CN105037830A - High-strength low-heat-generation composite material and preparation method thereof - Google Patents
High-strength low-heat-generation composite material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a rubber composite material in the field of function materials, in particular to a high-strength low-heat-generation composite material and a preparation method thereof. The high-strength low-heat-generation composite material is prepared in the mode that natural rubber dry rubber, reduced graphene oxide masterbatch, multi-walled carbon nanotube masterbatch, rubber additives and carbon black are organically combined in a mechanical blending method. The reduced graphene oxide masterbatch is prepared from reduced graphene oxide and natural latex through an in-situ reduction method and a latex co-precipitation method. The multi-walled carbon nanotube masterbatch is prepared from multi-walled carbon nanotubes and natural latex through a latex co-precipitation method. The reduced graphene oxide and the multi-walled carbon nanotubes are coated with the natural rubber latex, the dispersity of the reduced graphene oxide and the multi-walled carbon nanotubes is improved, then the interaction of the reduced graphene oxide, the multi-walled carbon nanotubes and the rubber is enhanced through crosslinking in the sulfuration process, and consequently the novel high-strength low-heat-generation composite material is prepared.
Description
Technical field
The present invention relates to the rubber composite of field of functional materials, specifically a kind of high strength low-heat-generation matrix material and preparation method thereof.
Background technology
Along with the development of modern science and technology and the progress of industrial civilization, various vehicle, the application of the automobile that especially running speed is high, weight-carrying capacity is large etc. is increasing.In order to improve the mechanical property of rubber tyre, meeting the needs of practical application, needing in rubber matrix to add carbon black as strengthening agent, but black-reinforced agent is while raising cross-linked rubber mechanical property, causes the compression heat generation of cross-linked rubber obviously to become large.Compression heat generation is very large for needing the use properties of the rubber item of repeated deformation to affect, because rubber is the poor conductor of heat, compression heat generation is too large, rubber item meeting rapid temperature increases, temperature raises and not only accelerates the thermo-oxidative ageing of rubber, and may the too high destruction causing rubber item of Yin Wendu, and at high temperature delamination or bulge easily appear in the tyre surface of tire and body piles, can cause time serious and get rid of tyre surface, in travelling summer, automotive tire burst is exactly a typical example.Except selecting the rubber raw materials of low-heat-generation, obtaining high strength, low-heat-generation rubber composite by formula, process optimization is Materials science important scientific problems urgently to be resolved hurrily.
In addition, along with the increasingly stringent of reducing emission of carbon dioxide policies and regulations and the increasingly in short supply of petroleum resources, how reducing the focus that vehicle fuel consume becomes automobile industry and user's concern, improve mechanical property, reducing heat-dissipating is one of important measures reducing vehicle fuel consume.
Summary of the invention
The present invention aims to provide and a kind ofly reduces compression fatigue heat-dissipating and a kind of high strength low-heat-generation matrix material that can improve mechanical property and preparation method thereof.
The present invention is achieved by the following technical solutions: a kind of high strength low-heat-generation matrix material, and it is prepared from by the combination of mechanical blending method by the dry glue of natural rubber, redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch, rubber ingredients and carbon black; Described redox graphene rubber master batch is that graphene oxide and natural rubber latex are prepared by in-situ reducing, latex coprecipitation method, and described multi-walled carbon nano-tubes rubber master batch is that multi-walled carbon nano-tubes and natural rubber latex are prepared by latex coprecipitation method.
High strength low-heat-generation matrix material of the present invention, not only can reduce compression fatigue heat-dissipating, and greatly can improve mechanical property.Therefore, the present invention is from the angle of composite materials, latex coprecipitation method, local reduction way, mechanical blending method are organically combined, by multi-walled carbon nano-tubes, redox graphene, carbon black and natural rubber organic composite, prepare the high strength low-heat-generation multi-walled carbon nano-tubes/redox graphene/carbon black/native rubber composite material having each component advantage concurrently.
Preferably, in the dry glue of described natural rubber, redox graphene rubber master batch natural rubber latex butt, many be 2:1:1 than the mass ratio of the butt of natural rubber latex in carbon nanotube rubber master batch.In the preparation of redox graphene rubber master batch, the mass ratio of the butt of graphene oxide and natural rubber latex is 1 ~ 3:50.In the preparation of multi-walled carbon nano-tubes rubber master batch, the mass ratio of the butt of multi-walled carbon nano-tubes and natural rubber latex is 1 ~ 2:50.
Further, described rubber ingredients comprise activator, anti-aging agent, promotor and vulcanizing agent.
