CN104130539A - Flame-retardant high-damping rubber composition using polynorbornene rubber as main body - Google Patents
Flame-retardant high-damping rubber composition using polynorbornene rubber as main body Download PDFInfo
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Abstract
The invention discloses a flame-retardant high-damping rubber composition using polynorbornene rubber as a main body. The composition adopts blended comixture of the polynorbornene rubber and chloroprene rubber as a basic material and uses tetramethyl acrylate diglycerol o-benzoate as a compatibilizer for blending and co-mixing the polynorbornene rubber and the chloroprene rubber. The blending and co-mixing ratio of the polynorbornene rubber to the chloroprene rubber is (65-60) to (35-40); the dosage of tetramethyl acrylate diglycerol o-benzoate compatibilizer is 5-10 parts by weight. The rubber composition uses a promoter TMTD, a promoter DM, a vulcanizing agent DTDM and a vulcanization system as a co-vulcanization agent, wherein the dosage of the promoter TMTD is 1.5-2.0 parts by weight, the dosage of the promoter DM is 1.5-2.0 parts by weight, and the dosage of the vulcanizing agent DTDM is 2.0-2.5 parts by weight. The rubber composition disclosed by the invention can be used for improving the flame retardant grade of the polynorbornene rubber and broadening the application range of the polynorbornene rubber; a rubber product prepared by using the rubber composition is excellent in flame-retardant, damping and shock-absorbing effect.
Description
Technical field
The present invention relates to a kind of rubber combination for the manufacture of fire-retardant high damping, specifically, relate to a kind of take itself there is the fire-retardant highly damping rubber composition that poly-norbornene rubber that high damping properties is feature is main body.
Background technology
Bullet train operation has become one of Chinese national economy growth and the requisite modern means of communication of social development, no matter from historical development, or technical progress aspect, the manufacturing tempo of bullet train and progressive levels are all quite surprising.In recent years, people have proposed requirements at the higher level to bullet train riding comfort, security, enforcement high speed.For this reason, ride security measures problem and noise problem and the fire-retardant requirement of high-damping blanket has been become to imperative problem of the bullet train of solution.Rubber is a kind of material with high inner friction performance, can be effectively the mechanical energy of vibrations and noise be converted into heat energy, and elastomeric material is easy to process, can be by extruding, the working method such as mold pressing, injection, make different shape, meet different working conditionss.Therefore, rubber is one of most popular damping material in engineering.
Poly-norbornene rubber is succeeded in developing by French CDFChimie company at first, and it is to be obtained by ethene and cyclopentadiene ring-opening copolymerization by Diels-Alder catalyst.Have following molecular structure, ASTM name code name is PNR.
The maximum feature of this rubber is very soft, can make durometer level and forgive the elastomer material of rubber sponge and various solids, in view of its high damping damping and amortization, can make shockproof, to alleviate noise component at aspects such as automobile, railway, navigation, building, sports goodss, the shock insulation material that is expected exploitation adaptation entire spectrum (is illustrated in clean brook chief editor < < robber materials handbook > >, Chemical Industry Press, in January, 2007 second edition, P360-363).But poly-norbornene rubber is combustible in air.When it is applied for damping damping, during especially for bullet train, often require it can there is certain flame retardant properties, therefore, the flame retardant properties that improves poly-norbornene rubber is of great significance.
Summary of the invention
The object of this invention is to provide a kind of flame retardant properties and obtain the high damping flame-retardant rubber composition that the poly-norbornene rubber that obviously improves is main body, can make thus the range of application of poly-norbornene rubber be entered one and widen.
The present invention realizes like this, it is a kind of fire-retardant highly damping rubber composition that poly-norbornene rubber is main body of take, it is characterized in that, said composition forms and to comprise that take poly-norbornene rubber and chloroprene rubber fusion blend is base mateiral, take the expanding material of tetramethyl-vinylformic acid two glycerol o-benzoates as poly-norbornene rubber and chloroprene rubber fusion blend.
In the present invention, in weight part, poly-norbornene rubber and chloroprene rubber fusion blending ratio are: 65-60/40-35.
In the present invention, the weight sum of poly-norbornene rubber and chloroprene rubber of take is 100 weight parts, and the consumption of described tetramethyl-vinylformic acid two glycerol o-benzoate expanding materials is 5-10 weight part.
