CN109942922B - Preparation method of graphene-based heat-oxidation-resistant V-belt wrapping composite rubber - Google Patents
Preparation method of graphene-based heat-oxidation-resistant V-belt wrapping composite rubber Download PDFInfo
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Abstract
The invention relates to the technical field of transmission triangular belts, in particular to a preparation method of graphene-based heat-oxidation-resistant V-belt wrapping composite rubber, gradually forming zinc hydroxide of micro-sheets on zinc salt to enable graphene slurry to be adhered to the surfaces of the micro-sheets of zinc hydroxide in situ, further increasing the temperature, adding inorganic fibers to gradually decompose and convert the micro-sheets of zinc hydroxide into microporous zinc oxide to enable the graphene to be tightly resident and compounded in micropores of the microporous zinc oxide, meanwhile, the composite micro powder of the zinc oxide and the graphene is coated on a macroscopic interface of the inorganic fiber, is adhered to the inorganic fiber and carried by the inorganic fiber, the V-belt coating adhesive can be effectively dispersed in rubber to be used as a V-belt coating adhesive, the heat oxidation resistance is greatly improved, the V-belt strength is increased, and the V-belt is suitable for being used in high-load and high-temperature environments.
Description
Technical Field
The invention relates to the technical field of V belts, in particular to a preparation method of graphene-based heat-oxidation-resistant V belt wrapping cloth composite rubber.
Background
The V-shaped belt is an endless annular belt, the cross section of the V-shaped belt is in an isosceles trapezoid shape, the working surfaces are two side surfaces which are in contact with the wheel groove, and the belt is not in contact with the bottom surface of the wheel groove. The V-shaped belt is pressed by two side surfaces of the V-shaped belt and the side surface of the wheel groove to generate friction force to transmit power. Compared with the flat belt drive, the friction force of the V belt drive is large, and thus large power can be transmitted. Meanwhile, the V-belt is more compact than a flat belt structure, and the V-belt is a driving belt without joints, so that the transmission is more stable, and the V-belt is the transmission which is most widely applied in belt transmission. The V-belt has high bearing capacity and long service life due to the characteristics of the belt body structure, and is suitable for occasions with large load fluctuation and severe working conditions. The V-belt is widely applied to the fields of industry, agriculture, automobiles and the like, particularly the fields of industrial equipment in complex environments such as petroleum, metallurgy, chemical industry, textile, hoisting and the like, and has high adaptability.
The V-belt mainly comprises a framework material polyester thread rope, an adhesive primer and a wrapping cloth, and rubber aging and wrapping cloth delamination are easily caused by heat generation during high-load and high-friction transmission. Therefore, the selection of the material and the structural design of the V-belt are very critical to prolong the service life.
The wrapping cloth of the V-belt is directly contacted with the turbine, so that the service life of the V-belt can be greatly prolonged by virtue of good heat resistance, wear resistance and acid and alkali resistance. The conventional V-belt wrapping cloth is subjected to gum dipping treatment by using chloroprene rubber, has good physical and mechanical properties, is oil-resistant, flame-retardant, sunlight-resistant, ozone-resistant and acid-alkali-resistant, but has poor high-temperature resistance in chloroprene rubber, can not timely dissipate heat when high temperature is generated by transmission friction, can easily generate high temperature of more than 120 ℃ in high load, can accelerate the aging of the V-belt, and thus is subjected to thermal oxidation aging, so that the service life of the V-belt is greatly shortened.
Graphene has good thermal conductivity and extremely high strength, and is the substance with the highest strength known to human beings. The graphene has a wide application range, is particularly suitable for rubber composite materials, and can endow the materials with properties beyond imagination. Such as high-strength plastics, high-strength rubber, high-thermal conductivity polyester and the like, have profound influence on the upgrading and updating of the existing materials. Theoretically, graphene as a filler can be mixed into rubber for direct use. However, since graphene is an atomic-scale layer structure, the enhancement and heat dissipation functions in rubber are generated by virtue of the winding of graphene and rubber molecular chains. If the atomic-level graphene cannot be effectively dispersed in the rubber, the enhancement, corrosion resistance and heat dissipation performance of the rubber are greatly reduced.
