CN103408855A - Rubber composite containing graphene oxide - Google Patents
Rubber composite containing graphene oxide Download PDFInfo
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- CN103408855A CN103408855A CN2013103817842A CN201310381784A CN103408855A CN 103408855 A CN103408855 A CN 103408855A CN 2013103817842 A CN2013103817842 A CN 2013103817842A CN 201310381784 A CN201310381784 A CN 201310381784A CN 103408855 A CN103408855 A CN 103408855A
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Abstract
The invention relates to a rubber composite containing graphene oxide. The rubber composite is characterized by comprising the following raw materials in parts by weight: 100 parts of chlorosulfonated polyethylene, 10-15 parts of ethylene-vinyl acetate rubber (EVM), 20-25 parts of hydrogenated butadiene-acrylonitrile rubber (HNBR), 0.5-5 parts of graphene oxide, 30-70 parts of hard carbon black with mean grain size of 15-25nm, 1-10 parts of dioctyl sebacate (DOS), 3-6 parts of zinc oxide, 3-6 parts of stearic acid, 0.5-4 parts of N,N-nickel dibutyl dithiocarbamate, 1-4 parts of dipentamethylenethiuram hexasulfide, 0.5-4 parts of PbO and 1-6 parts of insoluble sulfur. The rubber composite has the beneficial effects that by using the chlorosulfonated polyethylene, EVM and HNBR with low acrylonitrile content simultaneously, the rubber composite perfectly balances fuel oil resistance and low temperature resistance, distorts 2000 cycles under the low temperature condition of minus 55 DEG C, is free of cracks and distortion on the surface, and is suitable for alpine and low-temperature regions.
Description
Technical field
The present invention relates to a kind of graphene oxide rubber composite that contains.
Background technology
The stress maximum region of radial is tire shoulder and bead region, especially when overload is more serious, tyre bead is except bearing internal pressure stress, braking moment, sideslip and centrifugal force and wheel rim interference power etc., also because the body cord meridian is arranged, curtain cloth layer is few, the carcass softness, cause tire to be in always and repeatedly to deflect among state in the process of moving, under such stressed condition, the Steel Traveler tyre bead is stressed very large, makes carcass ply end points position easily produce disengaging.Due to the sidewall softness, while especially running at high speed in motion, can increase unstable, so tyre bead portion must strengthen greatly.Triangular shape core glue (abbreviation triangle rubber) is the important parts of tyre bead portion, be positioned at the Steel Traveler upper end, play a part to fill, locate, meet with stresses, not only to improving the distribution of radial lateral rigidity, play an important role, all even subduing property is good with sidewall district rigid-flexibility transition simultaneously.The performance requriements of triangle rubber is: good rigidity (high rigidity, high-modulus), ageing-resistant performance, extrusion performance, surface adhering performance, the suitable work in-process property endured.
High consumption carbon black coordinates with high consumption sulphur the main stream approach that remains the triangle rubber preparation field, although yet the carbon black of high consumption and sulfur consumption can improve the Young's modulus of triangle rubber effectively, but also can obviously improve the loss tangent of material, like this in vehicle traveling process, triangle rubber easily generates heat, its thermal fatigue can have a strong impact on the weather resistance of tire, reduces the work-ing life of tire.In addition, the carbon black dispersion difficulty of too high consumption, the processing viscosity of sizing material is high, and extrusion performance is poor, even like this, uses separately the degree of carbon black raising rubber vulcanizate module also limited, can't meet the requirement of the necessary more high-modulus of tyre triangular glue and hardness.
Graphite is a kind of common Nano filling, has the laminated structure of similar clay, under the state of peeling off, has very high shape factor, and graphite is one of material that specific tenacity is the highest.Use graphite-filled rubber to prepare matrix material and can obviously improve hardness and modulus.In Chinese patent application " tyre triangular glue rubber nano composite material " (application number 201210212113.9), use expanded graphite and hard (carbon) black and use and be filled in rubber matrix the rubber composite of preparing high rigidity, high-modulus.But, because the extent of exfoliation of expanded graphite is inadequate, and the dispersion of expanded graphite in rubber matrix and poor with the interfacial adhesion of matrix, make in the situation that expanded graphite to fill the more matrix material modulus of umber still limited with hardness raising degree.
