CN115418024B - Carbon nano tube/carbon black aggregate, preparation method and high-performance tire tread rubber composition - Google Patents
Carbon nano tube/carbon black aggregate, preparation method and high-performance tire tread rubber composition Download PDFInfo
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Abstract
The invention relates to the technical field of new rubber reinforcement materials, in particular to a carbon nano tube/carbon black aggregate, a preparation method and a high-performance tire tread rubber composition. The preparation method of carbon nanotube/carbon black aggregate, this method adds the carbon nanotube into the production process of the carbon black, give the advantage performance of the carbon nanotube to the carbon black, form a new type carbon black/carbon nanotube aggregate, this aggregate can maintain the structural advantage of the carbon nanotube, such as higher draw ratio and specific surface area, can also reduce the flying problem of the carbon nanotube effectively, have improved the dispersibility of the carbon nanotube in the rubber matrix, the most critical point is that can make the reinforcement effect of the carbon nanotube also improved at the same time, add this carbon nanotube/carbon black aggregate to sizing material can obviously improve the physical mechanical properties of sizing material, reduce hysteresis loss and rolling resistance of sizing material and not damaging its anti-wet-slip performance at the same time, have better development prospect.
Description
Technical Field
The invention relates to the technical field of new rubber reinforcement materials, in particular to a carbon nano tube/carbon black aggregate, a preparation method and a high-performance tire tread rubber composition.
Background
Carbon black is a common rubber reinforcing agent, and after the carbon black is added, the modulus and the wear resistance of the rubber material are improved by more than 10 times, so that the rubber industry cannot develop to the present day without carbon black and other nano reinforcing materials. With the progress of nanotechnology, various nanoparticles are sequentially applied to rubber materials to form rubber composite materials with excellent properties, and besides common carbon black, other materials including white carbon black, nano calcium carbonate, clay, nano zinc oxide, carbon nanotubes and graphene are also more commonly used, wherein the carbon nanotubes are considered to be novel rubber reinforced nano materials with very promising development due to the higher specific surface area, high length-diameter ratio and excellent mechanical, electrical and thermal properties.
Researches show that the reinforcing effect of the carbon nano tube is more excellent than that of carbon black and white carbon black, for example, in a rubber formula of China patent application (CN 113929989A, CN103694505A, CN101381483 and the like), the mechanical property of a rubber material can be obviously improved by adding a small amount of the carbon nano tube, fatigue resistance, crack growth resistance and heat resistance can be improved, and in addition, the unique electric conduction, heat conduction, electromagnetic shielding, wave absorption and the like of the rubber material are also provided. However, in the practical application process, the dispersion condition of the carbon nanotubes in the rubber material and the combination state of the carbon nanotubes and the rubber can directly influence the performance of the rubber material, the mechanical mixing method is the most commonly used carbon nanotube/rubber compounding method, but the dispersion effect is poor, the carbon nanotubes are easy to fly in the production and processing process, dust pollution can be caused, in-situ polymerization, solution blending, emulsion blending and other modes (China patent application CN110003503A, CN110606965A and the like) are also researched by scientific researchers in recent years to improve the dispersibility of the carbon nanotubes in the rubber, but the methods are not directly convenient by the mechanical mixing method, and a large amount of solvents are required to be consumed in the solution blending method, so that the solvents are toxic and pollute the environment.
The Chinese invention patent (CN 112080161A) applied by Hangzhou midwifery spring industry Co-Ltd of the applicant discloses a double-phase carbon black production process, which comprises the following steps: the crude oil formula adopts low-moisture raw oil with moisture content less than or equal to 2.0 percent; mixing raw oil in a reaction furnace section with high-temperature combustion air flow at a temperature of more than 1500 ℃; step 2): through powder jet technology, mixing silicon lattice powder with process water, spraying into a carbon black reaction furnace, and chemically combining the powdery silicon lattice powder with carbon black primary particles at high temperature to form Si-C and-Si-O-C-short chain structures; step 3): forming a double-phase carbon black aggregate through the aggregation of carbon black; step 4): and (3) collecting and separating carbon black smoke through a main bag filter, granulating, drying and storing the carbon black. The combined surface of the double-phase carbon black inherits the hydroxyl structure of the surface of the silicon lattice powder, the ortho-position hydroxyl forms an internal hydrogen bond, the isolated hydroxyl and the double hydroxyl form an external hydrogen bond with polar groups such as hydroxyl in rubber molecules, and a polymer molecular chain penetrates through a rubber polymer chain network in the rubber, so that the excellent comprehensive performance of the material is endowed.
