CN116144087A - High-temperature-resistant nitrile rubber noise reduction material - Google Patents
High-temperature-resistant nitrile rubber noise reduction material Download PDFInfo
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- CN116144087A CN116144087A CN202310137669.4A CN202310137669A CN116144087A CN 116144087 A CN116144087 A CN 116144087A CN 202310137669 A CN202310137669 A CN 202310137669A CN 116144087 A CN116144087 A CN 116144087A
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- rubber
- nitrile rubber
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- temperature
- resistant
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- 229920000459 Nitrile rubber Polymers 0.000 title claims abstract description 79
- 239000000463 material Substances 0.000 title claims abstract description 52
- 230000009467 reduction Effects 0.000 title claims abstract description 40
- 229920001971 elastomer Polymers 0.000 claims abstract description 66
- 238000002156 mixing Methods 0.000 claims abstract description 49
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 34
- 229920002379 silicone rubber Polymers 0.000 claims abstract description 32
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000003712 anti-aging effect Effects 0.000 claims abstract description 19
- 238000004132 cross linking Methods 0.000 claims abstract description 14
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 11
- 235000021355 Stearic acid Nutrition 0.000 claims abstract description 11
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims abstract description 11
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 claims abstract description 11
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000008117 stearic acid Substances 0.000 claims abstract description 11
- 229910052717 sulfur Inorganic materials 0.000 claims abstract description 11
- 239000011593 sulfur Substances 0.000 claims abstract description 11
- 239000011787 zinc oxide Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 48
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 47
- 229910044991 metal oxide Inorganic materials 0.000 claims description 46
- 150000004706 metal oxides Chemical class 0.000 claims description 46
- 239000004005 microsphere Substances 0.000 claims description 46
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 45
- 229920001021 polysulfide Polymers 0.000 claims description 43
- 239000005077 polysulfide Substances 0.000 claims description 43
- 150000008117 polysulfides Polymers 0.000 claims description 43
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 238000001816 cooling Methods 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 28
- 239000000047 product Substances 0.000 claims description 26
- 238000005406 washing Methods 0.000 claims description 25
- 238000002360 preparation method Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 22
- 229910021641 deionized water Inorganic materials 0.000 claims description 22
- WGTYBPLFGIVFAS-UHFFFAOYSA-M tetramethylammonium hydroxide Chemical compound [OH-].C[N+](C)(C)C WGTYBPLFGIVFAS-UHFFFAOYSA-M 0.000 claims description 20
- 238000001914 filtration Methods 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- 239000003431 cross linking reagent Substances 0.000 claims description 15
- 238000010438 heat treatment Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 14
- 239000012752 auxiliary agent Substances 0.000 claims description 14
- DOIRQSBPFJWKBE-UHFFFAOYSA-N dibutyl phthalate Chemical compound CCCCOC(=O)C1=CC=CC=C1C(=O)OCCCC DOIRQSBPFJWKBE-UHFFFAOYSA-N 0.000 claims description 14
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 14
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 14
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 14
- 239000004945 silicone rubber Substances 0.000 claims description 13
- 235000019441 ethanol Nutrition 0.000 claims description 12
- 229920002545 silicone oil Polymers 0.000 claims description 12
- AZQWKYJCGOJGHM-UHFFFAOYSA-N 1,4-benzoquinone Chemical compound O=C1C=CC(=O)C=C1 AZQWKYJCGOJGHM-UHFFFAOYSA-N 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 10
- 150000002751 molybdenum Chemical class 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 10
- 238000010992 reflux Methods 0.000 claims description 10
- 239000012266 salt solution Substances 0.000 claims description 10
- 238000001354 calcination Methods 0.000 claims description 9
- 240000002853 Nelumbo nucifera Species 0.000 claims description 8
- 235000006508 Nelumbo nucifera Nutrition 0.000 claims description 8
- 235000006510 Nelumbo pentapetala Nutrition 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- -1 bicyclic amidine Chemical class 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 238000001291 vacuum drying Methods 0.000 claims description 8
- 229920002554 vinyl polymer Polymers 0.000 claims description 8
- OWRCNXZUPFZXOS-UHFFFAOYSA-N 1,3-diphenylguanidine Chemical compound C=1C=CC=CC=1NC(=N)NC1=CC=CC=C1 OWRCNXZUPFZXOS-UHFFFAOYSA-N 0.000 claims description 7
- QYLFHLNFIHBCPR-UHFFFAOYSA-N 1-ethynylcyclohexan-1-ol Chemical compound C#CC1(O)CCCCC1 QYLFHLNFIHBCPR-UHFFFAOYSA-N 0.000 claims description 7
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 7
- 230000032683 aging Effects 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 229910017604 nitric acid Inorganic materials 0.000 claims description 7
- 229910052697 platinum Inorganic materials 0.000 claims description 7
- YLLIGHVCTUPGEH-UHFFFAOYSA-M potassium;ethanol;hydroxide Chemical compound [OH-].[K+].CCO YLLIGHVCTUPGEH-UHFFFAOYSA-M 0.000 claims description 7
- 239000004408 titanium dioxide Substances 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 7
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 6
- QABCGOSYZHCPGN-UHFFFAOYSA-N chloro(dimethyl)silicon Chemical compound C[Si](C)Cl QABCGOSYZHCPGN-UHFFFAOYSA-N 0.000 claims description 6
- 238000004073 vulcanization Methods 0.000 claims description 6
- YFKBXYGUSOXJGS-UHFFFAOYSA-N 1,3-Diphenyl-2-propanone Chemical compound C=1C=CC=CC=1CC(=O)CC1=CC=CC=C1 YFKBXYGUSOXJGS-UHFFFAOYSA-N 0.000 claims description 5
- JTPNRXUCIXHOKM-UHFFFAOYSA-N 1-chloronaphthalene Chemical compound C1=CC=C2C(Cl)=CC=CC2=C1 JTPNRXUCIXHOKM-UHFFFAOYSA-N 0.000 claims description 5
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 5
- 238000003483 aging Methods 0.000 claims description 5
- 239000012378 ammonium molybdate tetrahydrate Substances 0.000 claims description 5
- FIXLYHHVMHXSCP-UHFFFAOYSA-H azane;dihydroxy(dioxo)molybdenum;trioxomolybdenum;tetrahydrate Chemical compound N.N.N.N.N.N.O.O.O.O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O=[Mo](=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O.O[Mo](O)(=O)=O FIXLYHHVMHXSCP-UHFFFAOYSA-H 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 230000007935 neutral effect Effects 0.000 claims description 5
- 229910052757 nitrogen Inorganic materials 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 239000003921 oil Substances 0.000 claims description 5
- 239000012074 organic phase Substances 0.000 claims description 5
- 238000005204 segregation Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 239000002904 solvent Substances 0.000 claims description 5
- 239000006228 supernatant Substances 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 4
- MQIUGAXCHLFZKX-UHFFFAOYSA-N Di-n-octyl phthalate Natural products CCCCCCCCOC(=O)C1=CC=CC=C1C(=O)OCCCCCCCC MQIUGAXCHLFZKX-UHFFFAOYSA-N 0.000 claims description 3
