CN117209869B - Composite rubber material for preparing buffer block for vehicle - Google Patents
Composite rubber material for preparing buffer block for vehicle Download PDFInfo
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Abstract
The invention provides a composite rubber material for preparing a vehicle buffer block, which comprises natural rubber, crimped composite carbon fiber and a vulcanizing agent TMTD, wherein the weight part ratio of the natural rubber to the crimped composite carbon fiber is 100: (10-30), the coiled composite carbon fiber comprises a carbon fiber core part and a Kevlar film layer attached to the surface of the carbon fiber core part, the damping coefficient and the service life of natural rubber are improved by adding the coiled composite carbon fiber, the coiled composite carbon fiber can be elastically deformed along with the natural rubber under the action of high-strength fatigue, meanwhile, energy absorption and consumption can be carried out, heating under the action of rubber fatigue is avoided, and meanwhile, the carbon fiber has good heat conducting property and further improves the heat dissipation property of the carbon fiber, so that the service life of the carbon fiber is prolonged.
Description
Technical Field
The invention relates to the technical field of rubber composite materials, in particular to a composite rubber material for preparing a buffer block for a vehicle.
Background
The rubber type buffer block is widely applied to the automobile shock absorption buffer block, and provides huge performance improvement for the shock absorption buffer of an automobile through the excellent elasticity provided by the rubber type buffer block, but because the elastic impact action on the buffer block in the use environment of the automobile buffer block is frequent, and the working environment is relatively bad, the service life of the buffer block is relatively low, mainly because molecules in the rubber are broken under the action of solvents such as an oxidant and automobile oil in the long-term use process, the elasticity is gradually lost, even the chapping failure occurs, and the rubber is modified by the fiber or the sheet-shaped nanostructure with high modulus added in the same sense in the prior art, so that the service life of the rubber is prolonged, but the structural strength of the rubber is also increased, and the buffer performance is reduced.
How to improve the service life of the rubber material of the buffer block without affecting the buffer performance of the buffer block is a technical problem to be solved in the prior art.
Disclosure of Invention
In view of the above, the present invention provides a composite rubber material for preparing a bumper block for a vehicle, which aims to improve the service life of the bumper block while maintaining the elastic properties of rubber.
The technical scheme of the invention is realized as follows: the invention provides a composite rubber material for preparing a buffer block for a vehicle, which comprises the following components in parts by weight:
100 parts of natural rubber
10-30 Parts of coiled composite carbon fiber
0.3-5 Parts of vulcanizing agent TMTD;
The crimped composite carbon fiber comprises a crimped carbon fiber core and a Kevlar film attached to the outer surface of the carbon fiber core.
In the above embodiment, the crimped composite carbon fiber has a crimped shape, the crimped composite carbon fiber is dispersed in the natural rubber, and in the elastic deformation process of the rubber main body, the crimped composite carbon fiber deforms along with the rubber, so that energy is absorbed, the damping coefficient of the rubber is improved, meanwhile, the carbon fiber main body has good heat conducting property, the heat generating amount of the rubber in the deformation process can be reduced, and secondly, the carbon fiber has high structural strength, even if the rubber main body is partially damaged, the structural stability of the rubber main body can be maintained, so that the service life is prolonged, the carbon fiber is enabled to have a layered composite structure by the Kevlar film layer, and the carbon fiber is broken in order to avoid the huge elastic deformation process, and the Kevlar film layer is utilized to strengthen the carbon fiber, so that the elastic modulus of the crimped composite carbon fiber is greatly improved.
In some embodiments, the crimped composite carbon fibers have a diameter of 10-15 μm and the carbon fiber core has a diameter of 5-8 μm.
