CN105111551A - High-flame-retardance modified carboxyl nitrile-butadiene rubber composite material - Google Patents
High-flame-retardance modified carboxyl nitrile-butadiene rubber composite material Download PDFInfo
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Abstract
The invention discloses a high-flame-retardance modified carboxyl nitrile-butadiene rubber composite material. The high-flame-retardance modified carboxyl nitrile-butadiene rubber composite material is prepared from organosilicon modified carboxyl nitrile-butadiene rubber, epoxidated nitrile-butadiene rubber, chloroprene rubber, stearic acid, zinc oxide, zinc methacrylate, sulfur, dicumyl peroxide, precipitated white carbon black, molybdenum dioxide, carboxylated multi-walled carbon nanotubes, aluminum hydroxide, a flame retardant, graphite oxide, adipate, dibutyl phthalate, an accelerant CZ, an accelerant TMTD, an anti-aging agent RD, an anti-aging agent H, an anti-aging agent MB and an anti-aging agent AW. The high-flame-retardance modified carboxyl nitrile-butadiene rubber composite material provided by the invention is good in flame retardance and excellent in high- and low-temperature resistance and oil resistance.
Description
Technical field
The present invention relates to technical field of rubber material, particularly relate to a kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material.
Background technology
At present, macromolecular material has been widely used in the life of people, as plastics, rubber, fiber, coating and tackiness agent etc. are in great demand all over the world.Although macromolecular material has a lot of advantage relative to traditional material, its inflammableness makes it be restricted in the application of some special dimension.Rubber is as the widely used macromolecular material of one, and its flame retardant properties is not very desirable, and therefore, improving the flame retardant properties of elastomeric material, is current problem demanding prompt solution to meet the requirement of the society of high speed development.
Summary of the invention
Based on the technical problem that background technology exists, the present invention proposes a kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material, its flame retardant properties is good, resistant of high or low temperature and oil resistance excellence.
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 55-65 part, Epoxy acrylonitrile-butadirubber rubber 15-35 part, chloroprene rubber 5-20 part, stearic acid 1-2.5 part, zinc oxide 1-3 part, zinc methacrylate 0.2-1 part, sulphur 1-2 part, dicumyl peroxide 1-2 part, precipitated silica 10-25 part, molybdenum dioxide 5-20 part, functionalized multi-wall carbonnanotubes 10-25 part, aluminium hydroxide 3-10 part, fire retardant 4-10 part, graphite oxide 10-25 part, adipic acid ester 3-5 part, dibutyl phthalate 2-5 part, accelerant CZ 1-2 part, Vulcanization accelerator TMTD 1-1.5 part, anti-aging agent RD 0.8-2 part, antioxidant H 0.2-1 part, antioxidant MB 0.5-1.5 part, antioxidant A W0.3-1.5 part,
Wherein, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with isocyanatopropyl triethoxyl silane, dibutyl tin laurate and p-ten.-butylcatechol by carboxy nitrile rubber, pass into nitrogen, and 55-65 DEG C is warming up under whipped state, reaction 3-7h, cooling obtains organic-silicon-modified carboxy nitrile rubber;
The following technique of described fire retardant is prepared: by 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and vinyltriethoxysilane join in toluene, under whipped state, 95-100 DEG C is warming up to after passing into nitrogen, reaction 38-45min, then benzoyl peroxide is added, reaction 17-18h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
Preferably, the weight ratio of organic-silicon-modified carboxy nitrile rubber, Epoxy acrylonitrile-butadirubber rubber, chloroprene rubber is 60-65:20-30:9-16.
Preferably, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 61-64 part, Epoxy acrylonitrile-butadirubber rubber 22-28 part, chloroprene rubber 10-15 part, stearic acid 1.6-2.2 part, zinc oxide 1.5-2.7 part, zinc methacrylate 0.4-0.8 part, sulphur 1.3-1.8 part, dicumyl peroxide 1.2-1.9 part, precipitated silica 15-22 part, molybdenum dioxide 9-15 part, functionalized multi-wall carbonnanotubes 15-21 part, aluminium hydroxide 5-9 part, fire retardant 6-8 part, graphite oxide 13-22 part, adipic acid ester 3.5-4.5 part, dibutyl phthalate 3.8-4.5 part, accelerant CZ 1.2-1.8 part, Vulcanization accelerator TMTD 1.2-1.35 part, anti-aging agent RD 1-1.5 part, antioxidant H 0.5-0.9 part, antioxidant MB 0.8-1.3 part, antioxidant A W0.5-1.2 part.