- BJQHLKABXJIVAM-UHFFFAOYSA-N bis(2-ethylhexyl) phthalate Chemical group CCCCC(CC)COC(=O)C1=CC=CC=C1C(=O)OCC(CC)CCCC BJQHLKABXJIVAM-UHFFFAOYSA-N 0.000 claims description 3
- AFZSMODLJJCVPP-UHFFFAOYSA-N dibenzothiazol-2-yl disulfide Chemical compound C1=CC=C2SC(SSC=3SC4=CC=CC=C4N=3)=NC2=C1 AFZSMODLJJCVPP-UHFFFAOYSA-N 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 3
- 238000000643 oven drying Methods 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims description 2
- KUAZQDVKQLNFPE-UHFFFAOYSA-N thiram Chemical compound CN(C)C(=S)SSC(=S)N(C)C KUAZQDVKQLNFPE-UHFFFAOYSA-N 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 10
- 230000007774 longterm Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 16
- 238000010521 absorption reaction Methods 0.000 description 3
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 3
- 230000009471 action Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000005336 cracking Methods 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000009210 therapy by ultrasound Methods 0.000 description 2
- 206010063493 Premature ageing Diseases 0.000 description 1
- 208000032038 Premature aging Diseases 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 230000000269 nucleophilic effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 230000008646 thermal stress Effects 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
- C08L9/00—Compositions of homopolymers or copolymers of conjugated diene hydrocarbons
- C08L9/02—Copolymers with acrylonitrile
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2262—Oxides; Hydroxides of metals of manganese
-
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2296—Oxides; Hydroxides of metals of zinc
-
- 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
-
- 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
- Y02T—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO TRANSPORTATION
- Y02T10/00—Road transport of goods or passengers
- Y02T10/80—Technologies aiming to reduce greenhouse gasses emissions common to all road transportation technologies
- Y02T10/86—Optimisation of rolling resistance, e.g. weight reduction
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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to the technical field of rubber materials, in particular to a high-temperature-resistant nitrile rubber noise reduction material which is prepared from the following raw materials in parts by weight: 50-70 parts of modified nitrile rubber, 20-30 parts of high temperature resistant silicon rubber, 2-4 parts of zinc oxide, 1-3 parts of stearic acid, 3-6 parts of a silane coupling agent, 15-20 parts of a compatibilizer, 2-6 parts of an anti-aging agent, 2-3 parts of an accelerator and 1-3 parts of sulfur. According to the invention, the modified nitrile rubber is used as a main raw material, and the high-density flexible rubber material is formed by adding the high-temperature-resistant silicon rubber and carrying out blending, and the crosslinking of the molecular chains forms a crosslinked network structure, so that the thermal stability of the rubber material is obviously improved, and the modified nitrile rubber has good emission and refraction effects on sound waves, so that the attenuation of sound energy is obvious, and the modified nitrile rubber can meet the long-term use under a high-temperature environment and has good noise reduction effect.
Description
Technical Field
The invention relates to the technical field of rubber materials, in particular to a high-temperature-resistant nitrile rubber noise reduction material.
Background
The working load of sound sources such as transformers, reactors, engines and vibrating equipment in the places such as a transformer room, a mechanical equipment power cabin and the like is kept at a very high level throughout the year, so that the noise emission of the surrounding environment exceeds the standard, and the life quality of surrounding residents and the normal production of surrounding enterprises are seriously affected. The conventional noise reduction materials generally consider the noise reduction effect and do not pay special attention to high-temperature resistant places; in areas and places where heat is generated or released due to mechanical operation, materials generally have better high temperature resistance, so that higher requirements are also put on the high temperature resistance of the materials.
Most of the existing noise reduction materials on the market are non-vulcanized materials, the heat resistance is generally poor, the problems of premature aging, surface cracking, stickiness and the like are easily caused, the phenomenon of surface chipping or swelling is caused after long-time use, and the requirements of places with higher temperature on the noise reduction materials are often not met. For example, the invention patent with publication number of CN111995803A discloses a novel high-strength rubber sound insulation pad with new composite material and a preparation method thereof, and the low-temperature flexibility of the novel high-strength rubber sound insulation pad with new composite material is better by adding the polydimethyl vinyl siloxane, polyurethane emulsion and methyl vinyl ether-maleic anhydride copolymer to match in a specific proportion, so that the product keeps better sound absorption effect in a low-temperature environment; although the rubber material has a good sound absorption effect and a certain noise reduction performance, the rubber material is a non-vulcanized material, so that the rubber material has poor heat resistance, and the problems of early aging, surface cracking and the like are easy to occur in a high-temperature environment, thereby seriously affecting the service performance and restricting the popularization and application in the special field.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the high-temperature-resistant nitrile rubber noise reduction material, which takes modified nitrile rubber as a main raw material, and is formed into a high-density flexible rubber material by adding high-temperature-resistant silicon rubber and carrying out blending, and the cross-linking of molecular chains forms a cross-linked network structure, so that the thermal stability of the rubber material is obviously improved, and the high-temperature-resistant nitrile rubber noise reduction material has good emission and refraction effects on sound waves, so that the attenuation of sound energy is obvious, and the high-temperature-resistant nitrile rubber noise reduction material can meet the long-term use under a high-temperature environment and has good noise reduction effect.
In order to achieve the above purpose, the present invention provides the following technical solutions:
the high-temperature-resistant nitrile rubber noise reduction material is prepared from the following raw materials in parts by weight: 50-70 parts of modified nitrile rubber, 20-30 parts of high temperature resistant silicon rubber, 2-4 parts of zinc oxide, 1-3 parts of stearic acid, 3-6 parts of a silane coupling agent, 15-20 parts of a compatibilizer, 2-6 parts of an anti-aging agent, 2-3 parts of an accelerator and 1-3 parts of sulfur.
As a further preferable scheme of the invention, the compatibilizer is dioctyl phthalate and triphenyl phosphate according to the mass ratio of 1: (1-2) a mixture;
the anti-aging agent is at least one of an anti-aging agent RD and an anti-aging agent 4010 NA;
the accelerator is at least one of accelerator MBTS and accelerator TMTD.
