CN108467550B - Graphene-containing butyl rubber nanocomposite and dynamic heat generation detection method thereof - Google Patents
Graphene-containing butyl rubber nanocomposite and dynamic heat generation detection method thereof Download PDFInfo
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Abstract
The invention provides a butyl rubber nano composite material containing graphene and a dynamic heat generation detection method thereof. The graphene-containing butyl rubber nanocomposite greatly improves the damping performance of butyl rubber, obviously improves the sound insulation performance and the heat conduction performance of butyl rubber, and has the advantages which cannot be achieved by the traditional filler. The invention also provides a dynamic heat generation detection method of the butyl rubber containing the graphene, and the fiber grating sensor implanted in the butyl rubber structural member can monitor the internal temperature change of the rubber structural member in the dynamic service process in real time on line. Compared with the surface temperature detection method of the existing rubber structural member, the scheme for monitoring the internal temperature of the rubber structural member on line in real time has obvious progress. The material preparation and temperature detection method provided by the invention is simple and reliable, has a wide application range and strong practicability, and has good economic and social benefits.
Description
Technical Field
The invention belongs to the technical field of rubber materials, and relates to a butyl rubber nano composite material containing graphene and a dynamic heat generation detection method thereof.
Background
Vibration and noise are ubiquitous in various areas of production and life as contemporary worldwide problems. Among the measures for reducing vibration and noise, adding vibration-reducing and damping elements and sound-absorbing materials into machines which are easy to generate vibration and noise has become the most effective scheme for reducing vibration and noise.
At present, a plurality of polymer materials which meet the requirements and have excellent comprehensive properties are widely applied. The polymer materials have viscoelastic and internal damping characteristics, which are beneficial to simultaneously introducing damping and sound absorption mechanisms into the materials and obviously improving the vibration attenuation and sound absorption performance of the materials. Butyl Rubber (IIR) is a high molecular material with excellent performance, which is generated by carrying out cationic polymerization reaction on isobutene and Isoprene under the action of Friedel-Craft catalyst. The special molecular structure of the butyl rubber enables the internal friction and viscous loss of the butyl rubber to be large, so that the butyl rubber is a preferred material in the application field of vibration reduction and noise reduction.
Graphene is a carbon atom sp2The hybridized and arranged monoatomic layer is a flaky two-dimensional crystal which is arranged in a hexagonal annular honeycomb manner, graphene has an infinitely repeated periodic structure in a plane, and has only nanoscale in a direction perpendicular to the plane, the theoretical thickness of the graphene is only 0.335nm, and the graphene is a nano filler with macroscopic scale. The modulus of the graphene can be as high as 1TPa, the strength can be 130GPa, and the specific surface area can be 2630m2.g-1An aspect ratio of more than 1000 and an ultrahigh thermal conductivity (3000-5000 W.m.)-1.K-1) And conductivity (200000 cm)2.V-1.s-1). This indicates that graphene has great potential advantages in the aspects of high-efficiency enhancement and functionalization of high molecular materials. The excellent physical and mechanical properties of the graphene are utilized to provide good sound absorption, damping and heat conduction properties for the rubber matrix.
The main mechanism of vibration reduction and noise reduction is to convert vibration and sound energy into energy in other forms for dissipation, usually into heat energy, by utilizing viscous internal friction of a high polymer material under dynamic load, and finally cause temperature rise of a damping structural member. Therefore, the butyl rubber nanocomposite containing graphene is prepared by combining the respective advantages of butyl rubber and graphene nanomaterials, and the viscoelastic internal damping and heat-conducting properties of butyl rubber can be remarkably improved.