Disclosure of Invention
The existing V-belt is easy to be heated, rubbed, aged, loosened and even delaminated when working at high temperature and high load. The surface of the V-belt is coated with cloth, so that the thermal oxidation resistance can be effectively improved, but higher requirements are put on the coating adhesive. Therefore, the thermal oxidation resistance of the modified coating adhesive is significant for prolonging the service life of the V-belt. The graphene has excellent heat dissipation, high mechanical property, excellent weather resistance, excellent wear resistance and excellent acid and alkali resistance, and the material performance can be greatly improved by using a small amount of the graphene. However, graphene belongs to an atomic-scale material, and is easily adsorbed or agglomerated, and the dispersion difficulty in a rubber system is high, so how to effectively disperse graphene in a rubber body is very important for exerting the functions of graphene micro-membrane reinforcement and heat dissipation.
In order to uniformly disperse graphene in rubber to serve as V-belt wrapping cloth rubber and keep the maximum contact interface between the graphene and a rubber body material, the invention provides graphene-based heat-resistant oxidation V-belt wrapping cloth composite rubber and a preparation method thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a preparation method of graphene-based anti-thermal oxidation V belt wrapping cloth composite rubber, which is characterized by comprising the following steps of:
(1) cutting 1-2 parts by weight of chloroprene rubber into small blocks, adding 10-20 parts by weight of solvent, and placing in a closed container for more than 48 hours to form slurry; then adding 3-5 parts by weight of graphene and 0.5-1 part by weight of emulsifier sodium dodecyl sulfate, and uniformly stirring to obtain graphene slurry;
(2) adding 5-10 parts by weight of zinc salt and 10-15 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at high speed for 30-45 min; then adding 5-15 parts by weight of inorganic fiber, raising the temperature of the closed container to 180 ℃, stirring at a low speed and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) performing jet milling and loosening on the powder obtained in the step (2) to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20-30: 5-10 kneading for 5-10min in a kneading machine at the temperature of 60-80 ℃, then adding an accelerator, an anti-aging agent, an antioxidant, a flame retardant and a plasticizer, continuing to knead for 5-10min, adding sulfur, kneading for 30-60s for discharging, passing through an open mill for 3-5 times, discharging, isolating water, airing and stacking to obtain the graphene-based heat oxidation resistant V belt wrapping composite rubber.
Preferably, the solvent in the step (1) is toluene or chloroform; graphene slurry is obtained by dispersing graphene in slurry formed by chloroprene rubber, so that on one hand, graphene is easily and tightly combined with subsequent microporous zinc oxide, and on the other hand, the subsequently obtained composite graphene micro powder is easily dispersed in chloroprene rubber and nitrile rubber.
Preferably, the zinc salt in the step (2) is at least one of zinc acetylacetonate, zinc acetate and zinc chloride; the inorganic fiber is at least one of glass fiber, brucite fiber, needle-shaped wollastonite fiber, barium sulfate whisker, calcium carbonate whisker, potassium titanate whisker and ceramic fiber; by adding the inorganic fiber, the graphene zinc oxide is compounded and coated on the macroscopic interface of the inorganic fiber, so that the friction resistance and the heat resistance of the coating adhesive can be better improved. The high-speed stirring speed is 600-900 rpm; the rotating speed of the low-speed stirring is 50-100 rpm; at 80 ℃, zinc salt gradually forms micro-flake zinc hydroxide, so that graphene slurry is adhered to the surface of the micro-flake zinc hydroxide in situ, the micro-flake zinc hydroxide is gradually converted into micro-pore zinc oxide by further raising the temperature, the graphene is tightly resided and compounded in micro-pores of the micro-pore zinc oxide and is coated on a macro interface of inorganic fibers, and the obtained composite micro powder of the zinc oxide and the graphene is adhered to the inorganic fibers to promote dispersion in rubber.
Preferably, the jet mill in step (3) is a vortex jet mill, and the vortex air flow of the vortex jet mill preferably relaxes fluffy powder into inorganic fibers adhered with the composite graphene micro powder, so as to prevent agglomeration of particles.
Preferably, the accelerator in step (3) is at least one of conventional sulfenamides, thiazoles, thiurams, guanidines, thioureas and dithiocarbamates; the rubber vulcanizing agent can better assist rubber vulcanization and promote the crosslinking reaction of the vulcanizing agent and rubber molecules, thereby shortening the vulcanizing time.