Summary of the invention
The present invention has designed a kind of graphene oxide rubber composite that contains, the technical problem of its solution is that existing tyre triangular glue is inadequate by the extent of exfoliation due to expanded graphite in rubber nano composite material, and the dispersion of expanded graphite in rubber matrix and poor with the interfacial adhesion of matrix, make in the situation that expanded graphite to fill the more matrix material modulus of umber still limited with hardness raising degree.
In order to solve the technical problem of above-mentioned existence, the present invention has adopted following scheme:
A kind of graphene oxide rubber composite that contains, it is characterized in that: the quality proportioning of its feed composition is: 100 parts of chlorosulfonated polyethylenes, 10-15 part ethylene-vinyl acetate rubber (EVM), 20-25 part hydrogenated nitrile-butadiene rubber (HNBR), graphene oxide 0.5-5 part, median size is hard (carbon) black 30-70 part of 15-25nm, dioctyl sebacate (DOS) 1-10 part, zinc oxide 3-6 part, stearic acid 3-6 part, N, N-nickel dibutyl dithiocarbamate 0.5-4 part, six sulfuration di-penta methylene thiuram 1-4 part, PbO0.5-4 part and insoluble sulfur 1-6 parts.
Further, the lamellar spacing 1-2nm of graphene oxide, width 100-500nm.
Further, in ethylene-vinyl acetate rubber (EVM), the vinyl acetate massfraction is 60%-68%.
Further, in hydrogenated nitrile-butadiene rubber (HNBR), the massfraction of vinyl cyanide is 20-22%.
Hard (carbon) black is selected the product of the following trade mark: N115, N220, N234, N330 or N375, and median size is between 11-30nm, and reinforcing effect is good.
A kind of making method that contains the graphene oxide rubber composite: comprise the following steps: successively
Step 1, the graphene oxide powder is dispersed in deionized water in water, mass concentration is 0.1-0.4mg/mL, uses the ultrasonic echography 30-60min of power as 500-1000W, obtains the suspension of graphene oxide;
Step 2, chlorosulfonated polyethylene is joined in the suspension that step 1 obtains graphene oxide after forming emulsion blending and proceeds ultrasonication 20min, through flocculation, washing and dry, finally make rubber master batch successively;
Step 3, by the rubber master batch that makes in step 2 and ethylene-vinyl acetate rubber (EVM), hydrogenated nitrile-butadiene rubber (HNBR), graphene oxide properties-correcting agent, activator zinc oxide and stearic mixture, anti-aging agent N, N-nickel dibutyl dithiocarbamate, hard (carbon) black, softening agent dioctyl sebacate (DOS), vulcanization accelerator six sulfuration di-penta methylene thiurams, vulcanizing agent PbO and insoluble sulfur mix, mixing even, through sulfuration, obtain the tyre triangular glue rubber composite.
Further, the flocculation in step 2 can be adopted latex and graphene oxide mixture are joined to 0.5～1.5wt%CaCl
2In the aqueous solution, carry out.
Further, in step 3, graphene oxide properties-correcting agent used is isocyanic acid propyl-triethoxysilicane (IPTS) or APTES (KH550), and the mass ratio of graphene oxide properties-correcting agent and graphene oxide is 1:10-1:2.
With respect to original graphite, graphene oxide lamella extent of exfoliation after oxidation is higher, has very large specific surface area, the graphene oxide that adds minute quantity to peel away through ultrasonication in rubber composite, can significantly improve hardness and the modulus of matrix material, the triangle rubber position is strengthened greatly.
In addition, graphene oxide lamella and carbon black particle are isolated mutually, both can hinder the Second Aggregation of graphite, can strengthen the dispersion of carbon black again, add that graphene oxide fills umber seldom and the minimizing of carbon black loading, can significantly improve Drawing abillity, reduce dynamic heat build up, improve the thermal fatigue of tire, improve the work-ing life of tire.