As a further preferable scheme of the invention, the preparation method of the modified nitrile rubber comprises the following steps:
1) Respectively adding bisphenol A epoxy resin accounting for 1-3% of the mass of the liquid polysulfide rubber and bicyclic amidine accounting for 0.01-0.05% of the mass of the liquid polysulfide rubber, stirring for 40-50 hours at the constant temperature of 80-85 ℃ to obtain pretreated polysulfide rubber, and then uniformly mixing the pretreated polysulfide rubber, the modified metal oxide porous hollow microspheres and titanium dioxide on a mixer to obtain modified polysulfide rubber;
2) Evenly mixing manganese dioxide, dibutyl phthalate and an accelerator D to obtain a vulcanizing agent, evenly mixing modified polysulfide rubber, nitrile rubber and the vulcanizing agent, and vulcanizing and cross-linking to form after mixing by an internal mixer to obtain the modified nitrile rubber.
As a further preferable scheme of the invention, the mass ratio of the pretreated polysulfide rubber to the modified metal oxide porous hollow microsphere to the titanium dioxide is (100-150): (30-40): (10-18);
the mass ratio of the manganese dioxide to the dibutyl phthalate to the accelerator D is (30-50): (30-50): (1-2);
the mass ratio (3-6) of the modified polysulfide rubber, the nitrile rubber and the vulcanizing agent is as follows: (15-25): 1.
as a further preferable scheme of the invention, the preparation method of the high-temperature-resistant silicone rubber comprises the following steps:
1) Adding a tetramethyl ammonium hydroxide aqueous solution into a container, slowly dripping tetraethoxysilane into the container, stirring overnight at room temperature, then reacting for 10-15h at 60-64 ℃, distilling under reduced pressure to remove the solvent, cooling in a refrigerator to crystallize, filtering, repeatedly washing with acetone, and drying for later use;
2) Adding 5-10g of the product into a container filled with 30-40mL of dimethyl chlorosilane, 50-70mL of n-hexane and 100-160mLN, N-dimethylformamide, stirring and cooling to 0 ℃ at room temperature, adding 80-120mL of distilled water and stirring to room temperature, washing the separated organic phase to be neutral by deionized water, carrying out reduced pressure distillation, placing into a refrigerator for low-temperature crystallization, washing the product by methanol, filtering and drying to obtain a cross-linking agent;
3) Mixing 10-12g of quinone, 12-14g of dibenzyl ketone and 120-160mL of absolute ethyl alcohol, heating to 80-84 ℃, slowly dripping 8-10mL of potassium hydroxide ethanol solution, reacting for 15-20min under the protection of nitrogen, cooling to 0 ℃, carrying out suction filtration on the product, repeatedly washing by ethanol, drying, mixing with 30-40g of hydroxyl silicone oil and 3-6g of alpha-chloronaphthalene, placing in an oil bath pot, heating, stirring and refluxing for 8-12h under 220-230 ℃ and nitrogen atmosphere, standing, cooling and layering, adding methanol into an upper product for segregation and separation, and carrying out reduced pressure distillation at 150-160 ℃ to obtain a heat-resistant auxiliary agent;
4) Adding a cross-linking agent, ethynyl cyclohexanol, modified metal oxide porous hollow microspheres and a heat-resistant auxiliary agent into vinyl silicone oil, uniformly mixing, adding a platinum catalyst, stirring for 30-50min, placing into a vacuum drying oven, removing bubbles in the system at room temperature, pouring into a mould, and curing at room temperature to obtain the high-temperature-resistant silicone rubber.
As a further preferable embodiment of the present invention, the volume ratio of the aqueous tetramethylammonium hydroxide solution to tetraethoxysilane is (45-55): (6-10);
the concentration of the tetramethyl ammonium hydroxide aqueous solution is 10-13wt%;
the concentration of the potassium hydroxide ethanol solution is 15-18wt%;
the mass ratio of the vinyl silicone oil, the cross-linking agent, the ethynyl cyclohexanol, the modified metal oxide porous hollow microspheres, the heat-resistant auxiliary agent and the platinum catalyst is (40-60): (1-2): (0.005-0.008): (2-5): (3-6): (0.1-0.2).
As a further preferable scheme of the invention, the preparation method of the modified metal oxide porous hollow microsphere comprises the following steps:
1) Adding lotus pollen into absolute ethyl alcohol, dispersing uniformly, filtering, repeatedly cleaning with deionized water, drying at 60-70deg.C for 12-15 hr, calcining at 300-320 deg.C in air for 6-10 hr, cooling to room temperature, soaking in sufficient nitric acid solution for 30-50min, taking out, and oven drying to obtain pretreated pollen;
2) Dissolving 3.7-4.2g of ammonium molybdate tetrahydrate in 40-60mL of deionized water to obtain a molybdenum salt solution, dissolving 6.6-7.2g of citric acid in 30-50mL of ethylene glycol to obtain a citric acid solution, adding the molybdenum salt solution into the citric acid solution, fully stirring in a water bath at 80-85 ℃, refluxing in the water bath at 100-103 ℃ for 12-15h to obtain a sol, dispersing pretreated pollen in the sol, stirring for 3-5h, ageing, filtering, washing and drying the product, and calcining in air at 600-630 ℃ for 6-10h to obtain the metal oxide porous hollow microspheres;
3) Adding hexamethyldisilazane, deionized water and ethanol into a container, stirring in a water bath at 30-35 ℃ for 30-50min, adding metal oxide porous hollow microspheres, uniformly mixing, heating the water bath to 85-88 ℃ and reacting for 2-3h, standing for 1-2h after the reaction is finished, pouring out supernatant, standing for 5-10h at room temperature, and drying to obtain the modified metal oxide porous hollow microspheres.
As a further preferable scheme of the invention, the dosage proportion of the lotus pollen and the absolute ethyl alcohol is (10-15) g: (80-120) mL;
the concentration of the nitric acid solution is 6-8mol/L;
the mass ratio of the pretreated pollen to the sol is (0.3-0.5): (10-15).
As a further preferable scheme of the invention, the dosage proportion of the hexamethyldisilazane, the deionized water, the ethanol and the metal oxide porous hollow microsphere is (3-6) g: (1-2) mL: (50-80) mL: (60-80) g.
As a further preferable scheme of the invention, the preparation method of the high-temperature-resistant nitrile rubber noise reduction material comprises the following steps:
according to the weight portion, pouring the modified nitrile rubber, the high temperature resistant silicon rubber, the zinc oxide, the stearic acid, the silane coupling agent, the anti-aging agent and the dilatant into an internal mixer for mixing to form a mixed rubber, cooling to room temperature, pouring into an open mill, adding sulfur and an accelerant after the temperature of the mixed rubber is reduced to below 100 ℃, uniformly tamping, and performing vulcanization crosslinking molding to obtain the required high temperature resistant nitrile rubber noise reduction material.