In some embodiments, the method of making a crimped composite carbon fiber includes the steps of:
Step one, stretching polyacrylonitrile fibers to 3 to 4 times;
Step two, heating the polyacrylonitrile fiber to 100-200 ℃, and carrying out heat preservation treatment for 1-3s to obtain a curled polyacrylonitrile fiber;
Step three, heating the crimped polyacrylonitrile fiber to 200-300 ℃ in air, and carrying out heat preservation treatment for 50-60min; heating the curled acrylonitrile fiber to 1000-3000 ℃ in inert gas atmosphere, and carrying out heat preservation treatment for 3-5min to obtain a curled carbon fiber core;
And fourthly, soaking the core part of the crimped carbon fiber in the Kevlar spinning solution, and curing to obtain the crimped composite carbon fiber.
In some embodiments, in order to obtain the carbon fiber having a curl, the polyacrylonitrile is shrunk by stretching the polyacrylonitrile fiber and then heating, and because the internal crystals of the stretched polyacrylonitrile are unevenly distributed, the polyacrylonitrile is also curved due to the uneven distribution during the shrinkage process, thereby forming a curved polyacrylonitrile fiber, and the curved polyacrylonitrile fiber is carbonized to obtain the curled carbon fiber.
In the above embodiment, the crimped carbon fiber core is immersed in the kevlar spinning dope, and then washed with cold water and dried, thereby obtaining the crimped composite carbon fiber having the kevlar layer attached to the surface.
In some embodiments, the crimped composite carbon fibers are slit prior to feeding to make the composite rubber material.
In the above embodiment, the average length of the crimped composite carbon fiber is 1 to 3mm.
In the above embodiment, the kevlar spinning dope is a kevlar sulfuric acid solution, and preferably, the concentration of the kevlar sulfuric acid solution is 1-5 (wt)%.
In some embodiments, after stretching the polyacrylonitrile fiber to 3-4 times, before heating to 100-200 ℃, the incubation for 1-3s, further comprises: and soaking the polyacrylonitrile fiber into a polyamide solution, and then drying to obtain the polyacrylonitrile fiber with the polyamide on the surface.
In the above embodiment, the crimped carbon fiber is capable of deforming with compression expansion of rubber to absorb energy, and the deformation amount of the crimped carbon fiber depends on the expansion and contraction amount thereof in one dimension, which is determined by the stretching side length on the one hand and the degree of crimping on the other hand, so that the degree of crimping is further increased by utilizing the difference of the thermal expansion rates of two materials by compounding a polyamide on the surface of polyacrylonitrile, in order to increase the elastic deformation amount thereof, the degree of crimping, which is mainly determined by the difference of the thermal expansion rates of two adjacent sections of fibers when the drawn fiber is heated, is considered, and the degree of crimping is mainly determined by the difference of the thermal expansion rates of the two sections of fibers when the drawn fiber is heated, since the stretching magnification at the former stage is only 3 to 4 times, the amount of crimping is relatively small, and since the oriented crystallization of polyacrylonitrile after transitional stretching causes the subsequent thermal shrinkage rate to decrease, the application further increases the degree of crimping by utilizing the difference of the thermal expansion rates of two materials, which includes the radian of crimping and the number of crimping in the unit length of polyacrylonitrile fiber.
In some embodiments, the polyamide solution is a formic acid solution of polyamide, preferably the concentration of the formic acid solution of polyamide is 10-20 (wt)%.
On the other hand, the invention also provides a preparation method of the composite rubber material, which comprises the following steps:
Mixing natural rubber and crimped composite carbon fiber according to parts by weight, adding into an internal mixer for internal mixing, adding a vulcanizing agent TMTD after internal mixing, and vulcanizing to obtain the composite rubber material of the vehicle buffer block.
In some embodiments, the banburying time is 3-5 hours and the banburying temperature is 210-240 ℃. .
Compared with the prior art, the composite rubber material for preparing the buffer block for the vehicle has the following beneficial effects:
The composite rubber material disclosed by the invention adopts the curled composite carbon fiber as a composite reinforcing raw material, the characteristic that the curled fiber can be stretched and bent under the action of external force is utilized, the combination stability between the rubber base material and the curled carbon fiber is improved, the problem that the carbon fiber is invalid due to separation between microcosmic phase interfaces under the action of long-term fatigue stress is avoided, the service life is prolonged, and meanwhile, the characteristic that the curled fiber absorbs energy in the bending and straightening processes can be utilized, so that the fatigue loss of the rubber material is further reduced, the damping coefficient and fatigue resistance of the rubber material are improved, and the service life is prolonged.