Preferably, the antioxidant in the step (3) is selected from the antioxidant 124 or the antioxidant NBC.
Preferably, the antioxidant in step (3) is at least one of antioxidant 1010, antioxidant 300, antioxidant 168, antioxidant 1076 and antioxidant 246.
Preferably, the flame retardant in step (3) is at least one of chlorine wax-52, chlorine wax-40, decabromodiphenyl ether, melamine cyanurate and antimony trioxide.
Preferably, the plasticizer in the step (3) is paraffin wax or dioctyl phthalate.
Preferably, the mass ratio of the accelerator, the anti-aging agent, the antioxidant, the flame retardant, the plasticizer and the sulfur in the step (3) is 1-3: 0.5-1: 0.5-1: 1-3: 1-2: 10-20. The addition amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
Preferably, the isolation water in the step (4) is isolation water which is used for preventing the rubber sheet from being bonded conventionally, and can be purchased from commercial products or prepared; preferably, the isolation water is obtained by emulsifying white carbon black, fatty acid ester and emulsifier in water.
Moreover, the invention further provides the graphene-based anti-thermal oxidation V belt wrapping composite rubber prepared by the method. Graphene slurry is obtained by dispersing graphene in slurry formed by chloroprene rubber, so that on one hand, graphene is easily and tightly combined with subsequent microporous zinc oxide, and on the other hand, the subsequently obtained composite graphene micro powder is easily dispersed in chloroprene rubber and nitrile rubber. Graphene is dispersed in sizing agent formed by chloroprene rubber, zinc hydroxide in micro-sheets is gradually formed on zinc salt, so that the graphene slurry is adhered to the surfaces of the micro-sheet zinc hydroxide in situ, inorganic fibers are added by further raising the temperature, the micro-sheet zinc hydroxide is gradually decomposed and converted into microporous zinc oxide, so that the graphene is tightly resided and compounded in the micropores of the microporous zinc oxide, and is coated on the macroscopic interface of the inorganic fiber, which is different from direct compounding, in the process of converting zinc hydroxide into zinc oxide, as the zinc oxide single crystal grows and releases moisture, the obtained composite micro powder of the zinc oxide and the graphene uniformly grows and adheres to inorganic fiber and is carried by the inorganic fiber, the V-belt coating adhesive can be effectively dispersed in rubber to be used as a V-belt coating adhesive, the heat oxidation resistance is greatly improved, the V-belt strength is increased, and the V-belt is suitable for being used in high-load and high-temperature environments.
According to the invention, the graphene and the zinc oxide are tightly coated with the inorganic fiber, and the inorganic fiber is carried by the inorganic fiber, so that the inorganic fiber is more easily dispersed in a rubber body to form a heat dissipation network compared with the atomic-level graphene and the nano-scale zinc oxide, and the heat resistance and the wear resistance are improved.
Furthermore, as the graphene is arranged in the micropores of the microporous zinc oxide, and the chloroprene rubber is adhered to the inner and outer interfaces, the zinc oxide promotes the crosslinking of the chloroprene rubber, so that the microporous zinc oxide and the graphene form a whole, the defect that the V-shaped belt falls off due to high friction is overcome, and the V-shaped belt is suitable for being used in a high-load and high-temperature environment.
Compared with the prior art, the graphene-based anti-thermal oxidation V-belt wrapping cloth composite rubber has the outstanding characteristics and excellent effects that:
1. according to the invention, graphene is adhered to the microchip in situ through the formation of the microchip zinc hydroxide, the graphene is tightly resided and compounded in micropores of the microporous zinc oxide by further utilizing the conversion of the zinc hydroxide into the microporous zinc oxide, the obtained composite micro powder of the zinc oxide and the graphene is adhered to inorganic fibers, and can be effectively dispersed in rubber to be used as V-belt wrapping glue through the carrying of the inorganic fibers, so that the defect that the graphene is difficult to disperse in a rubber body is overcome, and the excellent dispersion of the graphene allows the wrapping glue to have the characteristics of high temperature resistance and easy heat dissipation, thereby improving the thermal oxidation resistance of the V-belt.