Preferably, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 63 parts, Epoxy acrylonitrile-butadirubber rubber 25 parts, chloroprene rubber 13 parts, stearic acid 2 parts, 2.2 parts, zinc oxide, zinc methacrylate 0.6 part, 1.5 parts, sulphur, dicumyl peroxide 1.6 parts, precipitated silica 20 parts, molybdenum dioxide 10 parts, functionalized multi-wall carbonnanotubes 18 parts, 8 parts, aluminium hydroxide, fire retardant 7 parts, graphite oxide 20 parts, adipic acid ester 4 parts, dibutyl phthalate 4.2 parts, accelerant CZ 1.6 parts, Vulcanization accelerator TMTD 1.25 parts, anti-aging agent RD 1.3 parts, antioxidant H 0.8 part, antioxidant MB 1 part, antioxidant A W1 part.
Preferably, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 5-10 part isocyanatopropyl triethoxyl silane, 0.1-0.3 part dibutyl tin laurate and 0.05-0.15 part p-ten.-butylcatechol by 55-80 part carboxy nitrile rubber by weight, pass into nitrogen, and 58-63 DEG C is warming up under whipped state, reaction 4-6h, cooling obtains described organic-silicon-modified carboxy nitrile rubber.
Preferably, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 8 parts of isocyanatopropyl triethoxyl silanes, 0.2 part of dibutyl tin laurate and 0.1 part of p-ten.-butylcatechol by 60 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 60 DEG C are warming up under whipped state, reaction 5.5h, cooling obtains described organic-silicon-modified carboxy nitrile rubber.
Preferably, the following technique of described fire retardant is prepared: by weight by 15-20 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 10-18 part vinyltriethoxysilane join in 50-80 part toluene, under whipped state, 95-100 DEG C is warming up to after passing into nitrogen, reaction 38-45min, then add 0.2-0.5 part benzoyl peroxide, reaction 17-18h, after reaction terminates, obtain described fire retardant through cooling, filtration, distillation.
Preferably, the following technique of described fire retardant is prepared: by weight by 17 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 15 parts of vinyltriethoxysilanes join in 70 parts of toluene, under whipped state, 98 DEG C are warming up to after passing into nitrogen, reaction 40min, then add 0.35 part of benzoyl peroxide, reaction 17.5h, after reaction terminates, obtain described fire retardant through cooling, filtration, distillation.
Preferably, the diameter of described functionalized multi-wall carbonnanotubes is 5-15nm, and length is 20-28 μm, and carboxyl massfraction is 3-5%.
In the present invention, carboxy nitrile rubber is mixed with isocyanatopropyl triethoxyl silane, take dibutyl tin laurate as catalyzer, take p-ten.-butylcatechol as stopper, react under the protection of nitrogen, isocyano-in hydroxyl in carboxy nitrile rubber and isocyanatopropyl triethoxyl silane is reacted, thus siloxanes has been incorporated in carboxy nitrile rubber, carboxy nitrile rubber and isocyanatopropyl triethoxyl silane are combined as a whole, with Epoxy acrylonitrile-butadirubber rubber, as rubber major ingredient after chloroprene rubber mixing, consistency is good, give thermotolerance and the oil-proofness of matrix material excellence, simultaneously, TMOS in organic-silicon-modified carboxy nitrile rubber can be surperficial with precipitated silica, functionalized multi-wall carbonnanotubes, the hydroxyl of graphite oxide, carboxyl reacts, improve precipitated silica, functionalized multi-wall carbonnanotubes, the consistency of graphite oxide and rubber, it is made to be uniformly dispersed in rubber matrix, give the intensity of matrix material excellence, thermotolerance and flame retardant resistance, in described fire retardant, by 9, after the assorted-10-phospho hetero phenanthrene-10-oxide compound of 10-dihydro-9-oxy mixes with vinyltriethoxysilane, under the initiation of benzoyl peroxide, there occurs reaction, 9,10-dihydro-9-oxa-10-phosphaphenanthrene-10-oxide and vinyltriethoxysilane are combined as a whole, improve 9,10-dihydro-9-oxy is mixed the consistency of-10-phospho hetero phenanthrene-10-oxide compound and each component, functionalized multi-wall carbonnanotubes and graphite oxide auxiliary under, flame retardant properties is good.
Embodiment
Below, by specific embodiment, technical scheme of the present invention is described in detail.