Graphene oxide properties-correcting agent is with the isocyanic acid propyl-triethoxysilicane (IPTS) of isocyanide ester group or with the APTES (KH550) of amino group, the isocyanide ester group can react with carboxyl and the hydroxyl on graphene oxide surface, amino group can react with epoxy group(ing) and the carboxyl on graphene oxide surface, complete in-situ modified process, after modification, can improve the dispersion of graphene oxide in rubber matrix, strengthen the interfacial adhesion effect with matrix.When the mass ratio of properties-correcting agent and graphene oxide was 1:10～1:2, modified effect was best.
In addition, the maximum characteristics of emulsion blending are to take full advantage of the form that most of commercial rubber all possesses latex, can prepare easily the rubber nano composite material of different matrix, can also extend to the polymeric matrix that other possesses emulsion form.
Technique by emulsion blending, graphene oxide is fully stripped and is dispersed into many nano level graphite flake layers with larger shape factor and specific surface area, be dispersed in rubber matrix, bound rubber macromole backbone and good processibility, even in the situation that amount of filler is less, the performance of materials is greatly improved than its corresponding macroscopic view or micron order material.
This contains the graphene oxide rubber composite and has following beneficial effect:
(1) the present invention adopts the HNBR of chlorosulfonated polyethylene, EVM and low acrylonitrile content and uses, perfectly balance fuel oil resistance and resistance to low temperature, in 2000 cycles of distortion under-55 ℃ of cold condition, material surface flawless and twisted phenomena, be applicable to high and cold low temp area and use.
(2) the present invention, by graphene oxide and hard (carbon) black and with being filled in rubber matrix, greatly improves hardness and the modulus of rubber composite, and has good processing characteristics.
(3) the present invention first makes rubber master batch by graphene oxide suspension and rubber latex emulsion blending that minute quantity is peeled away through ultrasonication, then after in-situ modified, also use with hard (carbon) black, prepare the rubber nano composite material of high rigidity and high-modulus, has good processing characteristics, and can obviously reduce the dynamic heat build up of matrix material, improve the work-ing life of tire.
Embodiment
Below in conjunction with embodiment, the present invention will be further described:
Embodiment 1: a kind of graphene oxide rubber composite that contains, the mass fraction of each component is: 100 parts of chlorosulfonated polyethylenes, 10 parts of ethylene-vinyl acetate rubber (EVM), 20 parts of hydrogenated nitrile-butadiene rubbers (HNBR), 3 parts of graphene oxides, hard (carbon) black N33060 part, 4 parts of dioctyl sebacates (DOS), 2 parts of stearic acid, 5 parts, zinc oxide, 5 parts of insoluble sulfurs, anti-aging agent N, 3 parts of N-nickel dibutyl dithiocarbamates, vulcanizing agent PbO2 part, 3 parts of vulcanization accelerator six sulfuration di-penta methylene thiurams.
Composite material preparation process: the graphene oxide powder is dispersed in deionized water in water, and mass concentration is 0.4mg/mL, uses the ultrasonic echography 45min of power as 750W, obtains the suspension of graphene oxide.100 parts of chlorosulfonated polyethylenes are joined to ultrasonication 15min in this suspension system, join 2wt%CaCl
2In the aqueous solution, through flocculation, washing and dry, make rubber master batch.By female limb with 10 parts of ethylene-vinyl acetate rubber (EVM), 20 parts of hydrogenated nitrile-butadiene rubbers (HNBR), graphene oxide properties-correcting agent (graphene oxide quality 10%), activator zinc oxide and stearic mixture, anti-aging agent N, the N-nickel dibutyl dithiocarbamate, hard (carbon) black, softening agent dioctyl sebacate (DOS), vulcanization accelerator six sulfuration di-penta methylene thiurams, vulcanizing agent PbO and insoluble sulfur mix, mixing even, molded vulcanization 45min on 25 tons of vulcanizing presses, curing temperature is 151 ℃, obtain the tyre triangular glue rubber composite.Its mechanical property is in Table 1.