2. According to the invention, as the graphene is in the micropores of the microporous zinc oxide, and the chloroprene rubber is adhered to the inner interface and the outer interface, and the zinc oxide promotes the crosslinking of the chloroprene rubber, the microporous zinc oxide and the graphene form a whole, and the compatibility with the interfaces of the chloroprene rubber and the nitrile rubber is good, the defect that the V-belt falls off due to high friction is overcome, and the V-belt is suitable for being used in a high-load and high-temperature environment.
3. The V-belt wrapping adhesive disclosed by the invention is uniformly dispersed with the combination of graphene and inorganic fiber, so that the V-belt wrapping adhesive is easy to dissipate heat, has good wear resistance, high temperature resistance, thermal oxidation resistance and acid and alkali resistance, and can be used in various severe environments such as long-term high temperature, high load, acid and alkali resistance and the like.
4. The preparation method is simple, the process is easy to control, and the method is suitable for large-scale production.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
(1) Cutting 1 part by weight of chloroprene rubber into small blocks smaller than 0.5cm, adding the small blocks into 10 parts by weight of toluene, and placing the small blocks in a closed container for 72 hours to form slurry capable of flowing naturally; then adding 3 parts by weight of graphene and 0.5 part by weight of emulsifier sodium dodecyl sulfate, and stirring for 10min in a closed container at the rotating speed of 200rpm to obtain graphene slurry;
(2) adding 10 parts by weight of zinc acetylacetonate and 10 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 600rpm for 30 min; then adding 5 parts by weight of needle-shaped wollastonite fibers, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 50rpm, simultaneously pumping out volatile matters by a vacuum pump, and drying for 25min to obtain dried fluffy powder;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20: 5 kneading for 10min in a kneading machine at the temperature of 80 ℃, then adding sulfonamide accelerator NOBS, anti-aging agent 124, antioxidant 300, flame retardant decabromodiphenyl ether and plasticizer No. 58 paraffin, continuing kneading for 5min, adding sulfur, kneading for 30s for discharging, thinning for 3 times through an open mill, discharging, airing after isolating water, stacking to obtain the graphene-based heat oxidation resistant V belt wrapping cloth composite rubber; wherein, the mixing mass ratio of the sulfenamide accelerator NOBS, the anti-aging agent 124, the antioxidant 300, the flame retardant decabromodiphenyl ether, the plasticizer No. 58 paraffin and the sulfur is 3: 0.5: 0.5: 1: 2: 15, the adding amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
Example 2
(1) Cutting 1 part by weight of chloroprene rubber into small blocks smaller than 0.5cm, adding the small blocks into 10 parts by weight of toluene, and placing the small blocks in a closed container for 72 hours to form slurry capable of flowing naturally; then adding 5 parts by weight of graphene and 1 part by weight of emulsifier sodium dodecyl sulfate, and stirring for 10min in a closed container at the rotating speed of 200rpm to obtain graphene slurry;
(2) adding 10 parts by weight of zinc acetate and 10 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 800rpm for 45 min; then adding 8 parts by weight of brucite fiber, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 50rpm, and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20: 7 kneading for 10min in a kneading machine at the temperature of 80 ℃, adding a thiuram accelerator TMTD, an anti-aging agent NBC, an antioxidant 1010, a flame retardant chlorinated wax-40 and a plasticizer dioctyl phthalate, continuing to knead for 10min, adding sulfur, kneading for 60s for discharging, passing through an open mill for 4 times, discharging sheets, passing through isolated water, airing and stacking to obtain the graphene-based thermal oxidation resistant V belt wrapping cloth composite rubber; wherein the mixing mass ratio of the thiuram accelerator TMTD, the anti-aging agent NBC, the antioxidant 1010, the flame retardant chlorinated wax-40, the plasticizer dioctyl phthalate and the sulfur is 1: 1: 0.5: 2: 1: 15, the adding amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
Example 3
(1) Cutting 2 parts by weight of chloroprene rubber into small pieces smaller than 0.5cm, adding the small pieces into 20 parts by weight of toluene, and placing the small pieces in a closed container for 72 hours to form slurry capable of flowing naturally; then adding 5 parts by weight of graphene and 1 part by weight of emulsifier sodium dodecyl sulfate, and stirring for 10min in a closed container at the rotating speed of 200rpm to obtain graphene slurry;
(2) adding 8 parts by weight of zinc chloride and 15 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 900rpm for 30 min; then adding 10 parts by weight of calcium carbonate whiskers, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 100rpm, and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 30: 10 kneading for 10min in a kneading machine at the temperature of 70 ℃, then adding dithiocarbamate accelerator VulkacitLDA, antioxidant 124, antioxidant 168, flame retardant antimony trioxide and plasticizer No. 58 paraffin wax, continuing kneading for 5min, adding sulfur, kneading for 40s for discharging, passing through an open mill for 5 times, discharging sheets, airing after passing through isolation water, and stacking to obtain the graphene-based heat oxidation resistant V belt wrapping cloth composite rubber; wherein the mixing mass ratio of dithiocarbamate accelerator Vulkacit LDA, anti-aging agent 124, antioxidant 168, flame retardant antimony trioxide, plasticizer No. 58 paraffin and sulfur is 3: 0.5: 0.5: 3: 2: 20, the adding amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder. The water-isolating agent is prepared by emulsifying white carbon black, fatty acid ester, NP-10 and water according to the mass ratio of 5:5:2: 120.