In addition, the invention provides a kind of preparation method of this matrix material, the steps include:
1. the preparation of redox graphene rubber master batch:
Joined in graphene oxide by aequum natural rubber latex, and add hydrazine hydrate, magnetic agitation 0.5 ~ 1h makes it mix, and graphene oxide in-situ reducing is become Graphene, and dripping concentration is the CaCl of 10-20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain redox graphene rubber master batch;
2. the preparation of multi-walled carbon nano-tubes rubber master batch:
Join in natural rubber latex by the multi-walled carbon nano-tubes of aequum, magnetic agitation 0.5 ~ 1h makes it mix, and dripping concentration is the CaCl of 10-20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain multi-walled carbon nano-tubes rubber master batch;
3. the preparation of matrix material:
The dry glue of natural rubber taking aequum joins Banbury mixer banburying 2 ~ 5min, then adds redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch successively, respectively banburying 1 ~ 2min; Add activator, anti-aging agent and carbon black, respectively banburying 5min; Rubber after banburying is mixing in two roller mill, add promotor, vulcanizing agent, thin-pass after bag roller heap glue, clot, play triangle bag and mix rear lower roll, acquisition high strength low-heat-generation matrix material.
In above-mentioned preparation method, the object of hydrazine hydrate is in-situ reducing graphene oxide, as long as therefore its add-on can redox graphene, this add-on is that those skilled in the art can control realization.
Further, that described activator adopts is SA and ZnO, and that described anti-aging agent adopts is RD and 4010NA, and that described promotor adopts is NOBS, and that described vulcanizing agent adopts is S.
Also have, the mass ratio of activator SA, ZnO and the dry glue of total rubber is 2:5:100, the mass ratio of the dry glue of anti-aging agent RD, 4010NA and total rubber is 1:1:100, the mass ratio of accelerant NOBS, vulcanizing agent S and the dry glue of total rubber is 1:1:50, and the mass ratio of the total mass of graphene oxide, multi-walled carbon nano-tubes and carbon black and the dry glue of total rubber is 40:100.The dry glue of described total rubber is the butt of natural rubber latex and the summation of the dry glue of natural rubber in the butt of natural rubber latex in redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch.
The redox graphene adopted in the present invention has the feature such as mechanical property, high thermal conductivity, high anisotropy, high-specific surface area of superelevation, multi-walled carbon nano-tubes has high intensity, greatly toughness and the feature such as density is less, but redox graphene, multi-walled carbon nano-tubes all exist the problem of not easily good distribution.The present invention is by adopting the coated redox graphene of natural rubber latex, multi-walled carbon nano-tubes, improve the dispersiveness of redox graphene, multi-walled carbon nano-tubes, and then by the crosslinked interaction increasing redox graphene, multi-walled carbon nano-tubes and rubber during sulfuration, thus prepare high strength, low-heat-generation advanced composite material.By the relative content of controlling functions filler, reinforcing filler, matrix, intensity and the thermogenesis performance of product effectively can be regulated and controled.The features such as matrix material of the present invention is with low cost, preparation technology simple, fillers dispersed degree is high, comprehensive mechanical property is excellent, dynamic compression heat build-up is few, have important application prospect in tire, vibroshock field.
Experiment: matrix material of the present invention and common native rubber composite material performance comparison
The preparation method of what matrix material of the present invention adopted is matrix material of the present invention, 3., the processing parameter that both adopt and performance comparison are in table 1 for the step that what common native rubber composite material adopted is in composite material and preparation method thereof of the present invention.
Table 1
Accompanying drawing explanation
Fig. 1 is the high strength low-heat-generation matrix material of embodiment 1 in embodiment, embodiment 2 and embodiment 3 preparation and the stress-strain curve comparison diagram of common native rubber composite material.
Fig. 2 is the high strength low-heat-generation matrix material of embodiment 1 in embodiment, embodiment 2 and embodiment 3 preparation and the compression fatigue heat-dissipating cylindricality comparison diagram of common native rubber composite material.