Disclosure of Invention
In order to solve the problem of dispersibility of carbon nanotubes in a rubber matrix, the applicant obtains a heuristic from the patent (CN 112080161A) of China and proposes a preparation method of carbon nanotube/carbon black aggregate, wherein the carbon nanotubes are added into the production process of carbon black, the dominant properties of the carbon nanotubes are endowed to the carbon black to form a novel carbon black/carbon nanotube aggregate, the aggregate can maintain the structural advantages of the carbon nanotubes, such as higher length-diameter ratio and specific surface area, the flying problem of the carbon nanotubes can be effectively reduced, the dispersibility of the carbon nanotubes in the rubber matrix is improved, meanwhile, the most critical point is that the reinforcing effect of the carbon nanotubes is also improved, the addition of the carbon nanotube/carbon black aggregate into a sizing material can obviously improve the physical and mechanical properties of the sizing material, and simultaneously, the hysteresis loss and rolling resistance of the sizing material are reduced without damaging the wet-skid resistance of the sizing material, so that the preparation method has a better development prospect.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a method of preparing a carbon nanotube/carbon black aggregate, the method comprising the steps of:
step 1): the crude oil formula adopts low-moisture raw material hydrocarbon with the moisture content less than or equal to 2.0 percent; the raw material hydrocarbon and a proper amount of air form a closed turbulence system, and part of raw material hydrocarbon and air are combusted to generate high temperature of more than 1500 ℃ so that the other part of raw material hydrocarbon is fully cracked into carbon black primary particles;
step 2): uniformly mixing the carbon nano tube with process water by a powder injection technology, and injecting the mixture into a carbon black reaction furnace, wherein the carbon nano tube and carbon black primary particles are tightly combined at high temperature to form a pre-agglomeration body;
step 3): forming carbon nanotube/carbon black aggregate by aggregation of carbon black;
step 4): the suspended carbon nano tube/carbon black aggregate flue gas is subjected to cooling, filtering and main bag filter collection and separation, and the aggregate is subjected to granulation, drying and storage.
Preferably, the raw oil comprises coal tar, anthracene oil, ethylene tar and mixed oil.
Preferably, the carbon nanotube/carbon black aggregate contains 1-10% by weight of carbon nanotubes.
Preferably, the concentration of the carbon nano tube in the suspension of the carbon nano tube and the process water is 15% -25%.
Preferably, the granulating and drying in the step 4) is to stir and granulate the powdery carbon nano tube/carbon black aggregate with a proper amount of water and a compatilizer in a granulator, then send the aggregate particles into a rotary dryer for drying, and finally obtain the carbon nano tube/carbon black aggregate after removing the water; preferably, the mass percentage of the powdery carbon nano tube/carbon black aggregate is 20-30%, the compatilizer is 1-5%, and the balance is water; preferably, the compatibilizer is molasses or lignosulfonate.
Further, the invention also discloses the carbon nano tube/carbon black aggregate prepared by the method. Furthermore, the invention also discloses application of the carbon nano tube/carbon black aggregate to the rubber reinforcing material which is used for completely or partially replacing carbon black.
The invention further discloses a high-performance tire rubber composition, wherein the total rubber consumption is 100 parts by weight, and the total carbon nano tube/carbon black aggregate is 45-60 parts; the carbon nanotube/carbon black aggregate is adopted.