In a particular embodiment, a kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, in its raw material, the weight part of organic-silicon-modified carboxy nitrile rubber can be 55,56,56.3,58,59,61,62,62.3,63,63.4,64,64.5,65 parts; The weight part of Epoxy acrylonitrile-butadirubber rubber can be 15,16,17,18,18.5,19,19.3,21,23,25,26,28,29,29.3,31,32,34.5,35 parts; The weight part of chloroprene rubber can be 5,6,7,8,8.6,9,9.3,10,10.6,11,11.3,12,13,15,16,16.3,18,18.6,19,19.3,20 parts; Stearic weight part can be 1,1.2,1.3,1.5,1.6,1.8,1.9,2,2.1,2.2,2.3,2.34,2.4,2.46,2.5 part; The weight part of zinc oxide can be 1,1.2,1.3,1.5,1.6,1.8,1.9,2,2.1,2.4,2.56,2.6,2.68,2.8,2.9,2.93,3 part; The weight part of zinc methacrylate can be 0.2,0.26,0.3,0.34,0.5,0.56,0.6,0.68,0.8,0.86,0.9,0.93,1 part; The weight part of sulphur can be 1,1.2,1.3,1.5,1.6,1.65,1.8,1.85,1.9,1.93,2 part; The weight part of dicumyl peroxide can be 1,1.2,1.3,1.5,1.6,1.8,1.85,1.9,1.96,2 part; The weight part of precipitated silica can be 10,12,13,15,16,16.3,18,19,19.3,21,23,23.4,24,24.6,25 parts; The weight part of molybdenum dioxide can be 5,6,7,8,8.5,9,9.3,10,10.6,11,13,15,16,16.3,17,17.5,18,18.6,19,19.3,20 parts; The weight part of functionalized multi-wall carbonnanotubes can be 10,12,13,13.5,15,16,16.3,17,17.5,18,18.6,19,19.3,21,23,23.4,24,24.6,25 parts; The weight part of aluminium hydroxide can be 3,4,5,5.6,6,6.3,7,7.5,8,8.6,9,9.3,10 parts; The weight part of fire retardant can be 4,5,6,7,8,8.6,9,9.3,10 parts; The weight part of graphite oxide can be 10,12,13,14,15,15.6,16,16.3,17,17.5,18,18.6,19,19.3,21,23,23.4,24,24.6,25 parts; The weight part of adipic acid ester can be 3,3.2,3.4,3.8,4,4.5,4.8,5 parts; The weight part of dibutyl phthalate can be 2,2.3,2.4,2.5,2.6,2.67,2.8,3,3.4,3.8,4,4.6,5 parts; The weight part of accelerant CZ can be 1,1.2,1.3,1.56,1.6,1.8,1.85,1.9,1.94,2 part; The weight part of Vulcanization accelerator TMTD can be 1,1.2,1.26,1.3,1.34,1.4,1.45,1.5 part; The weight part of anti-aging agent RD can be 0.8,0.86,0.9,0.93,1,1.2,1.6,1.68,1.7,1.75,1.8,1.86,1.9,1.93,2 part; The weight part of antioxidant H can be 0.2,0.26,0.3,0.34,0.4,0.45,0.5,0.56,0.6,0.63,0.7,0.86,0.9,0.93,1 part; The weight part of antioxidant MB can be 0.5,0.56,0.6,0.63,0.8,0.9,0.94,1,1.2,1.3,1.35,1.4,1.46,1.5 part; The weight part of antioxidant A W can be 0.3,0.38,0.5,0.56,0.6,0.67,0.7,0.75,0.8,0.86,0.9,1,1.2,1.3,1.35,1.4,1.46,1.5 part.