Embodiment
Embodiment 1
A kind of high strength low-heat-generation matrix material, the step of its preparation method is:
1. the preparation of redox graphene rubber master batch:
Joined in 0.5g graphene oxide by natural rubber latex containing 25g butt, and add hydrazine hydrate, magnetic agitation 0.5h makes it mix, and graphene oxide in-situ reducing is become Graphene, and dripping concentration is the CaCl of 10%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain redox graphene rubber master batch;
2. the preparation of multi-walled carbon nano-tubes rubber master batch:
Joined by 0.5g multi-walled carbon nano-tubes in the natural rubber latex containing 25g butt, magnetic agitation 1h makes it mix, and dripping concentration is the CaCl of 20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain multi-walled carbon nano-tubes rubber master batch;
3. the preparation of matrix material:
Take the dry glue of 50g natural rubber and join Banbury mixer banburying 2min, then add redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch successively, respectively banburying 1min; Add 2g activator SA, 5gZnO, 1g anti-aging agent RD, 1g4010NA and 39gN330, respectively banburying 5min; Rubber after banburying is mixing in two roller mill, add 2g accelerant NOBS, 2g vulcanizing agent S, thin-pass after bag roller heap glue, clot, play triangle bag and mix rear lower roll, acquisition high strength low-heat-generation matrix material.
Its tensile strength is 24.13MPa, and compression fatigue heat-dissipating is 10 DEG C, and compared with the native rubber composite material only having 40gN330 to fill with same technique, tensile strength improves 16%, and compression fatigue heat-dissipating reduces 16.7%.
Embodiment 2
A kind of high strength low-heat-generation matrix material, the step of its preparation method is:
1. the preparation of redox graphene rubber master batch:
Joined in 1g graphene oxide by natural rubber latex containing 25g butt, and add hydrazine hydrate, magnetic agitation 0.8h makes it mix, and graphene oxide in-situ reducing is become Graphene, and dripping concentration is the CaCl of 15%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain redox graphene rubber master batch;
2. the preparation of multi-walled carbon nano-tubes rubber master batch:
Joined by 0.8g multi-walled carbon nano-tubes in the natural rubber latex containing 25g butt, magnetic agitation 0.5h makes it mix, and dripping concentration is the CaCl of 10%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain multi-walled carbon nano-tubes rubber master batch;
3. the preparation of matrix material:
Take the dry glue of 50g natural rubber and join Banbury mixer banburying 4min, then add redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch successively, respectively banburying 2min; Add 2g activator SA, 5gZnO, 1g anti-aging agent RD, 1g4010NA and 38.2gN330, respectively banburying 5min; Rubber after banburying is mixing in two roller mill, add 2g accelerant NOBS, 2g vulcanizing agent S, thin-pass after bag roller heap glue, clot, play triangle bag and mix rear lower roll, acquisition high strength low-heat-generation matrix material.
Its tensile strength is 27.26MPa, and compression fatigue heat-dissipating is 11 DEG C, and compared with the native rubber composite material only having 40gN330 to fill with same technique, tensile strength improves 31%, and compression fatigue heat-dissipating reduces 8%.
Embodiment 3
A kind of high strength low-heat-generation matrix material, the step of its preparation method is:
1. the preparation of redox graphene rubber master batch:
Joined in 1.5g graphene oxide by natural rubber latex containing 25g butt, and add hydrazine hydrate, magnetic agitation 1h makes it mix, and graphene oxide in-situ reducing is become Graphene, and dripping concentration is the CaCl of 20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain redox graphene rubber master batch;
2. the preparation of multi-walled carbon nano-tubes rubber master batch:
Joined by 1g multi-walled carbon nano-tubes in the natural rubber latex containing 25g butt, magnetic agitation 0.8h makes it mix, and dripping concentration is the CaCl of 15%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain multi-walled carbon nano-tubes rubber master batch;
3. the preparation of matrix material:
Take the dry glue of 50g natural rubber and join Banbury mixer banburying 5min, then add redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch successively, respectively banburying 1min; Add 2g activator SA, 5gZnO, 1g anti-aging agent RD, 1g4010NA and 37.5gN330, respectively banburying 5min; Rubber after banburying is mixing in two roller mill, add 2g accelerant NOBS, 2g vulcanizing agent S, thin-pass after bag roller heap glue, clot, play triangle bag and mix rear lower roll, acquisition high strength low-heat-generation matrix material.
Its tensile strength is 28.47MPa, and compression fatigue heat-dissipating is 11.2 DEG C, and compared with the native rubber composite material only having 40gN330 to fill with same technique, tensile strength improves 36%, and compression fatigue heat-dissipating reduces 7%.
Claims (6)
1. a high strength low-heat-generation matrix material, is characterized in that, it is prepared from by the combination of mechanical blending method by the dry glue of natural rubber, redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch, rubber ingredients and carbon black; Described redox graphene rubber master batch is that graphene oxide and natural rubber latex are prepared by in-situ reducing, latex coprecipitation method, and described multi-walled carbon nano-tubes rubber master batch is that multi-walled carbon nano-tubes and natural rubber latex are prepared by latex coprecipitation method.