The invention improves the dispersion and processing performance of the carbon nano tube, reduces the Payne effect of the carbon black, reduces hysteresis loss, and can reduce the rolling resistance of the tire and prolong the service life of the tire on the premise of ensuring the wear resistance of the tire by applying the carbon nano tube/carbon black aggregate to the tire tread rubber composition.
The invention further discloses a high-performance tire tread rubber composition, which is prepared by mixing the following raw materials:
the carbon nanotube/carbon black aggregate is adopted.
Further, the invention also discloses a preparation method of the high-performance tire tread rubber composition, which comprises the following steps:
1) Mixing: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 40-55 rmp, mixing the internal mixer at the pressure of 4.5-6.5 MPa, cooling water at the temperature of 30-40 ℃, adding raw rubber, carbon nano tube/carbon black aggregate, an activating agent, an anti-aging agent, protective wax and other processing aids, mixing for 20-40 seconds, lifting a top bolt, staying for 10-15 seconds, pressing the top bolt, mixing to the temperature of 135-145 ℃, lifting the top bolt, staying for 10-15 seconds, pressing the top bolt, and discharging rubber at the temperature of 145-165 ℃, wherein the rubber is carbon nano tube/carbon black master batch;
2) And (3) adding sulfur: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 15-40 rmp, mixing the internal mixer at the pressure of 4.0-6.0 MPa, cooling water at the temperature of 30-40 ℃, adding carbon nano tube/carbon black master batch, vulcanizing agent, accelerator and scorch retarder of the tread composition, lifting a top bolt after mixing for 10-60 seconds, staying for 0-15 seconds, pressing the top bolt after mixing to the temperature of 70-85 ℃, lifting the top bolt after staying for 0-15 seconds, discharging rubber after the temperature of the rubber material is 100-120 ℃, and cooling the lower piece to room temperature to obtain the tread rubber for preparing the high-performance tire.
The invention has the technical effects that:
the technology mainly adds the carbon nano tube into the production process of the carbon black, endows the carbon nano tube with the dominant performance on the carbon black to form a novel carbon black/carbon nano tube aggregate, not only can maintain the structural advantages of the carbon nano tube such as higher length-diameter ratio and specific surface area, but also can effectively reduce the flying problem of the carbon nano tube, improves the dispersibility of the carbon nano tube in a rubber matrix, and simultaneously has the most critical point that the reinforcing effect of the carbon nano tube is also improved, and the addition of the carbon nano tube/carbon black aggregate into the rubber material can obviously improve the physical and mechanical properties of the rubber material, simultaneously reduce the hysteresis loss and rolling resistance of the rubber material without damaging the wet skid resistance of the rubber material, thereby having better development prospect.
Drawings
FIG. 1 is a scanning electron micrograph of example 1.
Fig. 2 is a scanning electron micrograph of comparative example 1.
FIG. 3 is a G' -Strain curve of example 1 and comparative example 1.
Detailed Description
The invention will be further illustrated with reference to specific examples, but the scope of the invention is not limited to these examples.
In the present invention:
carbon black N134: produced by cabot (china) investment limited.
Anti-aging agent 4020: the product is manufactured by Jiangsu san Orthochemistry Co., ltd, and has the trade name of age resister 4020 and the chemical name of N- (1, 3-dimethylbutyl) -N' -phenyl-p-phenylenediamine.
Anti-aging agent RD: the product is produced by Tianjin Michaelis chemical Co., ltd, and has the trade name of an anti-aging agent RD and the chemical name of a 2, 4-trimethyl-1, 2-dihydroquinoline polymer.
Anti-aging agent 4020: the product is manufactured by Shandong san Orthochemistry Co., ltd, and has the trade name of age resister 4020 and the chemical name of N- (1, 3-dimethyl) butyl-N' -phenyl p-phenylenediamine.
Accelerator NS: shandong Dai Ruike New Material Co., ltd., product name is NS, chemical name is N-tert-butyl-2-benzothiazole sulfenamide.