Embodiment 1
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 55 parts, Epoxy acrylonitrile-butadirubber rubber 35 parts, chloroprene rubber 5 parts, stearic acid 2.5 parts, 1 part, zinc oxide, zinc methacrylate 1 part, 1 part, sulphur, dicumyl peroxide 2 parts, precipitated silica 10 parts, molybdenum dioxide 20 parts, functionalized multi-wall carbonnanotubes 10 parts, 10 parts, aluminium hydroxide, fire retardant 4 parts, graphite oxide 25 parts, adipic acid ester 5 parts, dibutyl phthalate 5 parts, accelerant CZ 1 part, Vulcanization accelerator TMTD 1.5 parts, anti-aging agent RD 0.8 part, antioxidant H 1 part, antioxidant MB 0.5 part, antioxidant A W1.5 part, wherein, the diameter of described functionalized multi-wall carbonnanotubes is 5nm, and length is 28 μm, and carboxyl massfraction is 3%,
Described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 5 parts of isocyanatopropyl triethoxyl silanes, 0.3 part of dibutyl tin laurate and 0.05 part of p-ten.-butylcatechol by 80 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 63 DEG C are warming up under whipped state, reaction 4h, cooling obtains described organic-silicon-modified carboxy nitrile rubber;
The following technique of described fire retardant is prepared: by weight by 15 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 10 parts of vinyltriethoxysilanes join in 80 parts of toluene, under whipped state, 95 DEG C are warming up to after passing into nitrogen, reaction 45min, then 0.2 part of benzoyl peroxide is added, reaction 18h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
Embodiment 2
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 65 parts, Epoxy acrylonitrile-butadirubber rubber 15 parts, chloroprene rubber 20 parts, stearic acid 1 part, 3 parts, zinc oxide, zinc methacrylate 0.2 part, 2 parts, sulphur, dicumyl peroxide 1 part, precipitated silica 25 parts, molybdenum dioxide 5 parts, functionalized multi-wall carbonnanotubes 25 parts, 3 parts, aluminium hydroxide, fire retardant 10 parts, graphite oxide 10 parts, adipic acid ester 3 parts, dibutyl phthalate 2 parts, accelerant CZ 2 parts, Vulcanization accelerator TMTD 1 part, anti-aging agent RD 2 parts, antioxidant H 0.2 part, antioxidant MB 1.5 parts, antioxidant A W0.3 part, wherein, the diameter of described functionalized multi-wall carbonnanotubes is 15nm, and length is 20 μm, and carboxyl massfraction is 5%,
Organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 10 parts of isocyanatopropyl triethoxyl silanes, 0.1 part of dibutyl tin laurate and 0.15 part of p-ten.-butylcatechol by 55 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 58 DEG C are warming up under whipped state, reaction 6h, cooling obtains organic-silicon-modified carboxy nitrile rubber;
The following technique of described fire retardant is prepared: by weight by 20 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 18 parts of vinyltriethoxysilanes join in 50 parts of toluene, under whipped state, 100 DEG C are warming up to after passing into nitrogen, reaction 38min, then 0.5 part of benzoyl peroxide is added, reaction 17h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
Embodiment 3
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 63 parts, Epoxy acrylonitrile-butadirubber rubber 25 parts, chloroprene rubber 13 parts, stearic acid 2 parts, 2.2 parts, zinc oxide, zinc methacrylate 0.6 part, 1.5 parts, sulphur, dicumyl peroxide 1.6 parts, precipitated silica 20 parts, molybdenum dioxide 10 parts, functionalized multi-wall carbonnanotubes 18 parts, 8 parts, aluminium hydroxide, fire retardant 7 parts, graphite oxide 20 parts, adipic acid ester 4 parts, dibutyl phthalate 4.2 parts, accelerant CZ 1.6 parts, Vulcanization accelerator TMTD 1.25 parts, anti-aging agent RD 1.3 parts, antioxidant H 0.8 part, antioxidant MB 1 part, antioxidant A W1 part, wherein, organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 8 parts of isocyanatopropyl triethoxyl silanes, 0.2 part of dibutyl tin laurate and 0.1 part of p-ten.-butylcatechol by 60 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 60 DEG C are warming up under whipped state, reaction 5.5h, cooling obtains organic-silicon-modified carboxy nitrile rubber, the following technique of described fire retardant is prepared: by weight by 17 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 15 parts of vinyltriethoxysilanes join in 70 parts of toluene, under whipped state, 98 DEG C are warming up to after passing into nitrogen, reaction 40min, then 0.35 part of benzoyl peroxide is added, reaction 17.5h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
Embodiment 4