Compared with the prior art, the invention has the beneficial effects that:
according to the invention, the liquid polysulfide rubber is chemically modified through bisphenol A epoxy resin, a benzene ring high-temperature resistant chain segment is introduced into a molecular structure of the liquid polysulfide rubber, and the modified metal oxide porous hollow microsphere is introduced, so that the modified metal oxide porous hollow microsphere can be uniformly dispersed in the liquid polysulfide rubber and form interaction of an interface layer with molecular chains of the liquid polysulfide rubber, the interface bonding strength of the liquid polysulfide rubber and the interface layer is improved, so that the toughness of the polysulfide rubber can be effectively improved, under the action of high temperature, the generated thermal stress can cause the polysulfide rubber to generate more deformation, so that more heat can be absorbed, the formation of microcracks can be inhibited, the polysulfide rubber has high heat resistance, the modified polysulfide rubber and the nitrile rubber are vulcanized and crosslinked, so that the high-heat resistant molecular chains are introduced into the molecular chains of the nitrile rubber, so that the nitrile rubber has good high-temperature resistance, and the molecular chains of the nitrile rubber are crosslinked and wound with each other to form a three-dimensional network structure, so that the flexibility of the chain segment of the nitrile rubber is further improved, and the thermal stability of the nitrile rubber is further improved; the modified metal oxide porous hollow microsphere takes lotus pollen as a biological template, the pollen has a hierarchical porous structure, the pollen is internally provided with a complex multi-layer pore structure, part of sound waves can be reflected on the surface of the modified metal oxide porous hollow microsphere, and part of sound waves can be scattered in a hollow cavity, so that the propagation distance is increased to attenuate sound energy, and under the action of the sound waves, air in the cavity of the modified metal oxide porous hollow microsphere can be repeatedly compressed, so that heat exchange is generated between the air and the cavity wall, and the sound energy is converted into heat energy and consumed, so that the nitrile rubber has good noise reduction performance.
In the invention, tetraethoxysilane is used as a monomer, silanol molecules are obtained through hydrolysis reaction under the catalysis of tetramethyl ammonium hydroxide, silicon anions are generated by the silanol molecules under the alkaline condition, nucleophilic attack is carried out on the silanol molecules to form silicon oxygen silicon bonds, and alkylation substitution reaction is carried out on the silicon oxygen anions and dimethyl chlorosilane, so that a cross-linking agent is synthesized, the synthesized cross-linking agent and a heat-resistant auxiliary agent are introduced into a cross-linked network structure of silicon rubber, and a three-dimensional caged inorganic skeleton formed by Si-O-Si in the cross-linking agent has good thermal stability, and 8 active points of each molecule can participate in cross-linking, so that a high-density three-dimensional network structure is formed through hydrosilylation reaction, and the decomposition temperature of the silicon rubber is remarkably improved, so that the silicon rubber has high thermal stability; the three-dimensional network structure is formed to wrap the added modified metal oxide porous hollow microspheres, and a multi-layer network structure is formed on the surface of the modified metal oxide porous hollow microspheres, so that the modified metal oxide porous hollow microspheres can form multi-layer interfaces in a silicon rubber matrix, the reflection and refraction of sound waves can be increased to attenuate sound energy, and the silicon rubber has good noise reduction performance.
According to the invention, the modified nitrile rubber is used as a main raw material, and the high-density flexible rubber material is formed by adding the high-temperature-resistant silicon rubber and carrying out blending, and the crosslinking of the molecular chains forms a crosslinked network structure, so that the thermal stability of the rubber material is obviously improved, and the modified nitrile rubber has good emission and refraction effects on sound waves, so that the attenuation of sound energy is obvious, and the modified nitrile rubber can meet the long-term use under a high-temperature environment and has good noise reduction effect.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In the embodiment of the invention, the compatibilizer is dioctyl phthalate and triphenyl phosphate according to the mass ratio of 1:1.5 a mixture of; the anti-aging agent is an anti-aging agent RD; the accelerator is accelerator MBTS.
Example 1
The high-temperature-resistant nitrile rubber noise reduction material is prepared from the following raw materials in parts by weight: 50 parts of modified nitrile rubber, 20 parts of high temperature resistant silicon rubber, 2 parts of zinc oxide, 1 part of stearic acid, 3 parts of silane coupling agent, 15 parts of expanding agent, 2 parts of anti-aging agent, 2 parts of accelerator and 1 part of sulfur;
the preparation method of the high-temperature-resistant nitrile rubber noise reduction material comprises the following steps:
according to the weight portion, pouring the modified nitrile rubber, the high temperature resistant silicon rubber, the zinc oxide, the stearic acid, the silane coupling agent, the anti-aging agent and the dilatant into an internal mixer for mixing to form a mixed rubber, cooling to room temperature, pouring into an open mill, adding sulfur and an accelerant after the temperature of the mixed rubber is reduced to below 100 ℃, uniformly tamping, and performing vulcanization crosslinking molding to obtain the required high temperature resistant nitrile rubber noise reduction material.
The preparation method of the modified nitrile rubber comprises the following steps:
1) Respectively adding bisphenol A epoxy resin accounting for 1% of the mass of the liquid polysulfide rubber and 0.01% of bicyclic amidine into the liquid polysulfide rubber, stirring for 40 hours at the constant temperature of 80 ℃ at 130r/min to obtain pretreated polysulfide rubber, and uniformly mixing 100g of pretreated polysulfide rubber, 30g of modified metal oxide porous hollow microspheres and 10g of titanium dioxide on a mixer to obtain modified polysulfide rubber;
2) Uniformly mixing 30g of manganese dioxide, 30g of dibutyl phthalate and 1g of accelerator D to obtain a vulcanizing agent, and mixing modified polysulfide rubber, nitrile rubber and the vulcanizing agent according to a mass ratio of 3:15:1, mixing uniformly, and vulcanizing and crosslinking to form after mixing by an internal mixer to obtain the modified nitrile rubber.