Embodiment 2: a kind of graphene oxide rubber composite that contains, the mass fraction of each component is: 100 parts of chlorosulfonated polyethylenes, 15 parts of ethylene-vinyl acetate rubber (EVM), 25 parts of hydrogenated nitrile-butadiene rubbers (HNBR), 0.5 part of graphene oxide, hard (carbon) black N33060 part, 4 parts of dioctyl sebacates (DOS), 3 parts of stearic acid, 6 parts, zinc oxide, 2 parts of insoluble sulfurs, anti-aging agent N, 3 parts of N-nickel dibutyl dithiocarbamates, vulcanizing agent PbO4 part, 3 parts of vulcanization accelerator six sulfuration di-penta methylene thiurams.
Composite material preparation process: the graphene oxide powder is dispersed in deionized water in water, and mass concentration is 0.4mg/mL, uses the ultrasonic echography 45min of power as 750W, obtains the suspension of graphene oxide.100 parts of chlorosulfonated polyethylenes are joined to ultrasonication 15min in this suspension system, join 2wt%CaCl
2In the aqueous solution, through flocculation, washing and dry, make rubber master batch.By rubber master batch with 15 parts of ethylene-vinyl acetate rubber (EVM), 25 parts of hydrogenated nitrile-butadiene rubbers (HNBR), graphene oxide properties-correcting agent (graphene oxide quality 10%), activator zinc oxide and stearic mixture, anti-aging agent N, the N-nickel dibutyl dithiocarbamate, hard (carbon) black, softening agent dioctyl sebacate (DOS), vulcanization accelerator six sulfuration di-penta methylene thiurams, vulcanizing agent PbO and insoluble sulfur mix, mixing even, molded vulcanization 40min on 25 tons of vulcanizing presses, curing temperature is 155 ℃, obtain the tyre triangular glue rubber composite.Its mechanical property is in Table 1.
Embodiment 3: a kind of graphene oxide rubber composite that contains, the mass fraction of each component is: 100 parts of chlorosulfonated polyethylenes, 12 parts of ethylene-vinyl acetate rubber (EVM), 22 parts of hydrogenated nitrile-butadiene rubbers (HNBR), 5 parts of graphene oxides, hard (carbon) black N33050 part, 5 parts of dioctyl sebacates (DOS), 3 parts of stearic acid, 6 parts, zinc oxide, 6 parts of insoluble sulfurs, anti-aging agent N, 3 parts of N-nickel dibutyl dithiocarbamates, vulcanizing agent PbO4 part, 3 parts of vulcanization accelerator six sulfuration di-penta methylene thiurams.
Composite material preparation process: the graphene oxide powder is dispersed in deionized water in water, and mass concentration is 0.4mg/mL, uses the ultrasonic echography 45min of power as 750W, obtains the suspension of graphene oxide.100 parts of chlorosulfonated polyethylenes are joined to ultrasonication 15min in this suspension system, join 2wt%CaCl
2In the aqueous solution, through flocculation, washing and dry, make rubber master batch.By rubber master batch with 100 parts of chlorosulfonated polyethylenes, 12 parts of ethylene-vinyl acetate rubber (EVM), 22 parts of hydrogenated nitrile-butadiene rubbers (HNBR), graphene oxide properties-correcting agent (graphene oxide quality 10%), activator zinc oxide and stearic mixture, anti-aging agent N, the N-nickel dibutyl dithiocarbamate, hard (carbon) black, softening agent dioctyl sebacate (DOS), vulcanization accelerator six sulfuration di-penta methylene thiurams, vulcanizing agent PbO and insoluble sulfur mix, mixing even, molded vulcanization 50min on 25 tons of vulcanizing presses, curing temperature is 150 ℃, obtain the tyre triangular glue rubber composite.Its mechanical property is in Table 1.
The contrast of table 1 embodiment of the present invention mechanical property
As can be seen from Table 1, use minute quantity graphene oxide and carbon black use, hardness, stress at definite elongation, modulus all have obvious lifting, and dynamic loss factor reduces, and dynamic heat build up reduces.In 2000 cycles of distortion under-55 ℃ of cold condition, material surface flawless and twisted phenomena, be applicable to high and cold low temp area and use.