In view of the viscoelastic property of the rubber material, even if the thermal conductivity of the rubber material is improved by adding the graphene nano material, the phenomena of heat generation and severe temperature rise of the rubber structural member under dynamic load are difficult to avoid, which can seriously affect the service performance of the rubber damping structural member. Therefore, the heat generation state of the rubber structural part in the using process needs to be monitored on line in real time, and the long-term use performance of the rubber structural part is further evaluated. At present, the scheme of infrared thermography is commonly used for monitoring the heat generation state of a rubber structural part in real time, and when the scheme is used for monitoring the temperature of the structural part, the temperature of the structural part can only be limited to the surface temperature of the structural part, but the monitoring of the internal temperature of the structural part cannot be realized. However, in the case of a relatively large-sized structural member, the internal temperature is significantly higher than the surface temperature, so that it is difficult to estimate the heat generation state inside the rubber structural member by measuring the surface temperature of the structural member.
In order to monitor the conditions of heat generation and temperature rise inside a rubber sample, the conventional scheme is to punch a hole on the rubber sample and extend a needle-shaped temperature measuring sensor into the rubber sample for measurement. Chinese patent CN 104569041 a discloses a compression heat generation detector, which improves the existing Goodrich rubber compression heat generation tester, and avoids the disadvantage that the existing tester can not accurately measure the central temperature of the core of the sample in real time. However, in the measurement scheme of the compression test, the rubber structural member is inevitably subjected to hole opening operation, so that the structural integrity of the original rubber structural member is damaged, and the stress-strain state of the rubber structural member is inevitably changed in the loading process. In addition, when the temperature rise is measured by punching holes on the rubber structural member, only one point of the temperature inside the structural member can be measured when one hole is punched on the rubber structural member, and the temperature change conditions of a plurality of parts inside the structural member cannot be monitored simultaneously.
Disclosure of Invention
In order to overcome the defects, the invention provides the butyl rubber nanocomposite containing graphene, which has the advantages of better graphene dispersibility, simple process, good stability and easy realization of engineering; and aiming at the defect of internal temperature rise measurement of the conventional rubber structural member under dynamic load, a dynamic heat generation monitoring method of the butyl rubber nanocomposite containing graphene is provided, and the temperature change of the rubber structural member in the dynamic service process is monitored in real time on the premise of ensuring the integrity of the structural member through a fiber grating temperature sensor implanted in the butyl rubber structural member.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a graphene-butyl rubber nanocomposite structural member with a built-in fiber grating temperature sensor comprises the following steps:
1) arranging fiber gratings on a forming die with a groove for a fiber lead wire reserved in advance, and leading the fiber lead wire out of the groove of the die lead wire;
2) filling the butyl rubber nano composite material rubber compound containing graphene into a mould, and completely coating the fiber grating temperature sensor;
3) carrying out high-temperature vulcanization molding on the mold;
the grating area of the fiber grating is packaged by a stainless steel capillary;
the graphene-containing butyl rubber nanocomposite material is prepared from the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 3-8 parts of zinc oxide, 1-3 parts of stearic acid, 10-30 parts of carbon black, 20-40 parts of alumina hollow microspheres, 5-15 parts of graphene paraffin oil, 1-4 parts of an anti-aging agent, 1-3 parts of a promoter and 1-3 parts of sulfur;
wherein the graphene paraffin oil is a mixture of graphene and paraffin oil,
the anti-aging agent comprises: 2,2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD) and N- (1, 3-dimethyl) butyl-N' -phenyl-p-phenylenediamine (antioxidant DMPPD).
The existing rubber material has better tensile property, and generally, a fiber grating sensor is rarely implanted so as to prevent the sensor from being damaged or prevent the measurement result from generating larger deviation in the rubber tensile process. In order to overcome the problems, the method adopts the stainless steel capillary tube to package the grating region, simultaneously effectively improves the mechanical and damping properties of the butyl rubber by utilizing the doping of the graphene and the adjustment of the formula of the raw materials, ensures that the implanted fiber grating sensor has good compatibility with the base material, and has the following experimental results: the structural member prepared by the method can realize accurate measurement of the internal temperature rise of the structural member under dynamic load.
Preferably, the feed consists of the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 3-5 parts of zinc oxide, 1-2 parts of stearic acid, 10-20 parts of carbon black, 20-30 parts of alumina hollow microspheres, 5-10 parts of graphene paraffin oil, 1-2.5 parts of an anti-aging agent, 1-2 parts of an accelerator and 1-2 parts of sulfur.