Detailed Description
The following description of the embodiments of the present invention will clearly and fully describe the technical aspects of the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the present invention without making any inventive effort, are intended to fall within the scope of the present invention.
Unless defined otherwise, all technical terms and science used herein have the same meaning as commonly understood by one of ordinary skill in the art to which embodiments of the present invention belong. If the definitions set forth in this section are contrary to or otherwise inconsistent with the definitions set forth in the patents, patent applications, published patent applications and other publications incorporated herein by reference, the definitions set forth in this section are preferentially set forth in the definitions set forth herein.
The composite rubber material of the present invention will now be described with reference to specific examples:
Example 1
Preparation of crimped composite carbon fiber:
Heating polyacrylonitrile fiber precursor to 120 ℃, carrying out stretching treatment, wherein the stretching multiplying power is 3 times, cooling to 25 ℃ after stretching, then heating to 150 ℃ again under the condition of no stretching force, carrying out heat preservation treatment for 1s to obtain curled acrylonitrile fiber, continuously heating the curled acrylonitrile fiber to 250 ℃, carrying out heat preservation treatment for 50min, transferring the curled acrylonitrile fiber into a closed cavity, keeping the cavity in a nitrogen atmosphere, heating to 1500 ℃, carrying out heat preservation treatment for 3min, slowly cooling to room temperature, taking out to obtain curled carbon fiber, wherein the diameter of the carbon fiber is 5 mu m, preparing a Kevlar sulfuric acid solution with the mass concentration of 1%, soaking the curled carbon fiber in the Kevlar sulfuric acid solution, washing with water, and then drying in an oven at 150 ℃ to obtain carbon fiber with Kevlar attached to the surface, and the diameter of the carbon fiber with Kevlar attached to the surface is 10 mu m.
Cutting the carbon fiber with the Kevlar attached on the surface into short fibers with the length of 1-3mm by a short cutter, mixing the natural rubber and the short-cut curled composite carbon fiber according to the mass ratio of 100:10, adding the mixture into an internal mixer for banburying at the temperature of 210 ℃ for 3 hours, adding a vulcanizing agent TMTD, heating the mixture to 150 ℃ according to the mass ratio of 0.3:100, and extruding the mixture by an extruder to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Example 2
Preparation of crimped composite carbon fiber:
Heating polyacrylonitrile fiber precursor to 120 ℃, carrying out stretching treatment, wherein the stretching multiplying power is 4 times, cooling to 25 ℃ after stretching, then heating to 100 ℃ again under the condition of no stretching force, carrying out heat preservation treatment for 3s to obtain curled acrylonitrile fiber, continuously heating the curled acrylonitrile fiber to 200 ℃, carrying out heat preservation treatment for 60min, transferring the curled acrylonitrile fiber into a closed cavity, keeping the cavity in a nitrogen atmosphere, heating to 1000 ℃, carrying out heat preservation treatment for 5min, slowly cooling to room temperature, taking out to obtain curled carbon fiber, wherein the diameter of the carbon fiber is 8 mu m, preparing a Kevlar sulfuric acid solution with the mass concentration of 5%, soaking the curled carbon fiber in the Kevlar sulfuric acid solution, washing with water, and then drying in an oven at 150 ℃ to obtain carbon fiber with Kevlar attached to the surface, and the diameter of the carbon fiber with Kevlar attached to the surface is 12 mu m.