2. a kind of high strength low-heat-generation matrix material according to claim 1, it is characterized in that, in the dry glue of described natural rubber, redox graphene rubber master batch natural rubber latex butt, many be 2:1:1 than the mass ratio of the butt of natural rubber latex in carbon nanotube rubber master batch.
3. a kind of high strength low-heat-generation matrix material according to claim 2, is characterized in that, in the preparation of redox graphene rubber master batch, the mass ratio of the butt of graphene oxide and natural rubber latex is 1 ~ 3:50.
4. a kind of high strength low-heat-generation matrix material according to claim 2, is characterized in that, in the preparation of multi-walled carbon nano-tubes rubber master batch, the mass ratio of the butt of multi-walled carbon nano-tubes and natural rubber latex is 1 ~ 2:50.
5. a kind of high strength low-heat-generation matrix material according to claim 3 or 4, it is characterized in that, described rubber ingredients comprise activator, anti-aging agent, promotor and vulcanizing agent.
6. a kind of high strength low-heat-generation matrix material according to claim 5, it is characterized in that, the step of its preparation method is:
1. the preparation of redox graphene rubber master batch:
Joined in graphene oxide by aequum natural rubber latex, and add hydrazine hydrate, magnetic agitation 0.5 ~ 1h makes it mix, and graphene oxide in-situ reducing is become Graphene, and dripping concentration is the CaCl of 10-20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain redox graphene rubber master batch;
2. the preparation of multi-walled carbon nano-tubes rubber master batch:
Join in natural rubber latex by the multi-walled carbon nano-tubes of aequum, magnetic agitation 0.5 ~ 1h makes it mix, and dripping concentration is the CaCl of 10-20%
2as flocculation agent breakdown of emulsion, and in 70 DEG C of vacuum-dryings after cohesion, obtain multi-walled carbon nano-tubes rubber master batch;
3. the preparation of matrix material:
The dry glue of natural rubber taking aequum joins Banbury mixer banburying 2 ~ 5min, then adds redox graphene rubber master batch, multi-walled carbon nano-tubes rubber master batch successively, respectively banburying 1 ~ 2min; Add activator, anti-aging agent and carbon black, respectively banburying 5min; Rubber after banburying is mixing in two roller mill, add promotor, vulcanizing agent, thin-pass after bag roller heap glue, clot, play triangle bag and mix rear lower roll, acquisition high strength low-heat-generation matrix material.
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| CN105694130A (en) * | 2016-04-10 | 2016-06-22 | 北京化工大学 | Preparation method of high-electric-conductivity graphene/natural rubber nano-composite |
| CN106009072A (en) * | 2016-06-17 | 2016-10-12 | 山东容奈材料设计有限公司 | Raw material composition for tire and preparation method for tire |
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| CN108713038A (en) * | 2016-02-10 | 2018-10-26 | 卡博特公司 | Elastomer blend |
| CN109705407A (en) * | 2018-12-17 | 2019-05-03 | 苏州鼎烯聚材纳米科技有限公司 | A kind of production method of graphene rubber concentrate feed and graphene rubber |
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| CN110678508A (en) * | 2017-05-15 | 2020-01-10 | 大陆轮胎德国有限公司 | Sulfur-crosslinked rubber mixture containing Carbon Nanotubes (CNTs) for vehicle tires, vehicle tire with sulfur-crosslinked rubber mixture, and method for producing sulfur-crosslinked rubber mixture containing carbon nanotubes |
| CN112778581A (en) * | 2021-01-28 | 2021-05-11 | 中北大学 | Low rolling resistance wet-skid modified natural rubber composite material and preparation method thereof |
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| CN105419004A (en) * | 2015-12-25 | 2016-03-23 | 张家港大塚化学有限公司 | High-heat-conductive rubber composition, preparation method thereof and tyre |
| CN108713038A (en) * | 2016-02-10 | 2018-10-26 | 卡博特公司 | Elastomer blend |
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| WO2022037060A1 (en) * | 2020-08-19 | 2022-02-24 | 吴立中 | Preparation method for reduced graphene oxide nitrile rubber and for tooth block without tooth marks |
| CN112778581A (en) * | 2021-01-28 | 2021-05-11 | 中北大学 | Low rolling resistance wet-skid modified natural rubber composite material and preparation method thereof |
| CN112778581B (en) * | 2021-01-28 | 2022-03-29 | 中北大学 | Low rolling resistance wet-skid modified natural rubber composite material and preparation method thereof |
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