Preferably, the feed consists of the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 5-8 parts of zinc oxide, 2-3 parts of stearic acid, 20-30 parts of carbon black, 30-40 parts of alumina hollow microspheres, 10-15 parts of graphene paraffin oil, 2.5-4 parts of an anti-aging agent, 2-3 parts of a promoter and 2-3 parts of sulfur.
Different from the common graphene modified butyl rubber, the graphene-containing butyl rubber nanocomposite prepared by using the raw materials of the present application has the following advantages: in the vulcanization process, the rubber substrate and the copper plating layer on the surface of the stainless steel capillary tube form a strong chemical bond, and the sufficient interface strength between the rubber substrate and the copper plating layer is ensured.
Preferably, the graphene is multilayer flaky graphene, the diameter of the graphene is 2-20 micrometers, and the number of layers is 2-50;
preferably, the paraffin oil has the viscosity range of 5000-7000 cps;
preferably, the diameter of the alumina hollow microsphere is 0.4-1.5 microns, and the bulk density is 0.5-1.0 g/cm3。
The invention also provides a preparation method of the graphene-containing butyl rubber nanocomposite, which comprises the following steps:
1) mixing graphene and paraffin oil, and stirring at a high speed at a certain temperature to obtain graphene paraffin oil;
2) banburying: sequentially adding butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, alumina hollow microspheres, graphene paraffin oil and an anti-aging agent into an internal mixer, and discharging after internal mixing for a certain time to obtain an internal mixing blend;
3) adding a vulcanizing agent: and adding the banburying blend into an open mill, adding an accelerator and sulfur, and mixing for a certain time to obtain the butyl rubber nanocomposite containing graphene.
Wherein, preferably, the unsaturation degree of the raw butyl rubber is not less than 1.75 mol%;
preferably, the carbon black is thermal cracking carbon black;
preferably, the promoter is one or a combination of the following substances: tetramethylthiuram disulfide, dibenzothiazyl disulfide.
The invention also provides the butyl rubber nanocomposite containing graphene prepared by any one of the methods.
The invention also provides the graphene-butyl rubber nanocomposite structural member with the built-in fiber grating prepared by any one of the methods.
The invention also provides a dynamic temperature rise monitoring system for the vibration reduction structural part, which comprises: a light source, a vibration device, the graphene-butyl rubber nanocomposite structural component with the built-in fiber grating, an optical fiber lead, an optical fiber coupler, a fiber grating demodulator and a computer processor; the graphene-butyl rubber nanocomposite structural component with the built-in fiber grating is arranged on a vibrating device and connected with a fiber coupler through a fiber lead, the fiber coupler is further connected with a light source and a fiber grating demodulator respectively, and the fiber grating demodulator is connected with a computer processor.
The invention has the advantages of
(1) The butyl rubber nano composite material containing graphene obviously improves the mechanical and damping properties of butyl rubber, and particularly greatly improves the sound absorption and sound insulation properties of butyl rubber due to the structural characteristics of graphene, so that the butyl rubber nano composite material has incomparable advantages compared with traditional fillers.
(2) The butyl rubber nanocomposite containing graphene provided by the invention utilizes the excellent heat-conducting property of the graphene nanomaterial, so that the heat-conducting property of the prepared butyl rubber nanocomposite structural member is obviously improved, the temperature rise of the vibration-damping structural member is obviously reduced when the dynamic load is borne, and the durability of the vibration-damping rubber structural member is favorably improved.
(3) The temperature rise monitoring method of the graphene-butyl rubber vibration reduction structural member can accurately measure the temperature change process in the rubber on the basis of ensuring the integrity of the rubber structural member, and further can judge whether the rubber structural member is damaged or not, so that the aim of monitoring the service condition of the structural member is fulfilled. This is incomparable with the existing or widely used monitoring schemes, and the method of the invention has outstanding advantages and obvious progress.
(4) The material preparation method and the dynamic temperature rise monitoring method adopted by the invention have the advantages of simple operation, good test stability, convenience for engineering production, wide application range and better economic benefit and social benefit.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the application and, together with the description, serve to explain the application and are not intended to limit the application.