Cutting the carbon fiber with the Kevlar attached on the surface into short fibers with the length of 1-3mm by a short cutter, mixing the natural rubber and the short-cut curled composite carbon fiber according to the mass ratio of 100:20, adding the mixture into an internal mixer for banburying at the temperature of 240 ℃ for 5 hours, adding a vulcanizing agent TMTD, heating the mixture to the temperature of 150 ℃ according to the mass ratio of 1:100, and extruding the mixture by an extruder to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Example 3
Preparation of crimped composite carbon fiber:
Heating polyacrylonitrile fiber precursor to 120 ℃, carrying out stretching treatment, wherein the stretching multiplying power is 3.5 times, cooling to 25 ℃ after stretching, then heating to 200 ℃ again under the condition of no stretching force, carrying out heat preservation treatment for 1s to obtain curled acrylonitrile fiber, continuously heating the curled acrylonitrile fiber to 300 ℃, carrying out heat preservation treatment for 50min, transferring the curled acrylonitrile fiber into a closed cavity, keeping the cavity in a nitrogen atmosphere, heating to 3000 ℃, carrying out heat preservation treatment for 3min, slowly cooling to room temperature, taking out to obtain curled carbon fiber, wherein the diameter of the carbon fiber is 7 mu m, preparing a Kevlar sulfuric acid solution with the mass concentration of 3%, soaking the curled carbon fiber in the Kevlar sulfuric acid solution, washing with water, and then drying in an oven at 150 ℃ to obtain carbon fiber with Kevlar attached to the surface and the diameter of the carbon fiber attached with Kevlar being 14 mu m.
Cutting the carbon fiber with the Kevlar attached on the surface into short fibers with the length of 1-3mm by a short cutter, mixing the natural rubber and the short-cut curled composite carbon fiber according to the mass ratio of 100:15, adding the mixture into an internal mixer for banburying at 220 ℃ for 4 hours, adding a vulcanizing agent TMTD, heating the mixture to 150 ℃ according to the mass ratio of 2:100, and extruding the mixture by an extruder to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Example 4
Preparation of crimped composite carbon fiber:
Heating polyacrylonitrile fiber precursor to 120 ℃, carrying out stretching treatment, wherein the stretching multiplying power is 3.5 times, cooling to 25 ℃ after stretching, carrying out soaking treatment on the stretched polyacrylonitrile fiber in a polyamide formic acid solution with the mass concentration of 10%, then carrying out drying treatment, then carrying out heating to 200 ℃ again under the condition of no stretching force, carrying out heat preservation treatment for 1s to obtain curled acrylonitrile fiber, continuously heating the curled acrylonitrile fiber to 300 ℃, carrying out heat preservation treatment for 50min, transferring the curled acrylonitrile fiber into a closed cavity, keeping the cavity in a nitrogen atmosphere, heating to 3000 ℃, carrying out heat preservation treatment for 3min, slowly cooling to room temperature, taking out to obtain curled carbon fiber, wherein the diameter of the carbon fiber is 5 mu m, preparing a Kevlar sulfuric acid solution with the mass concentration of 3%, carrying out soaking treatment on the curled carbon fiber in a Kevlar sulfuric acid solution, washing and then drying in an oven at 150 ℃ to obtain carbon fiber with the surface attached with Kevlar and the diameter of the carbon fiber attached to 15 mu m.
Cutting the carbon fiber with the Kevlar attached on the surface into short fibers with the length of 1-3mm by a short cutting machine, mixing natural rubber and the short-cut curled composite carbon fiber according to the mass ratio of 100:15, adding the short-cut curled composite carbon fiber into an internal mixer for banburying at 220 ℃ for 4 hours, adding a vulcanizing agent TMTD, heating the vulcanizing agent TMTD to the natural rubber according to the mass ratio of 3:100, and extruding the mixture by an extruder after mixing to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Example 5
Preparation of crimped composite carbon fiber:
Heating polyacrylonitrile fiber precursor to 120 ℃, carrying out stretching treatment, wherein the stretching multiplying power is 3.5 times, cooling to 25 ℃ after stretching, carrying out soaking treatment on the stretched polyacrylonitrile fiber in a polyamide formic acid solution with the mass concentration of 20%, then carrying out drying treatment, then carrying out heating to 200 ℃ again under the condition of no stretching force, carrying out heat preservation treatment for 1s to obtain curled acrylonitrile fiber, continuously heating the curled acrylonitrile fiber to 300 ℃, carrying out heat preservation treatment for 50min, transferring the curled acrylonitrile fiber into a closed cavity, keeping the cavity in a nitrogen atmosphere, heating to 3000 ℃, carrying out heat preservation treatment for 3min, slowly cooling to room temperature, taking out to obtain curled carbon fiber, wherein the diameter of the carbon fiber is 5 mu m, preparing a Kevlar sulfuric acid solution with the mass concentration of 3%, carrying out soaking treatment on the curled carbon fiber in a Kevlar sulfuric acid solution, washing and then drying in an oven at 150 ℃ to obtain carbon fiber with the surface attached with Kevlar and the diameter of the carbon fiber attached to 15 mu m.