Example 4
(1) Cutting 1 part by weight of chloroprene rubber into small blocks smaller than 0.5cm, adding the small blocks into 10 parts by weight of toluene, and placing the small blocks in a closed container for 72 hours to form slurry capable of flowing naturally; then adding 5 parts by weight of graphene and 1 part by weight of emulsifier sodium dodecyl sulfate, and stirring for 10min in a closed container at the rotating speed of 200rpm to obtain graphene slurry;
(2) adding 5 parts by weight of zinc acetylacetonate and 10 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 900rpm for 45 min; then adding 12 parts by weight of glass fiber, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 50rpm, and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 30: 10 kneading for 5-10min in a kneading machine at the temperature of 60-80 ℃, adding a thiuram accelerator TMTD, an anti-aging agent NBC, an antioxidant 1076, a flame retardant decabromodiphenyl ether and a plasticizer No. 58 paraffin wax, continuing kneading for 5min, adding sulfur, kneading for 60s, discharging, passing through an open mill for 5 times, discharging sheets, and carrying out air drying and stacking after isolation water to obtain the graphene-based heat oxidation resistant V belt wrapping cloth composite rubber; wherein the mixing mass ratio of the thiuram accelerator TMTD, the anti-aging agent NBC, the antioxidant 1076, the flame retardant decabromodiphenyl ether, the plasticizer No. 58 paraffin and the sulfur is 1: 1: 1: 3: 2: 20, the adding amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
Comparative example 1
(1) Cutting 1 part by weight of chloroprene rubber into small blocks smaller than 0.5cm, adding the small blocks into 10 parts by weight of toluene, and placing the small blocks in a closed container for 72 hours to form slurry capable of flowing naturally; then adding 3 parts by weight of graphene and 0.5 part by weight of emulsifier sodium dodecyl sulfate, and stirring for 10min in a closed container at the rotating speed of 200rpm to obtain graphene slurry;
(2) adding 5 parts by weight of zinc oxide into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 600rpm for 30 min; then adding 5 parts by weight of needle-shaped wollastonite fibers, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 50rpm, and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers of the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber of the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20: 5 kneading for 10min in a kneading machine at the temperature of 80 ℃, then adding sulfonamide accelerator NOBS, anti-aging agent 124, antioxidant 300, flame retardant decabromodiphenyl ether and plasticizer No. 58 paraffin, continuing kneading for 5min, adding sulfur, kneading for 30s for discharging, thinning for 3 times through an open mill, discharging, airing after isolating water, stacking to obtain the graphene-based heat oxidation resistant V belt wrapping cloth composite rubber; wherein, the mixing mass ratio of the sulfenamide accelerator NOBS, the anti-aging agent 124, the antioxidant 300, the flame retardant decabromodiphenyl ether, the plasticizer No. 58 paraffin and the sulfur is 3: 0.5: 0.5: 1: 2: 15, the adding amount is 15 percent of the total mass of the inorganic fibers of the chloroprene rubber, the nitrile rubber and the composite graphene micro powder.