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 61 parts, Epoxy acrylonitrile-butadirubber rubber 28 parts, chloroprene rubber 10 parts, stearic acid 2.2 parts, 1.5 parts, zinc oxide, zinc methacrylate 0.8 part, 1.3 parts, sulphur, dicumyl peroxide 1.9 parts, precipitated silica 15 parts, molybdenum dioxide 15 parts, functionalized multi-wall carbonnanotubes 15 parts, 9 parts, aluminium hydroxide, fire retardant 6 parts, graphite oxide 22 parts, adipic acid ester 3.5 parts, dibutyl phthalate 4.5 parts, accelerant CZ 1.2 parts, Vulcanization accelerator TMTD 1.35 parts, anti-aging agent RD 1 part, antioxidant H 0.9 part, antioxidant MB 0.8 part, antioxidant A W1.2 part, wherein, the diameter of described functionalized multi-wall carbonnanotubes is 10nm, and length is 26 μm, and carboxyl massfraction is 4%,
Wherein, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 8 parts of isocyanatopropyl triethoxyl silanes, 0.12 part of dibutyl tin laurate and 0.09 part of p-ten.-butylcatechol by 53 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 59 DEG C are warming up under whipped state, reaction 5.3h, cooling obtains described organic-silicon-modified carboxy nitrile rubber;
The following technique of described fire retardant is prepared: by weight by 16 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 17 parts of vinyltriethoxysilanes join in 59 parts of toluene, under whipped state, 97 DEG C are warming up to after passing into nitrogen, reaction 43min, then 0.28 part of benzoyl peroxide is added, reaction 17.2h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
Embodiment 5
A kind of high flame retardant modified carboxyl nitile-butadiene rubber composite material that the present invention proposes, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 64 parts, Epoxy acrylonitrile-butadirubber rubber 22 parts, chloroprene rubber 15 parts, stearic acid 1.6 parts, 2.7 parts, zinc oxide, zinc methacrylate 0.4 part, 1.8 parts, sulphur, dicumyl peroxide 1.2 parts, precipitated silica 22 parts, molybdenum dioxide 9 parts, functionalized multi-wall carbonnanotubes 21 parts, 5 parts, aluminium hydroxide, fire retardant 8 parts, graphite oxide 13 parts, adipic acid ester 4.5 parts, dibutyl phthalate 3.8 parts, accelerant CZ 1.8 parts, Vulcanization accelerator TMTD 1.2 parts, anti-aging agent RD 1.5 parts, antioxidant H 0.5 part, antioxidant MB 1.3 parts, antioxidant A W0.5 part, wherein, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 8.6 parts of isocyanatopropyl triethoxyl silanes, 0.18 part of dibutyl tin laurate and 0.012 part of p-ten.-butylcatechol by 75 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 62 DEG C are warming up under whipped state, reaction 4.3h, cooling obtains described organic-silicon-modified carboxy nitrile rubber, the following technique of described fire retardant is prepared: by weight by 18 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 11 parts of vinyltriethoxysilanes join in 76 parts of toluene, under whipped state, 99 DEG C are warming up to after passing into nitrogen, reaction 39min, then 0.23 part of benzoyl peroxide is added, reaction 17.8h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
The above; be only the present invention's preferably embodiment; but protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses; be equal to according to technical scheme of the present invention and inventive concept thereof and replace or change, all should be encompassed within protection scope of the present invention.
Claims (9)
1. a high flame retardant modified carboxyl nitile-butadiene rubber composite material, it is characterized in that, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 55-65 part, Epoxy acrylonitrile-butadirubber rubber 15-35 part, chloroprene rubber 5-20 part, stearic acid 1-2.5 part, zinc oxide 1-3 part, zinc methacrylate 0.2-1 part, sulphur 1-2 part, dicumyl peroxide 1-2 part, precipitated silica 10-25 part, molybdenum dioxide 5-20 part, functionalized multi-wall carbonnanotubes 10-25 part, aluminium hydroxide 3-10 part, fire retardant 4-10 part, graphite oxide 10-25 part, adipic acid ester 3-5 part, dibutyl phthalate 2-5 part, accelerant CZ 1-2 part, Vulcanization accelerator TMTD 1-1.5 part, anti-aging agent RD 0.8-2 part, antioxidant H 0.2-1 part, antioxidant MB 0.5-1.5 part, antioxidant A W0.3-1.5 part,
Wherein, described organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with isocyanatopropyl triethoxyl silane, dibutyl tin laurate and p-ten.-butylcatechol by carboxy nitrile rubber, pass into nitrogen, and 55-65 DEG C is warming up under whipped state, reaction 3-7h, cooling obtains organic-silicon-modified carboxy nitrile rubber;
The following technique of described fire retardant is prepared: by 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and vinyltriethoxysilane join in toluene, under whipped state, 95-100 DEG C is warming up to after passing into nitrogen, reaction 38-45min, then benzoyl peroxide is added, reaction 17-18h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
2. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to claim 1, it is characterized in that, the weight ratio of organic-silicon-modified carboxy nitrile rubber, Epoxy acrylonitrile-butadirubber rubber, chloroprene rubber is 60-65:20-30:9-16.
3. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to claim 1 or 2, it is characterized in that, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 61-64 part, Epoxy acrylonitrile-butadirubber rubber 22-28 part, chloroprene rubber 10-15 part, stearic acid 1.6-2.2 part, zinc oxide 1.5-2.7 part, zinc methacrylate 0.4-0.8 part, sulphur 1.3-1.8 part, dicumyl peroxide 1.2-1.9 part, precipitated silica 15-22 part, molybdenum dioxide 9-15 part, functionalized multi-wall carbonnanotubes 15-21 part, aluminium hydroxide 5-9 part, fire retardant 6-8 part, graphite oxide 13-22 part, adipic acid ester 3.5-4.5 part, dibutyl phthalate 3.8-4.5 part, accelerant CZ 1.2-1.8 part, Vulcanization accelerator TMTD 1.2-1.35 part, anti-aging agent RD 1-1.5 part, antioxidant H 0.5-0.9 part, antioxidant MB 0.8-1.3 part, antioxidant A W0.5-1.2 part.
4. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-3, it is characterized in that, its raw material comprises following component by weight: organic-silicon-modified carboxy nitrile rubber 63 parts, Epoxy acrylonitrile-butadirubber rubber 25 parts, chloroprene rubber 13 parts, stearic acid 2 parts, 2.2 parts, zinc oxide, zinc methacrylate 0.6 part, 1.5 parts, sulphur, dicumyl peroxide 1.6 parts, precipitated silica 20 parts, molybdenum dioxide 10 parts, functionalized multi-wall carbonnanotubes 18 parts, 8 parts, aluminium hydroxide, fire retardant 7 parts, graphite oxide 20 parts, adipic acid ester 4 parts, dibutyl phthalate 4.2 parts, accelerant CZ 1.6 parts, Vulcanization accelerator TMTD 1.25 parts, anti-aging agent RD 1.3 parts, antioxidant H 0.8 part, antioxidant MB 1 part, antioxidant A W1 part.
5. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-4, it is characterized in that, organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 5-10 part isocyanatopropyl triethoxyl silane, 0.1-0.3 part dibutyl tin laurate and 0.05-0.15 part p-ten.-butylcatechol by 55-80 part carboxy nitrile rubber by weight, pass into nitrogen, and 58-63 DEG C is warming up under whipped state, reaction 4-6h, cooling obtains organic-silicon-modified carboxy nitrile rubber.
6. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-5, it is characterized in that, organic-silicon-modified carboxy nitrile rubber is prepared according to following technique: after being mixed with 8 parts of isocyanatopropyl triethoxyl silanes, 0.2 part of dibutyl tin laurate and 0.1 part of p-ten.-butylcatechol by 60 parts of carboxy nitrile rubbers by weight, pass into nitrogen, and 60 DEG C are warming up under whipped state, reaction 5.5h, cooling obtains organic-silicon-modified carboxy nitrile rubber.
7. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-6, it is characterized in that, the following technique of described fire retardant is prepared: by weight by 15-20 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 10-18 part vinyltriethoxysilane join in 50-80 part toluene, under whipped state, 95-100 DEG C is warming up to after passing into nitrogen, reaction 38-45min, then 0.2-0.5 part benzoyl peroxide is added, reaction 17-18h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
8. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-7, it is characterized in that, the following technique of described fire retardant is prepared: by weight by 17 part 9, assorted-10-phospho hetero phenanthrene-10-the oxide compound of 10-dihydro-9-oxy and 15 parts of vinyltriethoxysilanes join in 70 parts of toluene, under whipped state, 98 DEG C are warming up to after passing into nitrogen, reaction 40min, then 0.35 part of benzoyl peroxide is added, reaction 17.5h, obtains described fire retardant through cooling, filtration, distillation after reaction terminates.
9. high flame retardant modified carboxyl nitile-butadiene rubber composite material according to any one of claim 1-8, is characterized in that, the diameter of described functionalized multi-wall carbonnanotubes is 5-15nm, and length is 20-28 μm, and carboxyl massfraction is 3-5%.
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| CN110330708A (en) * | 2019-06-12 | 2019-10-15 | 福州大学 | A kind of recyclable regenerative rubber and preparation method thereof |
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Application publication date: 20151202 |