The preparation method of the high-temperature-resistant silicone rubber comprises the following steps:
1) Adding 45mL of tetramethyl ammonium hydroxide aqueous solution with the concentration of 10wt% into a container, slowly dripping 6mL of tetraethoxysilane into the container, stirring overnight at room temperature, reacting at 60 ℃ for 10h, distilling under reduced pressure to remove the solvent, cooling in a refrigerator to crystallize, filtering, repeatedly washing with acetone, and drying for later use;
2) Adding 5g of the product into a container filled with 30mL of dimethyl chlorosilane, 50mL of n-hexane and 100mLN, N-dimethylformamide, stirring and cooling to 0 ℃ at room temperature, then adding 80mL of distilled water and stirring to room temperature, washing the separated organic phase to be neutral by deionized water, carrying out reduced pressure distillation, placing into a refrigerator for low-temperature crystallization, washing the product by methanol, filtering and drying to obtain a cross-linking agent;
3) Mixing 10g of quinone, 12g of dibenzyl ketone and 120mL of absolute ethyl alcohol, heating to 80 ℃, slowly dropwise adding 8mL of potassium hydroxide ethanol solution with the concentration of 15wt%, reacting for 15min under the protection of nitrogen, cooling to 0 ℃, carrying out suction filtration on the product, repeatedly washing by ethanol, drying, mixing with 30g of hydroxy silicone oil and 3g of alpha-chloronaphthalene, placing in an oil bath pot, heating, stirring and refluxing for 8h at 220 ℃ under the nitrogen atmosphere, standing, cooling and layering, adding methanol into an upper product for segregation and separation, and carrying out reduced pressure distillation at 150 ℃ to obtain a heat-resistant auxiliary agent;
4) Adding 1g of cross-linking agent, 0.005g of ethynyl cyclohexanol, 2g of modified metal oxide porous hollow microspheres and 3g of heat-resistant auxiliary agent into 40g of vinyl silicone oil, uniformly mixing, adding 0.1g of platinum catalyst, stirring for 30min at 100r/min, placing into a vacuum drying oven, removing bubbles in the system at room temperature, pouring into a mold, and curing at room temperature to obtain the high-temperature-resistant silicone rubber.
The preparation method of the modified metal oxide porous hollow microsphere comprises the following steps:
1) 10g of lotus pollen is put into a container, 80mL of absolute ethyl alcohol is added and treated by 200W ultrasonic for 1h, the solution is repeatedly washed by deionized water after suction filtration, dried for 12h at 60 ℃, placed into air and calcined for 6h at 300 ℃, cooled to room temperature, immersed into a sufficient amount of nitric acid solution with the concentration of 6mol/L for 30min, taken out and dried, and pretreated pollen is obtained;
2) Dissolving 3.7g of ammonium molybdate tetrahydrate in 40mL of deionized water to obtain a molybdenum salt solution, dissolving 6.6g of citric acid in 30mL of ethylene glycol to obtain a citric acid solution, adding the molybdenum salt solution into the citric acid solution, fully stirring at 80 ℃ in a water bath, refluxing for 12 hours in a water bath at 100 ℃ to obtain a sol, dispersing 0.3g of pretreated pollen in 10g of the sol, stirring for 3 hours at 800r/min, filtering, washing and drying the product after ageing, and calcining for 6 hours at 600 ℃ in air to obtain the metal oxide porous hollow microspheres;
3) Adding 3g of hexamethyldisilazane, 1mL of deionized water and 50mL of ethanol into a container, stirring for 30min in a water bath kettle at 30 ℃, adding 60g of metal oxide porous hollow microspheres, uniformly mixing, heating the water bath temperature to 85 ℃ and reacting for 2h, standing for 1h after the reaction is finished, pouring out supernatant, standing for 5h at room temperature, and vacuum-drying for 4h at 120 ℃ to obtain the modified metal oxide porous hollow microspheres.
Example 2
The high-temperature-resistant nitrile rubber noise reduction material is prepared from the following raw materials in parts by weight: 60 parts of modified nitrile rubber, 25 parts of high temperature resistant silicon rubber, 3 parts of zinc oxide, 2 parts of stearic acid, 5 parts of silane coupling agent, 18 parts of expanding agent, 5 parts of anti-aging agent, 2.5 parts of accelerator and 2 parts of sulfur;
the preparation method of the high-temperature-resistant nitrile rubber noise reduction material comprises the following steps:
according to the weight portion, pouring the modified nitrile rubber, the high temperature resistant silicon rubber, the zinc oxide, the stearic acid, the silane coupling agent, the anti-aging agent and the dilatant into an internal mixer for mixing to form a mixed rubber, cooling to room temperature, pouring into an open mill, adding sulfur and an accelerant after the temperature of the mixed rubber is reduced to below 100 ℃, uniformly tamping, and performing vulcanization crosslinking molding to obtain the required high temperature resistant nitrile rubber noise reduction material.
The preparation method of the modified nitrile rubber comprises the following steps:
1) Respectively adding bisphenol A epoxy resin accounting for 2% of the mass of the liquid polysulfide rubber and 0.03% of bicyclic amidine into the liquid polysulfide rubber, stirring for 45 hours at a constant temperature of 82 ℃ at 180r/min to obtain pretreated polysulfide rubber, and uniformly mixing 130g of pretreated polysulfide rubber, 35g of modified metal oxide porous hollow microspheres and 14g of titanium dioxide on a mixer to obtain modified polysulfide rubber;
2) Uniformly mixing 40g of manganese dioxide, 40g of dibutyl phthalate and 1.5g of accelerator D to obtain a vulcanizing agent, and mixing modified polysulfide rubber, nitrile rubber and the vulcanizing agent according to a mass ratio of 5:20:1, mixing uniformly, and vulcanizing and crosslinking to form after mixing by an internal mixer to obtain the modified nitrile rubber.
The preparation method of the high-temperature-resistant silicone rubber comprises the following steps:
1) Adding 50mL of tetramethyl ammonium hydroxide aqueous solution with the concentration of 12wt% into a container, slowly dripping 8mL of tetraethoxysilane into the container, stirring overnight at room temperature, reacting at 62 ℃ for 13h, distilling under reduced pressure to remove the solvent, cooling in a refrigerator to crystallize, filtering, repeatedly washing with acetone, and drying for later use;
2) Adding 8g of the product into a container filled with 35mL of dimethyl chlorosilane, 60mL of n-hexane and 135mLN, N-dimethylformamide, stirring and cooling to 0 ℃ at room temperature, then adding 100mL of distilled water and stirring to room temperature, washing the separated organic phase to be neutral by deionized water, carrying out reduced pressure distillation, placing into a refrigerator for low-temperature crystallization, washing the product by methanol, filtering and drying to obtain a cross-linking agent;
3) Mixing 11g of quinone, 13g of dibenzyl ketone and 150mL of absolute ethyl alcohol, heating to 82 ℃, slowly dropwise adding 9mL of potassium hydroxide ethanol solution with the concentration of 16wt%, reacting for 18min under the protection of nitrogen, cooling to 0 ℃, carrying out suction filtration on the product, repeatedly washing by ethanol, drying, mixing with 35g of hydroxy silicone oil and 5g of alpha-chloronaphthalene, placing in an oil bath pot, heating, stirring and refluxing for 10h at 225 ℃ and under the nitrogen atmosphere, standing, cooling and layering, adding methanol into an upper product for segregation and separation, and carrying out reduced pressure distillation at 155 ℃ to obtain a heat-resistant auxiliary agent;
4) Adding 1.5g of cross-linking agent, 0.007g of ethynyl cyclohexanol, 3g of modified metal oxide porous hollow microspheres and 5g of heat-resistant auxiliary agent into 50g of vinyl silicone oil, uniformly mixing, adding 0.15g of platinum catalyst, stirring for 40min at 150r/min, placing into a vacuum drying oven, removing bubbles in the system at room temperature, pouring into a mold, and curing at room temperature to obtain the high-temperature-resistant silicone rubber.