Example 1
Preparation of carbon nanotube/carbon black aggregate:
step 1): the crude oil formula adopts low-moisture raw material hydrocarbon with the moisture content less than or equal to 2.0 percent; the raw material hydrocarbon and a proper amount of air form a closed turbulence system, and part of the raw material hydrocarbon and the air are combusted to generate high temperature (reaching more than 1500 ℃), so that the other part of the raw material hydrocarbon is fully cracked into carbon black primary particles;
step 2): uniformly mixing the carbon nano tube with process water by a powder injection technology, and injecting the mixture into a carbon black reaction furnace, wherein the concentration of the carbon nano tube in the suspension of the carbon nano tube and the process water is 20%, and the carbon nano tube and carbon black primary particles are tightly combined at high temperature to form a pre-agglomeration body; the powder injection technology is that carbon nano tubes are conveyed into an embedded double helix capable of precisely quantifying through a mechanical arch breaking device in a storage bin, an air flow arch breaking device and a coulter stirring device at the lower part of the bin, the carbon nano tubes metered by a weighing system and the precise quantitative helix enter a mass transfer cavity of a high-speed injection mixer, are instantly mixed with an injection carrier, namely process water, the carbon nano tubes are forcedly dispersed into the injection carrier in the movement process, are rapidly dispersed into uniform suspension in a diffuser at the tail part of the injector through pressure change, and are conveyed into a pressure atomization system;
step 3): forming a carbon nano tube/carbon black aggregate by the aggregation of carbon black, wherein the weight content of the carbon nano tube in the carbon nano tube/carbon black aggregate is 8%;
step 4): the suspended carbon nano tube/carbon black aggregate flue gas is subjected to cooling, filtering and main bag filter collection and separation, the separated tail gas is used for tail gas furnace heat supply and boiler power generation, finally, the powdery carbon nano tube/carbon black aggregate and a proper amount of water and compatilizer are stirred in a granulator to granulate, and then, aggregate particles are sent into a rotary dryer to be dried, and the water is removed to finally obtain the carbon nano tube/carbon black aggregate; the mass percentage of the powdery carbon nano tube/carbon black aggregate is 25%, the compatilizer is 2%, and the balance is water; preferably, the compatibilizer is molasses or lignosulfonate.
The high-performance tire tread rubber composition comprises the following raw materials in parts by weight: 100 parts of natural rubber, 2 parts of stearic acid, 3.5 parts of zinc oxide, 1.3 parts of sulfur, 2.6 parts of accelerator NS, 1.5 parts of anti-aging agent 4020.5 parts of anti-aging agent RD 1 parts, 0.75 part of anti-aging agent DTPD, 1.5 parts of protective wax, 52 parts of carbon nano tube/carbon black aggregate and 0.25 part of scorch retarder CTP.
Preparation of high performance tire tread rubber composition: step 1) mixing: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 45rmp, mixing the internal mixer at 5.5MPa, cooling water at 35 ℃, adding raw rubber, carbon nano tube/carbon black, an activating agent, an anti-aging agent, protective wax and other processing aids, mixing for 35 seconds, lifting a top bolt, staying for 7 seconds, pressing the top bolt, lifting the top bolt, mixing to 140 ℃, staying for 10 seconds, pressing the top bolt, and discharging the rubber at 155 ℃, wherein the rubber is the carbon nano tube/carbon black master batch. Step 2) adding sulfur: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 20rmp, mixing the internal mixer at 5MPa, cooling water at 35 ℃, adding carbon nano tube/carbon black master batch, vulcanizing agent, accelerator and anti-scorching agent of the tread composition, lifting a top plug after mixing for 40 seconds, pressing the plug for 5 seconds, lifting the top plug when mixing to 80 ℃, pressing the top plug for 7 seconds, lifting the plug for discharging rubber when the temperature of the rubber material is 113 ℃, and cooling a lower piece to room temperature to obtain the tread rubber for preparing the high-performance tire.