Rubber combination described in the present invention be take accelerant disulfide tetra methylthiuram TMTD+ accelerator dibenzothiazyl disulfide DM+ vulcanizing agent dimorpholinyl disulfide DTDM be co-curing agent with vulcanization system, the weight sum of poly-norbornene rubber and chloroprene rubber of take is 100 weight parts, Vulcanization accelerator TMTD consumption is 1.5～2.0 weight parts, altax consumption is 1.5～2.0 weight parts, and vulcanizing agent DTDM consumption is 2.0～2.5 weight parts.
Adopt Vulcanization accelerator TMTD+altax+vulcanizing agent DTDM and use vulcanization system as effective initiation tetramethyl-vinylformic acid two glycerol o-benzoates and poly-norbornene rubber and chloroprene rubber covulcanization.
Polymer blending technology is the technology that is usually used at present elastomeric material modification, can realize learning from other's strong points to offset one's weaknesses of two or more materials, chloroprene rubber is that in the conventional rubber known of people, flame resistivity is best, its oxygen index is 33, so the present invention is just conceived to improve with chloroprene rubber the flame retardant properties of poly-norbornene rubber, chemical structure in view of poly-norbornene rubber, there is certain difference in the aspects such as inter-vulcanizability and chloroprene rubber, to the physical and mechanical properties of its blended vulcanizate, can have a huge impact, therefore in order to realize both effective blend, the present invention is to chloroprene rubber and poly-norbornene rubber blended ratio, compatilizer, the method of covulcanization system has been done meticulous screening.
The consistency of poly-norbornene rubber and chloroprene rubber fusion blend components has significant impact to the structural state of blend and physical and mechanical properties etc., when thering is good consistency between blend components, disperse phase structure in blend has small distribution, and this blend just has good physical and mechanical properties and some other superperformance.On the contrary, when the consistency of blend component is poor, through the component of fusion blend, can not mix fully, in blend, two components have formed coarse distribution.The blend of this coarse distribution has poor physical and mechanical properties and some other bad performance.For improving the compatible effect of this blend component, contriver adopts the method for adding tetramethyl-vinylformic acid two glycerol o-benzoate expanding materials, it is 100 weight parts that the consumption of expanding material be take poly-norbornene rubber and chloroprene rubber weight sum, and the consumption of expanding material is 5-10 weight part.
Poly-norbornene rubber and chloroprene rubber fusion blend, itself and with the strength and extension property of cross-linked rubber, the increase with chloroprene rubber content declines, flame retardant resistance increase.The present invention considers the over-all properties of resistance to fire-retardant highly damping rubber composition, and poly-norbornene rubber and chloroprene rubber fusion blending ratio, be: 65-60/40-35 by weight.
During two or more blend rubber, the performance of final product depends on that can they realize covulcanization to a great extent, and the realization of covulcanization has great relation with the curing system of selecting again.According to the present invention, adopt accelerant disulfide tetra methylthiuram TMTD+ accelerator dibenzothiazyl disulfide DM+ vulcanizing agent dimorpholinyl disulfide DTDM and use vulcanization system as effective initiation tetramethyl-vinylformic acid two glycerol o-benzoates and poly-norbornene rubber and chloroprene rubber covulcanization, first this be because using Vulcanization accelerator TMTD+altax+vulcanizing agent DTDM paralled system during as linking agent, the tetramethyl-vinylformic acid two generation graft polymerization of glycerol o-benzoate and poly-norbornene rubbers in sulfuration, the rubber of chloroprene rubber forms space reticulated structure, realize covulcanization, in addition this and be easy to get with vulcanization system is general, easy to utilize.The sulfuration over-all propertieies such as the material making has high-tenacity and elongation, and anti-tear, compression set is little.At this moment take poly-norbornene rubber and chloroprene rubber add with together be 100 weight parts, Vulcanization accelerator TMTD consumption is 1.5～2.0 weight parts, altax consumption is 1.5～2.0 weight parts, vulcanizing agent DTDM consumption is 2.0～2.5 weight parts.
In the component of rubber combination of the present invention, also comprise strengthening agent, weighting agent, promoting agent, flame retardant.
Strengthening agent described in the present invention is that high abrasion furnace carbon black N330, described weighting agent are that aluminium hydroxide, described promoting agent are that stearic acid, zinc oxide and magnesium oxide, described flame retardant are decabromodiphynly oxide.