The preparation method of the modified metal oxide porous hollow microsphere comprises the following steps:
1) Placing 13g of lotus pollen into a container, adding 100mL of absolute ethyl alcohol, performing ultrasonic treatment for 1.5h at 260W, repeatedly cleaning with deionized water after suction filtration, drying at 65 ℃ for 13h, calcining at 310 ℃ in air for 8h, cooling to room temperature, immersing into a sufficient amount of nitric acid solution with the concentration of 7mol/L for 40min, taking out, and drying to obtain pretreated pollen;
2) Dissolving 4g of ammonium molybdate tetrahydrate in 50mL of deionized water to obtain a molybdenum salt solution, dissolving 7g of citric acid in 40mL of ethylene glycol to obtain a citric acid solution, adding the molybdenum salt solution into the citric acid solution, fully stirring at 82 ℃ in a water bath, refluxing for 13h in a 101 ℃ water bath to obtain a sol, dispersing 0.4g of pretreated pollen in 13g of the sol, stirring for 4h at 900r/min, filtering, washing and drying the product after ageing, and calcining in air at 620 ℃ for 8h to obtain the metal oxide porous hollow microspheres;
3) Adding 5g of hexamethyldisilazane, 1.5mL of deionized water and 70mL of ethanol into a container, stirring for 40min in a water bath kettle at 32 ℃, adding 70g of metal oxide porous hollow microspheres, uniformly mixing, heating the water bath temperature to 86 ℃ and reacting for 2.5h, standing for 1.5h after the reaction is finished, pouring out supernatant, standing for 7h at room temperature, and vacuum drying for 5h at 125 ℃ to obtain the modified metal oxide porous hollow microspheres.
Example 3
The high-temperature-resistant nitrile rubber noise reduction material is prepared from the following raw materials in parts by weight: 70 parts of modified nitrile rubber, 30 parts of high temperature resistant silicon rubber, 4 parts of zinc oxide, 3 parts of stearic acid, 6 parts of silane coupling agent, 20 parts of expanding agent, 6 parts of anti-aging agent, 3 parts of accelerator and 3 parts of sulfur;
the preparation method of the high-temperature-resistant nitrile rubber noise reduction material comprises the following steps:
according to the weight portion, pouring the modified nitrile rubber, the high temperature resistant silicon rubber, the zinc oxide, the stearic acid, the silane coupling agent, the anti-aging agent and the dilatant into an internal mixer for mixing to form a mixed rubber, cooling to room temperature, pouring into an open mill, adding sulfur and an accelerant after the temperature of the mixed rubber is reduced to below 100 ℃, uniformly tamping, and performing vulcanization crosslinking molding to obtain the required high temperature resistant nitrile rubber noise reduction material.
The preparation method of the modified nitrile rubber comprises the following steps:
1) Respectively adding bisphenol A epoxy resin accounting for 3 percent of the mass of the liquid polysulfide rubber and 0.05 percent of bicyclic amidine into the liquid polysulfide rubber, stirring for 50 hours at a constant temperature of 85 ℃ at 200r/min to obtain pretreated polysulfide rubber, and uniformly mixing 150g of pretreated polysulfide rubber, 40g of modified metal oxide porous hollow microspheres and 18g of titanium dioxide on a mixer to obtain modified polysulfide rubber;
2) 50g of manganese dioxide, 50g of dibutyl phthalate and 2g of accelerator D are uniformly mixed to obtain a vulcanizing agent, and the modified polysulfide rubber, the nitrile rubber and the vulcanizing agent are mixed according to a mass ratio of 6:25:1, mixing uniformly, and vulcanizing and crosslinking to form after mixing by an internal mixer to obtain the modified nitrile rubber.
The preparation method of the high-temperature-resistant silicone rubber comprises the following steps:
1) Adding 55mL of tetramethyl ammonium hydroxide aqueous solution with the concentration of 13wt% into a container, slowly dripping 10mL of tetraethoxysilane into the container, stirring overnight at room temperature, reacting at 64 ℃ for 15h, distilling under reduced pressure to remove the solvent, cooling in a refrigerator to crystallize, filtering, repeatedly washing with acetone, and drying for later use;
2) Adding 10g of the product into a container filled with 40mL of dimethyl chlorosilane, 70mL of n-hexane and 160mLN, N-dimethylformamide, stirring and cooling to 0 ℃ at room temperature, then adding 120mL of distilled water and stirring to room temperature, washing the separated organic phase to be neutral by deionized water, carrying out reduced pressure distillation, placing into a refrigerator for low-temperature crystallization, washing the product by methanol, filtering and drying to obtain a cross-linking agent;
3) Mixing 12g of quinone, 14g of dibenzyl ketone and 160mL of absolute ethyl alcohol, heating to 84 ℃, slowly dropwise adding 10mL of 18wt% potassium hydroxide ethanol solution, reacting for 20min under the protection of nitrogen, cooling to 0 ℃, carrying out suction filtration on the product, repeatedly washing by ethanol, drying, mixing with 40g of hydroxy silicone oil and 6g of alpha-chloronaphthalene, placing in an oil bath pot, heating, stirring and refluxing for 12h at 230 ℃ and under nitrogen atmosphere, standing, cooling and layering, adding methanol into an upper product for segregation and separation, and carrying out reduced pressure distillation at 160 ℃ to obtain a heat-resistant auxiliary agent;
4) Adding 2g of cross-linking agent, 0.008g of ethynyl cyclohexanol, 5g of modified metal oxide porous hollow microspheres and 6g of heat-resistant auxiliary agent into 60g of vinyl silicone oil, uniformly mixing, adding 0.2g of platinum catalyst, stirring for 50min at 160r/min, placing into a vacuum drying oven, removing bubbles in the system at room temperature, pouring into a mold, and curing at room temperature to obtain the high-temperature-resistant silicone rubber.