Compared with example 1, in comparative example 1, the inorganic fiber is coated on the graphene and the microporous zinc oxide by compounding the graphene and the microporous zinc oxide without adopting a method of firstly generating the microchip zinc hydroxide and then generating the microporous zinc oxide, but the graphene, the zinc oxide and the inorganic fiber are directly compounded, and the dispersion of the graphene in the rubber body is influenced because the graphene, the zinc oxide and the inorganic fiber cannot be stably carried.
Comparative example 2
(1) Adding 5 parts by weight of graphene into 10 parts by weight of toluene, placing the mixture in a closed container for 72 hours, then adding 1 part by weight of emulsifier sodium dodecyl sulfate, and stirring the mixture in the closed container at the rotating speed of 200rpm for 10 minutes to obtain graphene slurry;
(2) adding 10 parts by weight of zinc acetate and 10 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at a high speed of 800rpm for 45 min; then adding 8 parts by weight of brucite fiber, raising the temperature of the closed container to 180 ℃, stirring at a low speed of 50rpm, and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained;
(3) crushing and loosening the powder obtained in the step (2) by using a vortex airflow powder to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20: 7 kneading for 10min in a kneading machine at the temperature of 80 ℃, adding a thiuram accelerator TMTD, an anti-aging agent NBC, an antioxidant 1010, a flame retardant chlorinated wax-40 and a plasticizer dioctyl phthalate, continuing to knead for 10min, adding sulfur, kneading for 60s for discharging, passing through an open mill for 4 times, discharging sheets, passing through isolated water, airing and stacking to obtain the graphene-based thermal oxidation resistant V belt wrapping cloth composite rubber; wherein the mixing mass ratio of the thiuram accelerator TMTD, the anti-aging agent NBC, the antioxidant 1010, the flame retardant chlorinated wax-40, the plasticizer dioctyl phthalate and the sulfur is 1: 1: 0.5: 2: 1: 15, the adding amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
Compared with example 1, comparative example 2 does not disperse in the neoprene solution in advance when the graphene and the zinc oxide are loaded, thereby affecting the compatibility and the dispersibility of the obtained composite graphene and the rubber matrix.
And (3) performance testing:
under the same conditions, the wrapping cloth rubber obtained in the examples 1-4 and the comparative examples 1-2 is subjected to open mill hot refining, then the polyester cotton canvas base material is coated with the rubber by a four-roll calender to prepare wrapping cloth, and the V belt with the core material skeleton of polyester yarn produced in the same batch is coated and thermally vulcanized to obtain the wrapping cloth V belt with the upper width of 17mm, the belt height of 11mm, the angle of 40 degrees and the angle of 500 lnch. The V-belt fatigue performance is tested by referring to GB/T15328-2009 standard, and the performances of the coating rubber in the aspects of wear resistance and heat dissipation are reflected by the fatigue resistance and the temperature of the wheel, as shown in Table 1.
Table 1:
| test sample | V-band fatigue life/h | Fatigue wheel temperature/° c | Appearance of wrapping cloth |
| Example 1 | 225 | 86 | Wrapping cloth is intact |
| Example 2 | 227 | 90 | Wrapping cloth is intact |
| Example 3 | 217 | 87 | Wrapping cloth is intact |
| Example 4 | 231 | 88 | Wrapping cloth is intact |
| Comparative example 1 | 197 | 101 | Breakage of cloth covering layer |
| Comparative example 2 | 186 | 97 | The cloth covering layer falls off |
Traditionally, the temperature is easily increased to more than 100 ℃ during the V-belt test, the high-temperature workability of the V-belt is affected, fatigue and delamination fracture are easily generated under high load, the obtained coating rubber has excellent heat dissipation, and the heat dissipation and heat resistance in time enable the thermal oxidation resistance of the V-belt to be enhanced and the fatigue life to be prolonged. However, we note that in comparative example 1, the inorganic fiber is coated on the graphene and the microporous zinc oxide by compounding the graphene and the microporous zinc oxide by a method of firstly generating the microchip zinc hydroxide and then generating the microporous zinc oxide, but the graphene, the zinc oxide and the inorganic fiber are directly compounded, and the dispersion of the graphene in the rubber body is affected because the graphene, the microporous zinc oxide and the inorganic fiber cannot be stably carried. Comparative example 2 since graphene is not completely dispersed in chloroprene rubber by the method of the present invention, the dispersion of graphene and the compatibility with matrix rubber are affected, thereby affecting the heat dissipation of the wrap of the V-band and the close adhesion of the wrap to the primer.