Cutting the carbon fiber with the Kevlar attached on the surface into short fibers with the length of 1-3mm by a short cutter, mixing the natural rubber and the short-cut curled composite carbon fiber according to the mass ratio of 100:15, adding the mixture into an internal mixer for banburying at 220 ℃ for 4 hours, adding a vulcanizing agent TMTD, heating the mixture to 150 ℃ according to the mass ratio of 5:100, and extruding the mixture by an extruder to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Comparative example 1
Mixing natural rubber and chopped carbon fiber according to the mass ratio of 100:15, adding the mixture into an internal mixer for processing, wherein the internal mixing temperature is 220 ℃, the internal mixing time is 4 hours, then adding a vulcanizing agent TMTD, the mass ratio of the vulcanizing agent TMTD to the natural rubber is 2:100, heating to 150 ℃, and extruding by an extruder after mixing to obtain the composite rubber material.
Preparing a buffer block:
the obtained composite rubber material is prepared into a general buffer block special for trucks with the gross weight of 500g in an extrusion mode.
Comparative example 2
Preparing a buffer block:
mixing natural rubber with a vulcanizing agent TMTD, heating the mixture to 150 ℃ according to the mass ratio of the vulcanizing agent TMTD to the natural rubber of 2:100, extruding the mixture by an extruder to obtain a composite rubber material, and preparing the composite rubber material into a universal buffer block special for trucks with the gross weight of 500g by an extrusion mode.
Respectively carrying out 50 ten thousand times of fatigue treatment on the prepared buffer blocks, wherein the fatigue loading sinusoidal force has a peak value of 5N and a frequency of 2Hz, and respectively carrying out statistical calculation on the height, the radial diameter, the surface crack and the compression deformation of the buffer blocks before and after fatigue to obtain the results shown in the following table:
| Grouping | Height before fatigue | Post fatigue height | Diameter before fatigue | Post fatigue diameter |
| Example 1 | 50mm | 48.8 | 33mm | 33.4 |
| Example 2 | 50mm | 49.1 | 33mm | 33.3 |
| Example 3 | 50mm | 49.0 | 33mm | 33.3 |
| Example 4 | 50mm | 49.4 | 33mm | 33.2 |
| Example 5 | 50mm | 49.4 | 33mm | 33.1 |
| Comparative example 1 | 50mm | 47.8 | 33mm | 33.8 |
| Comparative example 2 | 50mm | 46.2 | 33mm | 34.2 |
The data show that compared with the conventional rubber buffer block and the conventional carbon fiber composite rubber buffer block, the buffer block prepared from the composite rubber can greatly reduce fatigue deformation.
The following data were obtained by calculation of the surface crack observation and compression set, wherein the compression set was 100% of the compression height/pre-fatigue height.