The above has carried out exemplary description to the present invention in conjunction with the embodiments; obvious realization of the present invention is not subject to the restrictions described above; as long as the various improvement of having adopted method design of the present invention and technical scheme to carry out; or without improving, design of the present invention and technical scheme are directly applied to other occasion, all in protection scope of the present invention.
Claims (4)
1. one kind contains the graphene oxide rubber composite, it is characterized in that: the quality proportioning of its feed composition is: 100 parts of chlorosulfonated polyethylenes, 10-15 part ethylene-vinyl acetate rubber (EVM), 20-25 part hydrogenated nitrile-butadiene rubber (HNBR), graphene oxide 0.5-5 part, median size is hard (carbon) black 30-70 part of 15-25nm, dioctyl sebacate (DOS) 1-10 part, zinc oxide 3-6 part, stearic acid 3-6 part, N, N-nickel dibutyl dithiocarbamate 0.5-4 part, six sulfuration di-penta methylene thiuram 1-4 part, PbO0.5-4 part and insoluble sulfur 1-6 parts.
2. contain according to claim 1 the graphene oxide rubber composite, it is characterized in that: the lamellar spacing 1-2nm of graphene oxide, width 100-500nm.
3. contain according to claim 1 the graphene oxide rubber composite, it is characterized in that: in ethylene-vinyl acetate rubber (EVM), the vinyl acetate massfraction is 60%-70%.
4. contain according to claim 1 the graphene oxide rubber composite, it is characterized in that: in hydrogenated nitrile-butadiene rubber (HNBR), the massfraction of vinyl cyanide is 20-25%.
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| CN104672647A (en) * | 2015-01-29 | 2015-06-03 | 柳州市中配橡塑配件制造有限公司 | Rubber for high-speed tire |
| CN104672643A (en) * | 2015-01-29 | 2015-06-03 | 柳州市中配橡塑配件制造有限公司 | Rubber for truck tire |
| CN104672645A (en) * | 2015-01-29 | 2015-06-03 | 柳州市中配橡塑配件制造有限公司 | Rubber for truck bumper |
| WO2017139115A1 (en) * | 2016-02-10 | 2017-08-17 | Cabot Corporation | Elastomer compounds |
| CN107417997A (en) * | 2017-09-29 | 2017-12-01 | 徐州九鼎机电总厂 | A kind of rubber composite of high content graphene |
| US10204715B2 (en) | 2016-03-31 | 2019-02-12 | Schlumberger Technology Corporation | Submersible power cable |
| CN109679161A (en) * | 2018-11-27 | 2019-04-26 | 北京化工大学 | A kind of carboxy nitrile rubber/stannic oxide/graphene nano composite material and preparation method obstructing hazardous chemical solvent |
| US10443339B2 (en) | 2016-06-23 | 2019-10-15 | Schlumberger Technology Corporation | Elastomeric materials |
| CN112409959A (en) * | 2019-08-20 | 2021-02-26 | 广东顺德三和化工有限公司 | Chlorosulfonated polyethylene rubber sealant and preparation method thereof |
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|---|---|---|---|---|
| CN104672647A (en) * | 2015-01-29 | 2015-06-03 | 柳州市中配橡塑配件制造有限公司 | Rubber for high-speed tire |
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| US10443339B2 (en) | 2016-06-23 | 2019-10-15 | Schlumberger Technology Corporation | Elastomeric materials |
| CN107417997A (en) * | 2017-09-29 | 2017-12-01 | 徐州九鼎机电总厂 | A kind of rubber composite of high content graphene |
| CN109679161A (en) * | 2018-11-27 | 2019-04-26 | 北京化工大学 | A kind of carboxy nitrile rubber/stannic oxide/graphene nano composite material and preparation method obstructing hazardous chemical solvent |
| CN109679161B (en) * | 2018-11-27 | 2020-07-24 | 北京化工大学 | Carboxyl nitrile rubber/graphene oxide nanocomposite capable of blocking hazardous chemical solvents and preparation method thereof |
| CN112409959A (en) * | 2019-08-20 | 2021-02-26 | 广东顺德三和化工有限公司 | Chlorosulfonated polyethylene rubber sealant and preparation method thereof |
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Application publication date: 20131127 |