Comparative example 1
The high-performance tire tread rubber composition comprises the following raw materials in parts by weight: 100 parts of natural rubber, 2 parts of stearic acid, 3.5 parts of zinc oxide, 1.3 parts of sulfur, 2.6 parts of accelerator NS, 1.5 parts of anti-aging agent 4020.5 parts of anti-aging agent RD 1 parts, 0.75 part of anti-aging agent DTPD, 1.5 parts of protective wax, 52 parts of carbon black N and 0.25 part of scorch retarder CTP. The preparation is described in example 1.
Comparative example 2
The high-performance tire tread rubber composition comprises the following raw materials in parts by weight: 100 parts of natural rubber, 2 parts of stearic acid, 3.5 parts of zinc oxide, 1.3 parts of sulfur, 2.6 parts of accelerator NS, 1.5 parts of anti-aging agent 4020.5 parts of anti-aging agent RD 1 parts, 0.75 part of anti-aging agent DTPD, 1.5 parts of protective wax, 50 parts of carbon black N, 2 parts of carbon nano tube and 0.25 part of scorch retarder CTP. Preparation method referring to comparative example 1, carbon nanotubes were added in the mixing section.
In fig. 1 and 2, white tubular white dots are carbon nanotubes, in comparative example 1, the carbon nanotubes can be seen to be aggregated in a red rectangular frame, and the local dispersion is relatively uneven, in example 1, the carbon nanotubes are not aggregated obviously, the dispersion is better, the corresponding tan delta is smaller, and as can be seen from a G' -Strain curve, the Payne effect of the vulcanized rubber of example 1 is smaller than that of comparative example 1, which also shows that the dispersion and processing performance of the carbon nanotubes can be improved through the process, and simultaneously, the Payne effect of carbon black and hysteresis loss are also reduced.
In the above matters, the tread rubber composition with low rolling resistance and high performance and the preparation method thereof, compared with the tread rubber composition adopting carbon nano tube/carbon black aggregate in example 1, are found to have improved wear resistance, reduced heat generation and improved mechanical strength by comparing 1 and 2; compared with tread rubber produced by a nano composite technology of adding only carbon black and directly adding carbon black and carbon nano tubes in the mixing process, the tread rubber composition has more excellent performance, and the carbon nano tubes are more uniformly dispersed in the process, so that the performance of the embodiment and the comparative example shows that the tread rubber composition for the high-performance tire prepared by the invention reduces the rolling resistance of the tire and prolongs the service life of the tire on the premise of ensuring the wear resistance of the tire.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art. The generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (12)
1. A method for preparing a carbon nanotube/carbon black aggregate, comprising the steps of:
step 1): the crude oil formula adopts low-moisture raw material hydrocarbon with the moisture content less than or equal to 2.0 percent; the raw material hydrocarbon and a proper amount of air form a closed turbulence system, and part of raw material hydrocarbon and air are combusted to generate high temperature of more than 1500 ℃ so that the other part of raw material hydrocarbon is fully cracked into carbon black primary particles;
step 2): uniformly mixing the carbon nano tube with process water by a powder injection technology, and injecting the mixture into a carbon black reaction furnace, wherein the carbon nano tube and carbon black primary particles are tightly combined at high temperature to form a pre-agglomeration body;
step 3): forming carbon nanotube/carbon black aggregate by aggregation of carbon black;
step 4): the suspended carbon nano tube/carbon black aggregate flue gas is subjected to cooling, filtering and main bag filter collection and separation, and the aggregate is subjected to granulation, drying and storage.
2. The method of claim 1, wherein the crude oil formulation comprises coal tar, anthracene oil, ethylene tar, or a blend oil.
3. The method of claim 1, wherein the carbon nanotube/carbon black aggregate comprises 1% -10% by weight of carbon nanotubes.
4. The method of claim 1, wherein the concentration of carbon nanotubes in the carbon nanotube and process water suspension is 15% -25%.