The data show that the buffer block adopting the embodiment of the invention has good service life and stability, and can still keep good appearance stability and performance stability after long-time high-strength fatigue treatment compared with the conventional carbon fiber composite rubber buffer block, and has remarkable performance advantages compared with the conventional rubber buffer block.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (5)
1. The composite rubber material for preparing the buffer block for the vehicle is characterized by comprising the following components in parts by weight:
100 parts of natural rubber
10-30 Parts of coiled composite carbon fiber;
0.3-5 parts of vulcanizing agent TMTD;
The crimped composite carbon fiber comprises a carbon fiber core part and a Kevlar film attached to the carbon fiber core part, wherein the crimped composite carbon fiber has a diameter of 10-15 mu m and a length of 1-3mm, the diameter of the carbon fiber core part is 5-8 mu m, and the preparation method of the crimped composite carbon fiber comprises the following steps: stretching polyacrylonitrile fiber to 3-4 times, heating to 100-200 ℃, carrying out heat preservation treatment for 1-3s to obtain curled polyacrylonitrile fiber, heating the curled polyacrylonitrile fiber to 200-300 ℃ in air, and carrying out heat preservation treatment for 50-60min; and heating the crimped polyacrylonitrile fiber to 1000-3000 ℃ in an inert gas atmosphere, carrying out heat preservation treatment for 3-5 min to obtain a crimped carbon fiber core, soaking the crimped carbon fiber core in a Kevlar spinning solution, and curing to obtain the crimped composite carbon fiber.
2. The composite rubber material for preparing a cushion block for a vehicle according to claim 1, wherein after stretching the polyacrylonitrile fiber 3 to 4 times, before heating to 100 to 200 ℃ and heat-insulating treatment for 1 to 3s, the composite rubber material further comprises immersing the polyacrylonitrile fiber in a polyamide solution and then drying to obtain the polyacrylonitrile fiber having a polyamide on the surface.
3. The composite rubber material for producing a cushion block for a vehicle according to claim 2, wherein the polyamide solution is a formic acid solution of polyamide.
4. A method for producing a composite rubber material for producing a cushion block for a vehicle according to any one of claims 1 to 3, characterized by comprising the steps of:
Mixing natural rubber and crimped composite carbon fiber according to parts by weight, adding into an internal mixer for internal mixing, adding a vulcanizing agent TMTD after internal mixing, and obtaining the composite rubber material of the vehicle buffer block after vulcanization treatment.
5. The method for preparing a composite rubber material for a bumper block for a vehicle according to claim 4, wherein the banburying time is 3 to 5 hours and the banburying temperature is 210 to 240 ℃.
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| JP3737849B2 (en) * | 1996-03-31 | 2006-01-25 | 大阪瓦斯株式会社 | Method for producing carbon fiber three-dimensional structure |
| JP3215656B2 (en) * | 1997-09-01 | 2001-10-09 | 栖二 元島 | Method and apparatus for producing coiled carbon fiber |
| JP4535808B2 (en) * | 2003-08-26 | 2010-09-01 | 昭和電工株式会社 | Crimped carbon fiber and its production method |
| CN100503913C (en) * | 2003-08-26 | 2009-06-24 | 昭和电工株式会社 | Crimped carbon fiber and production method thereof |
| TW200508431A (en) * | 2003-08-26 | 2005-03-01 | Showa Denko Kk | Crimped carbon fiber and production method thereof |
| JP5935299B2 (en) * | 2011-11-16 | 2016-06-15 | 東レ株式会社 | Fiber-reinforced composite material and method for producing fiber-reinforced composite material. |
| CN108864773B (en) * | 2018-06-13 | 2020-07-24 | 四川理工学院 | A modified helical carbon nanofiber, its preparation method and application, and a rubber composite material |
| CN113861459B (en) * | 2021-11-25 | 2023-07-21 | 四川轻化工大学 | A kind of helical nano carbon fiber reinforced rubber composite material and preparation method thereof |
| CN114771055B (en) * | 2022-05-19 | 2022-11-15 | 广州市铭成橡塑科技有限公司 | Spiral nanofiber reinforced composite rubber pad |
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| 李安玲 ; 孔令豪 ; 李占君 ; 张勇 ; 王广飞 ; 亓明 ; .短切碳纤维对天然橡胶/顺丁橡胶复合材料性能的影响.合成橡胶工业.2020,(02),全文. * |
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