used was 36%, the hydrogenation rate was 96% and the Mooney viscosity was 85; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 8 mu m; the D50 particle diameter of the nickel-plated carbon fiber is 100 mu m, and the content of surface chemical nickel plating is 80%; the D50 particle diameter of the nickel-plated carbon nano tube is 60 mu m, and the content of surface chemical nickel plating is 80%; the cross-linking agent is 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane (bis, 25), the lubricant is Rhine wax 654, the main antioxidant is 2, 4-trimethyl-1, 2-dihydroquinoline polymer, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components according to the mass ratios of example 3 in Table 1 were precisely weighed and mechanically mixed in an open mill for 25 minutes at a roll temperature of 50℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 70 ℃ to obtain a calendered sheet. And transferring the pressed rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 170 ℃, the time is 25min, and the pressure is 10MPa, so that the L-band wave-absorbing oil-resistant rubber sheet is obtained.
Example 4
The formulation is shown in Table 1.
The hydrogenated nitrile rubber (HNBR) used had an acrylonitrile content of 44%, a hydrogenation rate of 96% and a Mooney viscosity of 85; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 6 mu m; the D50 particle diameter of the nickel-plated carbon fiber is 80 mu m, and the content of surface chemical nickel plating is 80%; the D50 particle diameter of the nickel-plated carbon nano tube is 80 mu m, and the content of surface chemical nickel plating is 80%; the cross-linking agent is dicumyl peroxide (DCP), the lubricant is polyethylene wax, the main antioxidant is N-isopropyl-N' -phenyl p-phenylenediamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components according to the mass ratios of example 4 in Table 1 were precisely weighed and mechanically mixed in an open mill for 35 minutes at a roll temperature of 60℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 70 ℃ to obtain a calendered sheet. And transferring the rolled rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 160 ℃, the time is 30min, and the pressure is 13MPa, so that the L-band wave-absorbing oil-resistant rubber sheet is obtained.
Comparative example 1
The formulation is shown in Table 1.
In comparison with example 2, the comparative example has no hydrogenated nitrile rubber and no carbon-based wave-absorbing filler added.
Ethylene propylene rubber, ENB content 5.7%, ethylene content 65% and Mooney viscosity 23 are used; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 6 mu m; the cross-linking agent is dicumyl peroxide (DCP), the lubricant is stearic acid, the main antioxidant is 4.4' -bis (alpha-dimethylbenzyl) diphenylamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components of comparative example 1 in Table 1 were precisely weighed in mass ratios, mechanically mixed in an open mill for 35 minutes at a roll temperature of 60℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 60 ℃ to obtain a calendered sheet. And transferring the pressed rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 160 ℃, the time is 10min, and the pressure is 10MPa, so that the wave-absorbing rubber sheet is obtained.
Comparative example 2
The formulation is shown in Table 1.
In comparison with example 2, comparative example 2 was free of carbon-based wave-absorbing filler.
The hydrogenated nitrile rubber (HNBR) used had an acrylonitrile content of 25%, a hydrogenation rate of 95% and a Mooney viscosity of 80; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 6 mu m; the cross-linking agent is dicumyl peroxide (DCP), the lubricant is stearic acid, the main antioxidant is 4.4' -bis (alpha-dimethylbenzyl) diphenylamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components of comparative example 2 in Table 1 were precisely weighed in mass ratios, mechanically mixed in an open mill for 35 minutes at a roll temperature of 60℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 60 ℃ to obtain a calendered sheet. And transferring the pressed rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 160 ℃, the time is 10min, and the pressure is 10MPa, so that the wave-absorbing rubber sheet is obtained.
Comparative example 3
The formulation is shown in Table 1.
In contrast to example 2, comparative example 3 does not have hydrogenated nitrile rubber.
Ethylene propylene rubber, ENB content 5.7%, ethylene content 65% and Mooney viscosity 23 are used; the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 6 mu m; the D50 particle diameter of the nickel-plated carbon fiber is 80 mu m, and the content of surface chemical nickel plating is 60%; the D50 particle diameter of the nickel-plated carbon nano tube is 100 mu m, and the content of surface chemical nickel plating is 60%; the cross-linking agent is dicumyl peroxide (DCP), the lubricant is stearic acid, the main antioxidant is 4.4' -bis (alpha-dimethylbenzyl) diphenylamine, and the auxiliary antioxidant is tetraphenol antioxidant 1010. The preparation process conditions are as follows: the components of comparative example 3 in Table 1 were precisely weighed in mass ratios, mechanically mixed in an open mill for 35 minutes at a roll temperature of 60℃to obtain a uniformly dispersed mixture. And standing the premixed sizing mixture for 10 hours at room temperature, carrying out reverse refining for 5 times by an open mill, and carrying out preforming by a calendering device at the calendering temperature of 60 ℃ to obtain a calendered sheet. And transferring the pressed rubber sheet to a plate vulcanizing machine for mold pressing vulcanization, wherein the mold pressing temperature is 160 ℃, the time is 10min, and the pressure is 10MPa, so that the wave-absorbing rubber sheet is obtained.
The wave-absorbing rubber sheets prepared in examples 1 to 4 and comparative examples 1 to 3 were subjected to mechanical properties, wave-absorbing properties and oil resistance tests, and the test results are shown in Table 2.
Table 2 results of sheet property tests of examples 1 to 4 and comparative examples
As can be seen from Table 2, comparative example 2 has a tensile strength of 9.2MPa and an elongation at break of 730% which is significantly superior to those of comparative examples 1 and 3 of ethylene-propylene substrates. The tensile strength of the sheets of examples 1-4 is greater than 7MPa, and the elongation at break is greater than 490%, which indicates that the tensile strength and the elongation at break of the hydrogenated nitrile rubber sheets are obviously better than those of the ethylene propylene rubber base material.