5. The method according to claim 1, wherein the granulating and drying in the step 4) is carried out by granulating the powdery carbon nanotube/carbon black aggregate with an appropriate amount of water and a compatibilizer by stirring in a granulator, then feeding the aggregate particles into a rotary dryer for drying, and finally removing the water.
6. The method according to claim 5, wherein the powdery carbon nanotube/carbon black aggregate is 20-30% by mass, the compatibilizer is 1-5% by mass, and the balance is water.
7. The method of claim 5, wherein the compatibilizer is molasses or lignosulfonate.
8. A carbon nanotube/carbon black aggregate prepared by the method of any one of claims 1-7.
9. Use of the carbon nanotube/carbon black aggregate of claim 8 for replacing carbon black in whole or in part as a rubber reinforcement.
10. A high-performance tire rubber composition is characterized in that: the total rubber consumption is 100 weight parts, and the carbon nano tube/carbon black aggregate is 45-60 weight parts; the carbon nanotube/carbon black aggregate according to claim 8.
11. The high-performance tire tread rubber composition is characterized by being prepared by mixing the following raw materials:
100 parts of raw rubber
45-60 parts of carbon nano tube/carbon black aggregate
1 to 12 parts of active agent
0.8 to 6 portions of accelerant
0.8 to 6 portions of vulcanizing agent
1 to 5 portions of anti-aging agent
0.5 to 2.5 portions of protective wax
0 to 0.3 part of scorch retarder CTP
0-6 parts of other processing aids;
the carbon nanotube/carbon black aggregate according to claim 8.
12. A method of preparing a high performance tire tread stock composition as in claim 11, comprising the steps of:
1) Mixing: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 40-55 rmp, mixing the internal mixer at the pressure of 4.5-6.5 MPa, cooling water at the temperature of 30-40 ℃, adding raw rubber, carbon nano tube/carbon black aggregate, an activating agent, an anti-aging agent, protective wax and other processing aids, mixing for 20-40 seconds, lifting a top bolt, staying for 10-15 seconds, pressing the top bolt, mixing to the temperature of 135-145 ℃, lifting the top bolt, staying for 10-15 seconds, pressing the top bolt, and discharging rubber at the temperature of 145-165 ℃, wherein the rubber is carbon nano tube/carbon black master batch;
2) And (3) adding sulfur: starting an internal mixer, setting the rotation speed of a rotor of the internal mixer to be 15-40 rmp, mixing the internal mixer at the pressure of 4.0-6.0 MPa, cooling water at the temperature of 30-40 ℃, adding carbon nano tube/carbon black master batch, vulcanizing agent, accelerator and scorch retarder of the tread composition, lifting a top bolt after mixing for 10-60 seconds, staying for 0-15 seconds, pressing the top bolt after mixing to the temperature of 70-85 ℃, lifting the top bolt after staying for 0-15 seconds, discharging rubber after the temperature of the rubber material is 100-120 ℃, and cooling the lower piece to room temperature to obtain the tread rubber for preparing the high-performance tire.
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| US20080233402A1 (en) * | 2006-06-08 | 2008-09-25 | Sid Richardson Carbon & Gasoline Co. | Carbon black with attached carbon nanotubes and method of manufacture |
| CN111333060A (en) * | 2020-04-23 | 2020-06-26 | 上海轮匠科技有限公司 | Wet compounding method of graphene oxide/carbon nano tube and carbon nano carbon black |
| CN113652011A (en) * | 2021-07-05 | 2021-11-16 | 中策橡胶集团有限公司 | Low-heat-generation high-heat-conductivity tread rubber composition, mixing method thereof and tire |
| CN114292450B (en) * | 2022-01-04 | 2023-05-26 | 中策橡胶集团股份有限公司 | Dry mixing method of tire rubber composition, tread composition and low-rolling-resistance high-performance tire |
| CN114854202B (en) * | 2022-06-07 | 2024-01-26 | 浙江柔灵科技有限公司 | Carbon black-carbon nano tube mixed silica gel filled electrode material and process thereof |
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