Of the present inventionly take fire-retardant highly damping rubber composition that poly-norbornene rubber is main body compared with prior art, there is obvious progress, first, it has improved the flame retardant rating of poly-norbornene rubber, thereby widened the use range of poly-norbornene rubber, secondly, the present invention selects compatilizer tetramethyl-vinylformic acid two glycerol o-benzoates, selecting Vulcanization accelerator TMTD+altax+vulcanizing agent DTDM is also co-curing agent with vulcanization system, these materials are all the common agents in Chemical market, thereby source be easy to get, easy to utilize.With the present composition, manufacture the fire-retardant position of high damping shock absorption of riding train, through user's experiment detection and entrucking tyre mileage test, fire-retardant damping shock absorption effect is excellent.Rubber combination of the present invention can be prepared in ordinary rubber source mill, has industrial applications future widely.
Embodiment
Below in conjunction with embodiment, the present invention is done into an explanation, but the present invention is never confined to these embodiment.The performance test results described in embodiment, the numerical value that all refers to adopt the method for corresponding national Specification to record.
In the following embodiments, table 1 is depicted as the basic recipe that embodiment raw material forms, and the component in basic recipe increases or reduce adjustment according to specific embodiment.
Table 1
| Component title | Consumption (weight part) |
| Poly-norbornene rubber+chloroprene rubber | 100 |
| High abrasion carbon black N330 | 30 |
| Aluminium hydroxide Al (OH) 3 | 120 |
| Expanding material, oligomer ester-I | 5-10 |
| Zinc oxide | 5 |
| Magnesium oxide | 4 |
| Decabromodiphynly oxide | 10 |
| Stearic acid | 1.0 |
| Vulcanization accelerator TMTD | 1.5-2 |
| Altax | 1.5-2 |
| Vulcanizing agent DTDM | 2-2.5 |
Embodiment 1
By poly-norbornene rubber 62 weight parts, chloroprene rubber 38 weight parts, expanding material tetramethyl-vinylformic acid two glycerol o-benzoate 10 weight parts, 30 weight part strengthening agent high abrasion carbon black N330, weighting agent aluminium hydroxide Al (OH) 3120 weight parts, promoting agent zinc oxide 5 weight parts, magnesium oxide 4 weight parts, stearic acid 1 weight part, flame retardant decabromodiphynly oxide 10 weight parts all add in Banbury mixer mixing, melting temperature is 45 ℃～70 ℃, and mixing time is 20～40 minutes; Co-curing agent accelerant disulfide tetra methylthiuram TMTD2 weight part+accelerator dibenzothiazyl disulfide DM2 weight part+vulcanizing agent dimorpholinyl disulfide DTDM2.5 weight part adds in Banbury mixer for 5～10 minutes before mixing end, mixing together with other components.Make rubber combination product.
Comparative example 1
Except using poly-norbornene rubber 50 weight parts, chloroprene rubber 50 weight parts, other formulas and operation steps, all with embodiment 1, make rubber combination product.
Comparative example 2
Except using poly-norbornene rubber 80 weight parts, chloroprene rubber 20 weight parts, other formulas and operation steps, all with embodiment 1, make rubber combination product.
Embodiment 1 and comparative example 1,2 make rubber combination product performance detected result relatively in Table 2.
Table 2
Embodiment 2
Except using poly-norbornene rubber 65 weight parts, chloroprene rubber 35 weight parts, other formulas and operation steps are all with embodiment 1, and the performance of the rubber combination obtaining is tensile strength at yield 16.8Mpa, pulls apart unit elongation 493%, hardness (Shao A): 66, OI oxygen index 32.
Embodiment 3
Except using poly-norbornene rubber 60 weight parts, chloroprene rubber 40 weight parts, other formulas and operation steps are all with embodiment 1, and the performance of the rubber combination obtaining is tensile strength at yield 15.9Mpa, pulls apart unit elongation 439%, hardness (Shao A): 66, OI oxygen index 32.