In comparison with example 2, the hydrogenated nitrile rubber and the carbon-based wave-absorbing filler were not added in comparative example 1, the carbon-based wave-absorbing filler was not added in comparative example 2, and the hydrogenated nitrile rubber was not added in comparative example 3. From the test result of the wave-absorbing performance, the wave-absorbing center frequency of comparative example 1 is 5.5GHz, the maximum wave-absorbing rate is-11 dB, and the wave-absorbing frequency is in the wave-absorbing frequency band of C wave band (4-8 GHz); comparative example 2 on the basis of comparative example 1, hydrogenated nitrile rubber is introduced as a matrix, the wave absorption center frequency is 3.1GHz, the maximum wave absorption rate is-11 dB, and the wave absorption frequency is in the S-band (2-4 GHz), compared with comparative example 1, after the hydrogenated nitrile rubber is introduced, the wave absorption center frequency moves about 2GHz towards the lower frequency, but does not reach the wave absorption frequency of the L-band (1-2 GHz); comparative example 3 based on comparative example 1, carbon-based wave-absorbing filler was introduced, the wave-absorbing center frequency was 4.1GHz, the maximum wave-absorbing rate was-12 dB, and the wave-absorbing frequency was in the C-band (4 to 8 GHz), and after the carbon-based wave-absorbing filler was introduced, the wave-absorbing center frequency was shifted to a low frequency by about 1GHz, and did not reach the wave-absorbing frequency of the L-band (1 to 2 GHz), as compared with comparative example 1; however, with the simultaneous introduction of the hydrogenated nitrile rubber, the nickel-plated carbon fiber and the nickel-plated carbon nanotube, the center frequency of the wave-absorbing rubber sheet was shifted toward the L-band, the wave-absorbing center frequency of the sheets of examples 1 to 4 was in the L-band (1 to 2 GHz), and the maximum wave-absorbing rate was less than-10 dB, showing a good synergistic wave-absorbing effect.
In comparison with example 2, comparative examples 1 and 3 do not use hydrogenated nitrile rubber as a matrix, and the volume change rate and the mass change rate of the oil resistance test are large. The mass change rate of the comparative example 1 in the No. 1 standard oil reaches 19.8%, the volume change rate reaches 86.3%, the mass change rate reaches 41.6% in the oil resistance test of the No. 3 standard oil, the volume change rate reaches 146.0%, obvious swelling phenomenon is reflected, and the oil resistance test results of the comparative example 3 and the comparative example 1 are similar. After the hydrogenated nitrile rubber matrix is introduced, the mass change rate and the volume change rate of the comparative example 2 and the examples 1 to 4 are less than 2.5% in the 1# standard oil, and less than 15% in the 3# standard oil, and excellent oil resistance is achieved.
Claims (7)
1. The L-band wave-absorbing oil-resistant rubber sheet is characterized by comprising the following components in parts by mass: 100 parts by mass of hydrogenated nitrile rubber; 400-650 parts by mass of carbonyl iron; 30-120 parts by mass of nickel-plated carbon fiber; 30-80 parts by mass of nickel-plated carbon nano tube; 1-5 parts of cross-linking agent; 1.5-7 parts by mass of an antioxidant;
the carbonyl iron is lamellar carbonyl iron, and the D50 particle size is 2-8 mu m;
the preparation method of the L-band wave-absorbing oil-resistant rubber sheet comprises the following steps: weighing the raw materials according to the proportion, and then mixing by an open mill, discharging by a calendaring process, and vulcanizing by a flat vulcanizing machine to obtain the L-band wave-absorbing oil-resistant rubber sheet;
the mixing temperature of the open mill is 50-60 ℃ and the mixing time is 25-35min; standing at room temperature for more than 8 hours after mixing, and reversely refining for 5-8 times by an open mill.
2. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1, wherein the L-band wave-absorbing oil-resistant rubber sheet further comprises 1-5 parts by mass of a lubricant.
3. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1 or 2, wherein the hydrogenated nitrile rubber is a hydrogenated butadiene-acrylonitrile copolymer; the cross-linking agent is one or more of dicumyl peroxide, dibenzoyl peroxide and 2, 5-dimethyl-2, 5-bis (tert-butylperoxy) hexane; the lubricant is one or more of stearic acid, zinc stearate, polyethylene wax, rhin wax 654, rhin powder 16, rhin powder 25 and Rhin powder 54.
4. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1 or 2, wherein the nickel-plated carbon fiber is carbon fiber with surface modified by chemical nickel plating, the nickel plating amount is 60-80%, and the D50 particle size is 60-100 μm; the nickel-plated carbon nanotube is a carbon nanotube with a surface chemically nickel-plated modified, the nickel plating amount is 60-80%, and the D50 particle size is 60-100 mu m.
5. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1 or 2, wherein the antioxidant consists of a main antioxidant and an auxiliary antioxidant in a mass ratio of 1-5:1; the main antioxidant is an amine antioxidant; the auxiliary antioxidant is a phenolic antioxidant.
6. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1, wherein the sheet-forming temperature of the calendaring process is 60-70 ℃.
7. The L-band wave-absorbing oil-resistant rubber sheet according to claim 1, wherein the vulcanizing temperature of the press vulcanizer is 150-180 ℃, the vulcanizing time is 10-30min, and the vulcanizing pressure is 7-15MPa.
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