Claims (6)
1. A preparation method of graphene-based heat oxidation resistant V-belt wrapping composite rubber is characterized by comprising the following steps:
(1) cutting 1-2 parts by weight of chloroprene rubber into small blocks, adding 10-20 parts by weight of solvent, and placing in a closed container for more than 48 hours to form slurry; then adding 3-5 parts by weight of graphene and 0.5-1 part by weight of emulsifier sodium dodecyl sulfate, and uniformly stirring to obtain graphene slurry;
(2) adding 5-10 parts by weight of zinc salt and 10-15 parts by weight of ammonia water into the graphene slurry obtained in the step (1), heating to 80 ℃ in a closed container, and stirring at high speed for 30-45 min; then adding 5-15 parts by weight of inorganic fiber, heating the temperature of the closed container to 180 ℃, stirring at a low speed and simultaneously pumping out volatile matters by a vacuum pump until dry fluffy powder is obtained; the zinc salt is at least one of zinc acetylacetonate, zinc acetate and zinc chloride; the inorganic fiber is at least one of glass fiber, brucite fiber, needle-shaped wollastonite fiber, barium sulfate whisker, calcium carbonate whisker, potassium titanate whisker and ceramic fiber; the high-speed stirring speed is 600-900 rpm; the rotating speed of the low-speed stirring is 50-100 rpm;
(3) performing jet milling and loosening on the powder obtained in the step (2) to obtain inorganic fibers adhered with the composite graphene micro powder;
(4) and (3) mixing chloroprene rubber, nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder obtained in the step (3) in a mass ratio of 100: 20-30: 5-10 kneading for 5-10min in a kneading machine at the temperature of 60-80 ℃, then adding an accelerator, an anti-aging agent, an antioxidant, a flame retardant and a plasticizer, continuing to knead for 5-10min, adding sulfur, kneading for 30-60s for discharging, passing through an open mill for 3-5 times, discharging, isolating water, airing and stacking to obtain the graphene-based heat oxidation resistant V belt wrapping composite rubber.
2. The preparation method of the graphene-based anti-thermal oxidation V belt wrapping composite rubber according to claim 1, characterized by comprising the following steps: the solvent in the step (1) is toluene or chloroform.
3. The preparation method of the graphene-based anti-thermal oxidation V belt wrapping composite rubber according to claim 1, characterized by comprising the following steps: and (3) selecting a vortex jet mill for jet milling.
4. The preparation method of the graphene-based anti-thermal oxidation V belt wrapping composite rubber according to claim 1, characterized by comprising the following steps: the accelerator in the step (4) is at least one of conventional sulfenamides, thiazoles, thiurams, guanidines, thiourea and dithiocarbamate; the anti-aging agent is selected from anti-aging agent 124 or anti-aging agent NBC; the antioxidant is at least one of antioxidant 1010, antioxidant 300, antioxidant 168, antioxidant 1076 and antioxidant 246; the flame retardant is at least one of chlorine wax-52, chlorine wax-40, decabromodiphenyl ether, melamine cyanurate and antimony trioxide; the plasticizer is paraffin or dioctyl phthalate.
5. The preparation method of the graphene-based anti-thermal oxidation V belt wrapping composite rubber according to claim 1, characterized by comprising the following steps: the mass ratio of the accelerator, the anti-aging agent, the antioxidant, the flame retardant, the plasticizer and the sulfur in the step (4) is 1-3: 0.5-1: 0.5-1: 1-3: 1-2: 10-20 parts of; the addition amount is 15 percent of the total mass of the chloroprene rubber, the nitrile rubber and the inorganic fiber adhered with the composite graphene micro powder.
6. The graphene-based anti-thermal oxidation V-belt wrapping composite rubber is characterized in that: prepared by the process of any one of claims 1 to 5.
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Denomination of invention: A preparation method of graphene based anti thermal oxidation V-belt coated composite rubber Effective date of registration: 20220114 Granted publication date: 20210312 Pledgee: Zhejiang Tiantai Rural Commercial Bank Co.,Ltd. Sanhe sub branch Pledgor: ZHEJIANG BAIHUA BUBBER BELT Co.,Ltd. Registration number: Y2022330000080 |