Embodiment 4
By poly-norbornene rubber 65 weight parts, chloroprene rubber 35 weight parts, expanding material tetramethyl-vinylformic acid two glycerol o-benzoate 7 weight parts, 30 weight part strengthening agent high abrasion carbon black N330, weighting agent aluminium hydroxide Al (OH) 3120 weight parts, promoting agent zinc oxide 5 weight parts, magnesium oxide 4 weight parts, stearic acid 1 weight part, flame retardant decabromodiphynly oxide 10 weight parts all add in Banbury mixer mixing, melting temperature is 45 ℃～70 ℃, and mixing time is 20～40 minutes; Co-curing agent accelerant disulfide tetra methylthiuram TMTD1.5 weight part+accelerator dibenzothiazyl disulfide DM1.5 weight part+vulcanizing agent dimorpholinyl disulfide DTDM2.0 weight part adds in Banbury mixer for 5～10 minutes before mixing end, mixing together with other components.Make rubber combination product.
Comparative example 3
Except being 2 weight parts with expanding material tetramethyl-vinylformic acid two glycerol o-benzoates (oligomer ester-I), other formulas and operation steps, all with embodiment 4, make rubber combination product.
Comparative example 4
Except being 15 weight parts with expanding material tetramethyl-vinylformic acid two glycerol o-benzoates (oligomer ester-I), other formulas and operation steps, all with embodiment 4, make rubber combination product.
Comparative example 5
Except not adding expanding material tetramethyl-vinylformic acid two glycerol o-benzoates (oligomer ester-I), other formulas and operation steps, all with embodiment 4, make rubber combination product.
Embodiment 4 and comparative example 3,4,5 make rubber combination product performance detected result relatively in Table 3.
Table 3.
Embodiment 5
Except expanding material tetramethyl-vinylformic acid two glycerol o-benzoates (oligomer ester-I) are 10 weight parts, other formulas and operation steps are all with embodiment 4, the performance of the rubber combination obtaining is tensile strength at yield 16.1Mpa, pull apart unit elongation 459%, hardness (Shao A): 66, OI oxygen index 32.
Embodiment 6
Except expanding material tetramethyl-vinylformic acid two glycerol o-benzoates (oligomer ester-I) are 5 weight parts, other formulas and operation steps are all with embodiment 4, the performance of the rubber combination obtaining is tensile strength at yield 15.5Mpa, pull apart unit elongation 440%, hardness (Shao A): 66, OI oxygen index 32.
Embodiment 7
By poly-norbornene rubber 60 weight parts, chloroprene rubber 40 weight parts, expanding material tetramethyl-vinylformic acid two glycerol o-benzoate 5 weight parts, 30 weight part strengthening agent high abrasion carbon black N330, weighting agent aluminium hydroxide Al (OH) 3120 weight parts, promoting agent zinc oxide 5 weight parts, magnesium oxide 4 weight parts, stearic acid 1 weight part, flame retardant decabromodiphynly oxide 10 weight parts all add in Banbury mixer mixing, melting temperature is 45 ℃～70 ℃, and mixing time is 20～40 minutes; Co-curing agent accelerant disulfide tetra methylthiuram TMTD1.7 weight part+accelerator dibenzothiazyl disulfide DM1.7 weight part+vulcanizing agent dimorpholinyl disulfide DTDM2.2 weight part adds in Banbury mixer for 5～10 minutes before mixing end, mixing together with other components.Make rubber combination product.
Comparative example 6
Except using alone vulcanization system: vulcanization accelerator tetramethyl-thiuram disulfide TMTD1.7 weight part+vulcanizing agent dimorpholinyl disulfide DTDM2.2 weight part, other formulas and operation steps, all with embodiment 7, make rubber combination product.
Comparative example 7
Except using alone vulcanization system: vulcanization accelerator dibenzothiazyl disulfide DM1.7 weight part+vulcanizing agent dimorpholinyl disulfide DTDM2.2 weight part, other formulas and operation steps, all with embodiment 7, make rubber combination product.
Comparative example 8
Except using other vulcanization systems: accelerator CZ 1.7 weight parts+accelerant B Z1.7 weight part+vulcanizing agent DTDM2.2 weight part, other formulas and operation steps, all with embodiment 7, make rubber combination product.
Above-mentioned accelerator CZ is N-cyclohexyl-2-benzothiazole sulfonamide, and accelerant B Z is zinc dibutyl dithiocaarbamate.
Embodiment 7 and comparative example 6,7,8 make rubber combination product performance detected result relatively in Table 4.
Table 4
Embodiment 8
Except co-curing agent is Vulcanization accelerator TMTD 2.0 weight parts+altax 2.0 weight parts+vulcanizing agent DTDM2.5 weight part with vulcanization system, other formulas and operation steps are all with embodiment 7, the performance of the rubber combination obtaining is tensile strength at yield 16.9Mpa, pull apart unit elongation 452%, hardness (Shao A): 66, OI oxygen index 33.