The preparation method of the modified metal oxide porous hollow microsphere comprises the following steps:
1) Placing 15g of lotus pollen into a container, adding 120mL of absolute ethyl alcohol, performing ultrasonic treatment for 2 hours at 300W, repeatedly cleaning with deionized water after suction filtration, drying at 70 ℃ for 15 hours, calcining at 320 ℃ in air for 10 hours, cooling to room temperature, immersing into a sufficient amount of nitric acid solution with the concentration of 8mol/L for 50 minutes, taking out, and drying to obtain pretreated pollen;
2) Dissolving 4.2g of ammonium molybdate tetrahydrate in 60mL of deionized water to obtain a molybdenum salt solution, dissolving 7.2g of citric acid in 50mL of ethylene glycol to obtain a citric acid solution, adding the molybdenum salt solution into the citric acid solution, fully stirring at a water bath of 85 ℃, refluxing in the water bath of 103 ℃ for 15 hours to obtain a sol, dispersing 0.5g of pretreated pollen in 15g of the sol, stirring at 1000r/min for 5 hours, filtering, washing and drying the product after ageing, and calcining in the air at 630 ℃ for 10 hours to obtain the metal oxide porous hollow microspheres;
3) Adding 6g of hexamethyldisilazane, 2mL of deionized water and 80mL of ethanol into a container, stirring in a water bath kettle at 35 ℃ for 50min, adding 80g of metal oxide porous hollow microspheres, uniformly mixing, heating the water bath temperature to 88 ℃ and reacting for 3h, standing for 2h after the reaction is finished, pouring out supernatant, standing at room temperature for 10h, and vacuum-drying at 130 ℃ for 6h to obtain the modified metal oxide porous hollow microspheres.
Comparative example 1: this comparative example is substantially the same as example 1 except that a conventional nitrile rubber is used instead of the modified nitrile rubber.
Comparative example 2: this comparative example is substantially the same as example 1 except that the modified metal oxide porous hollow microspheres are not added during the preparation of the modified nitrile rubber.
Comparative example 3: this comparative example is substantially the same as example 1 except that no high temperature resistant silicone rubber is contained.
Comparative example 4: this comparative example is substantially the same as example 1 except that no heat resistant auxiliary agent is added during the preparation of the high temperature resistant silicone rubber.
Comparative example 5: this comparative example is substantially the same as example 1 except that the modified metal oxide porous hollow microspheres are not added during the preparation of the high temperature resistant silicone rubber.
Test experiment:
the high temperature resistant nitrile rubber noise reduction material samples provided in examples 1-3 and comparative examples 1-5 were pressed out into a film having a thickness of 2.0.+ -. 0.2mm by a calender, and then drum-vulcanized and crosslinked by setting a thickness of 2mm in a drum-type vulcanizing machine having a drum diameter of 700mm, and vulcanization parameters were: the temperature was 150℃and the linear velocity of the vulcanizing drum was 0.12m/min, so that samples were obtained, and then the samples were subjected to high temperature resistance test, and the results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the high-temperature-resistant nitrile rubber noise reduction material has low change loss rate of mechanical properties after long-time high-temperature air aging treatment, does not influence normal use, has good high-temperature resistance, and can meet normal use in a high-temperature environment.
The sample was subjected to a test for noise reduction performance by cutting a 1.2mX1.1m template, and the test results are shown in Table 2.
TABLE 2
| Example 1 | Example 2 | Example 3 | Comparative example 1 | |
| Noise reduction dB | 31.5 | 32.7 | 32.3 | 23.5 |
| Comparative example 2 | Comparative example 3 | Comparative example 4 | Comparative example 5 | |
| Noise reduction dB | 24.7 | 23.1 | 30.2 | 24.3 |
As can be seen from Table 2, the high-temperature-resistant nitrile rubber noise reduction material has good noise reduction performance, has excellent sound absorption effect and can effectively inhibit noise emission of the surrounding environment.
The preferred embodiments of the invention disclosed above are intended only to assist in the explanation of the invention. The preferred embodiments are not exhaustive or to limit the invention to the precise form disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best understand and utilize the invention. The invention is limited only by the claims and the full scope and equivalents thereof.
Claims (10)
1. The high-temperature-resistant nitrile rubber noise reduction material is characterized by being prepared from the following raw materials in parts by weight: 50-70 parts of modified nitrile rubber, 20-30 parts of high temperature resistant silicon rubber, 2-4 parts of zinc oxide, 1-3 parts of stearic acid, 3-6 parts of a silane coupling agent, 15-20 parts of a compatibilizer, 2-6 parts of an anti-aging agent, 2-3 parts of an accelerator and 1-3 parts of sulfur.
2. The high-temperature-resistant nitrile rubber noise reduction material according to claim 1, wherein the compatibilizer is dioctyl phthalate and triphenyl phosphate in a mass ratio of 1: (1-2) a mixture;
the anti-aging agent is at least one of an anti-aging agent RD and an anti-aging agent 4010 NA;
the accelerator is at least one of accelerator MBTS and accelerator TMTD.
3. The high temperature resistant nitrile rubber noise reducing material according to claim 1, wherein the preparation method of the modified nitrile rubber is as follows:
1) Respectively adding bisphenol A epoxy resin accounting for 1-3% of the mass of the liquid polysulfide rubber and bicyclic amidine accounting for 0.01-0.05% of the mass of the liquid polysulfide rubber, stirring for 40-50 hours at the constant temperature of 80-85 ℃ to obtain pretreated polysulfide rubber, and then uniformly mixing the pretreated polysulfide rubber, the modified metal oxide porous hollow microspheres and titanium dioxide on a mixer to obtain modified polysulfide rubber;
2) Evenly mixing manganese dioxide, dibutyl phthalate and an accelerator D to obtain a vulcanizing agent, evenly mixing modified polysulfide rubber, nitrile rubber and the vulcanizing agent, and vulcanizing and cross-linking to form after mixing by an internal mixer to obtain the modified nitrile rubber.
4. The high-temperature-resistant nitrile rubber noise reduction material according to claim 3, wherein the mass ratio of the pretreated polysulfide rubber, the modified metal oxide porous hollow microspheres and the titanium dioxide is (100-150): (30-40): (10-18);
the mass ratio of the manganese dioxide to the dibutyl phthalate to the accelerator D is (30-50): (30-50): (1-2);
the mass ratio (3-6) of the modified polysulfide rubber, the nitrile rubber and the vulcanizing agent is as follows: (15-25): 1.