Embodiment 9
Except co-curing agent is Vulcanization accelerator TMTD 1.5 weight parts+altax 1.5 weight parts+vulcanizing agent DTDM2.0 weight part with vulcanization system, other formulas and operation steps are all with embodiment 7, the performance of the rubber combination obtaining is tensile strength at yield 16..0Mpa, pull apart unit elongation 483%, hardness (Shao A): 66, OI oxygen index 33.
Claims (8)
1. take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body for one kind, it is characterized in that, said composition forms and to comprise that take poly-norbornene rubber and chloroprene rubber fusion blend is base mateiral, take the expanding material of tetramethyl-vinylformic acid two glycerol o-benzoates as poly-norbornene rubber and chloroprene rubber fusion blend.
2. according to claim 1ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, in weight part, poly-norbornene rubber and chloroprene rubber fusion blending ratio are: 65-60/40-35.
3. according to claim 1ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, the weight sum of poly-norbornene rubber and chloroprene rubber of take is 100 weight parts, and the consumption of described tetramethyl-vinylformic acid two glycerol o-benzoate expanding materials is 5-10 weight part.
4. according to claim 1ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, this rubber combination be take accelerant disulfide tetra methylthiuram TMTD+ accelerator dibenzothiazyl disulfide DM+ vulcanizing agent dimorpholinyl disulfide DTDM be co-curing agent with vulcanization system, the weight sum of poly-norbornene rubber and chloroprene rubber of take is 100 weight parts, Vulcanization accelerator TMTD consumption is 1.5～2.0 weight parts, altax consumption is 1.5～2.0 weight parts, and vulcanizing agent DTDM consumption is 2.0～2.5 weight parts.
5. according to claim 4ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, the weight sum of poly-norbornene rubber and chloroprene rubber of take is 100 weight parts, Vulcanization accelerator TMTD consumption is 1.7 weight parts, altax consumption is 1.7 weight parts, and vulcanizing agent DTDM consumption is 2.2 weight parts.
6. according to claim 4ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, the component of said composition also comprises strengthening agent, weighting agent, promoting agent and flame retardant.
7. according to claim 6ly take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body, it is characterized in that, described strengthening agent is that high abrasion furnace carbon black N330, described weighting agent are that aluminium hydroxide, described promoting agent are that stearic acid, zinc oxide and magnesium oxide, described flame retardant are decabromodiphynly oxide.
8. the compounding process of take the fire-retardant highly damping rubber composition that poly-norbornene rubber is main body described in a claim 1-6, it is characterized in that, by the component of said composition, comprise that poly-norbornene rubber, chloroprene rubber, expanding material tetramethyl-vinylformic acid two glycerol o-benzoates, strengthening agent, weighting agent, promoting agent, flame retardant all add in Banbury mixer mixing, melting temperature is 45 ℃～70 ℃, and mixing time is 20～40 minutes; Co-curing agent accelerant disulfide tetra methylthiuram TMTD+ accelerator dibenzothiazyl disulfide DM+ vulcanizing agent dimorpholinyl disulfide DTDM adds in Banbury mixer for 5～10 minutes before mixing end, mixing together with other components.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104694155A (en) * | 2013-12-05 | 2015-06-10 | 窦洪波 | Ultrasonic resonance desulfurization electrochemical technology reactor and reaction technology thereof |
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| CN101747595A (en) * | 2008-12-03 | 2010-06-23 | 娄颖 | Composition for manufacturing low-hardness rubber material |
| CN103724908A (en) * | 2013-12-31 | 2014-04-16 | 长城汽车股份有限公司 | Low-hardness high-damping rubber composition and preparation method thereof |
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| KR100356584B1 (en) * | 1995-02-22 | 2003-03-19 | 금호산업 주식회사 | Polynorbornene-based rubber composition for filler of tire tread rubber |
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| CN101205336A (en) * | 2006-12-18 | 2008-06-25 | 上海华向橡胶制品有限公司 | Composition for manufacturing low-hardness rubber material |
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| CN104694155B (en) * | 2013-12-05 | 2017-10-10 | 年雪丽 | Ultrasonic resonance desulfurization electrification technology reactor and reaction process |
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