5. the high temperature resistant nitrile rubber noise reducing material according to claim 1, wherein the preparation method of the high temperature resistant silicone rubber is as follows:
1) Adding a tetramethyl ammonium hydroxide aqueous solution into a container, slowly dripping tetraethoxysilane into the container, stirring overnight at room temperature, then reacting for 10-15h at 60-64 ℃, distilling under reduced pressure to remove the solvent, cooling in a refrigerator to crystallize, filtering, repeatedly washing with acetone, and drying for later use;
2) Adding 5-10g of the product into a container filled with 30-40mL of dimethyl chlorosilane, 50-70mL of n-hexane and 100-160mLN, N-dimethylformamide, stirring and cooling to 0 ℃ at room temperature, adding 80-120mL of distilled water and stirring to room temperature, washing the separated organic phase to be neutral by deionized water, carrying out reduced pressure distillation, placing into a refrigerator for low-temperature crystallization, washing the product by methanol, filtering and drying to obtain a cross-linking agent;
3) Mixing 10-12g of quinone, 12-14g of dibenzyl ketone and 120-160mL of absolute ethyl alcohol, heating to 80-84 ℃, slowly dripping 8-10mL of potassium hydroxide ethanol solution, reacting for 15-20min under the protection of nitrogen, cooling to 0 ℃, carrying out suction filtration on the product, repeatedly washing by ethanol, drying, mixing with 30-40g of hydroxyl silicone oil and 3-6g of alpha-chloronaphthalene, placing in an oil bath pot, heating, stirring and refluxing for 8-12h under 220-230 ℃ and nitrogen atmosphere, standing, cooling and layering, adding methanol into an upper product for segregation and separation, and carrying out reduced pressure distillation at 150-160 ℃ to obtain a heat-resistant auxiliary agent;
4) Adding a cross-linking agent, ethynyl cyclohexanol, modified metal oxide porous hollow microspheres and a heat-resistant auxiliary agent into vinyl silicone oil, uniformly mixing, adding a platinum catalyst, stirring for 30-50min, placing into a vacuum drying oven, removing bubbles in the system at room temperature, pouring into a mould, and curing at room temperature to obtain the high-temperature-resistant silicone rubber.
6. The high temperature resistant nitrile rubber noise reducing material according to claim 5, wherein the volume ratio of the aqueous solution of tetramethyl ammonium hydroxide to tetraethoxysilane is (45-55): (6-10);
the concentration of the tetramethyl ammonium hydroxide aqueous solution is 10-13wt%;
the concentration of the potassium hydroxide ethanol solution is 15-18wt%;
the mass ratio of the vinyl silicone oil, the cross-linking agent, the ethynyl cyclohexanol, the modified metal oxide porous hollow microspheres, the heat-resistant auxiliary agent and the platinum catalyst is (40-60): (1-2): (0.005-0.008): (2-5): (3-6): (0.1-0.2).
7. The high temperature resistant nitrile rubber noise reducing material according to any one of claims 3 to 6, wherein the preparation method of the modified metal oxide porous hollow microspheres is as follows:
1) Adding lotus pollen into absolute ethyl alcohol, dispersing uniformly, filtering, repeatedly cleaning with deionized water, drying at 60-70deg.C for 12-15 hr, calcining at 300-320 deg.C in air for 6-10 hr, cooling to room temperature, soaking in sufficient nitric acid solution for 30-50min, taking out, and oven drying to obtain pretreated pollen;
2) Dissolving 3.7-4.2g of ammonium molybdate tetrahydrate in 40-60mL of deionized water to obtain a molybdenum salt solution, dissolving 6.6-7.2g of citric acid in 30-50mL of ethylene glycol to obtain a citric acid solution, adding the molybdenum salt solution into the citric acid solution, fully stirring in a water bath at 80-85 ℃, refluxing in the water bath at 100-103 ℃ for 12-15h to obtain a sol, dispersing pretreated pollen in the sol, stirring for 3-5h, ageing, filtering, washing and drying the product, and calcining in air at 600-630 ℃ for 6-10h to obtain the metal oxide porous hollow microspheres;
3) Adding hexamethyldisilazane, deionized water and ethanol into a container, stirring in a water bath at 30-35 ℃ for 30-50min, adding metal oxide porous hollow microspheres, uniformly mixing, heating the water bath to 85-88 ℃ and reacting for 2-3h, standing for 1-2h after the reaction is finished, pouring out supernatant, standing for 5-10h at room temperature, and drying to obtain the modified metal oxide porous hollow microspheres.
8. The high-temperature-resistant nitrile rubber noise reducing material according to claim 7, wherein the usage ratio of the lotus pollen to the absolute ethyl alcohol is (10-15) g: (80-120) mL;
the concentration of the nitric acid solution is 6-8mol/L;
the mass ratio of the pretreated pollen to the sol is (0.3-0.5): (10-15).
9. The high temperature resistant nitrile rubber noise reducing material according to claim 7, wherein the ratio of the amounts of hexamethyldisilazane, deionized water, ethanol and metal oxide porous hollow microspheres is (3-6) g: (1-2) mL: (50-80) mL: (60-80) g.
10. The high temperature resistant nitrile rubber noise reducing material according to claim 1, wherein the preparation method of the high temperature resistant nitrile rubber noise reducing material is as follows:
according to the weight portion, pouring the modified nitrile rubber, the high temperature resistant silicon rubber, the zinc oxide, the stearic acid, the silane coupling agent, the anti-aging agent and the dilatant into an internal mixer for mixing to form a mixed rubber, cooling to room temperature, pouring into an open mill, adding sulfur and an accelerant after the temperature of the mixed rubber is reduced to below 100 ℃, uniformly tamping, and performing vulcanization crosslinking molding to obtain the required high temperature resistant nitrile rubber noise reduction material.
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| CN101591422A (en) * | 2009-06-08 | 2009-12-02 | 江南大学 | A kind of preparation method of reactive fluid rubber-epoxide resin polymer |
| CN105810447A (en) * | 2016-04-29 | 2016-07-27 | 陕西科技大学 | Preparation method of porous spherical biological carbon and application |
| CN106317893A (en) * | 2016-09-08 | 2017-01-11 | 沈阳化工大学 | Novel silicone rubber containing phenyl-terminated methylvinyl(tetraphenyl)phenyl |
| CN107522960A (en) * | 2017-09-25 | 2017-12-29 | 西南科技大学 | The preparation method of damping noise reduction rubber nano composite material device |
| WO2022134932A1 (en) * | 2020-12-22 | 2022-06-30 | 华南理工大学 | High-pt-content and high-performance catalyst having high stability and anti-polarity reversal performance and preparation method therefor |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101591422A (en) * | 2009-06-08 | 2009-12-02 | 江南大学 | A kind of preparation method of reactive fluid rubber-epoxide resin polymer |
| CN105810447A (en) * | 2016-04-29 | 2016-07-27 | 陕西科技大学 | Preparation method of porous spherical biological carbon and application |
| CN106317893A (en) * | 2016-09-08 | 2017-01-11 | 沈阳化工大学 | Novel silicone rubber containing phenyl-terminated methylvinyl(tetraphenyl)phenyl |
| CN107522960A (en) * | 2017-09-25 | 2017-12-29 | 西南科技大学 | The preparation method of damping noise reduction rubber nano composite material device |
| WO2022134932A1 (en) * | 2020-12-22 | 2022-06-30 | 华南理工大学 | High-pt-content and high-performance catalyst having high stability and anti-polarity reversal performance and preparation method therefor |
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