Fig. 1 is a schematic cross-sectional view of a graphene-butyl rubber nanocomposite structural member containing an embedded fiber grating sensor according to the present invention.
101-stainless steel capillary with copper plated on the surface, 102-fiber grating temperature sensor, 103-graphene-butyl rubber nanocomposite structural component and 104-fiber grating lead.
Fig. 2 is a schematic view of monitoring of dynamic heat generation of graphene-butyl rubber nanocomposite.
201-a light source, 202-a fiber coupler, 203-a sample fixing and loading device, 204-a graphene-butyl rubber nanocomposite structural component, 205-a fiber grating temperature sensor, 206-a computer processor and 207-a fiber grating demodulator.
FIG. 3 is a cloud chart of finite element simulation results of a temperature field of a rubber structural member under dynamic load.
Detailed Description
It should be noted that the following detailed description is exemplary and is intended to provide further explanation of the disclosure. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present application. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
The present invention will be further described with reference to specific examples.
The technical scheme of the invention is as follows:
the butyl rubber nano composite material containing graphene is a mixture of butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, alumina hollow microspheres, graphene paraffin oil, an anti-aging agent, an accelerator and sulfur, and the butyl rubber nano composite material contains the following components in parts by mass in a formula: 100 parts of butyl rubber raw rubber, 3-8 parts of zinc oxide, 1-3 parts of stearic acid, 10-30 parts of carbon black, 20-40 parts of alumina hollow microspheres, 5-15 parts of graphene paraffin oil, 1-4 parts of an anti-aging agent, 1-3 parts of an accelerator and 1-3 parts of sulfur.
The graphene paraffin oil is a uniform mixture of graphene and paraffin oil.
The anti-aging agent comprises: 2,2, 4-trimethyl-1, 2-dihydroquinoline polymer (antioxidant RD) and N- (1, 3-dimethyl) butyl-N' -phenyl-p-phenylenediamine (antioxidant DMPPD).
The graphene is multilayer flaky graphene, the diameter of the graphene is 2-20 micrometers, and the number of layers is 2-50.
The viscosity range of the paraffin oil is 5000-7000 cps; if the viscosity of the paraffin oil is too high, the graphene and the paraffin oil are difficult to be uniformly stirred when being mixed, and the graphene is seriously agglomerated; if the viscosity of the paraffin oil is very low, the graphene is re-aggregated even if the graphene is kept stand for a short time after the graphene and the paraffin oil are stirred and dispersed; through repeated tests, the viscosity of the paraffin oil is preferably 5000-7000 cps.
The preparation method of the graphene paraffin oil comprises the following steps: placing graphene and paraffin oil in a container in sequence according to the mass part ratio of 20: 100-50: 100, stirring by adopting a high-speed rotary stirrer at the temperature of 30-70 ℃, stirring at the rotating speed of 200-1200 rpm for 0.5-5 h, and standing for 0.5h without re-aggregation or precipitation, thereby obtaining the uniformly mixed graphene paraffin oil.
The unsaturation degree of the raw butyl rubber is not less than 1.75 mol%.
The carbon black is thermal cracking carbon black.
The diameter of the alumina hollow microsphere is 0.4-1.5 microns, and the bulk density is 0.5-1.0 g/cm3。
The accelerant is one or the combination of the following substances: tetramethylthiuram disulfide (accelerator TMTD), dibenzothiazyl disulfide (accelerator DM).
A dynamic heat generation monitoring system of a graphene-butyl rubber nanocomposite vibration reduction structural member is characterized in that a fiber grating sensor is implanted into the structural member before a butyl rubber structural member is vulcanized and formed, and the butyl rubber structural member with the embedded fiber grating temperature sensor is formed after the butyl rubber structural member is formed.
The specific preparation and temperature rise monitoring steps of the graphene-butyl rubber nanocomposite structural member are as follows:
(1) preparing a fiber grating temperature sensor: according to the requirement of the internal temperature test of the rubber structural part, a plurality of grating areas are distributed on each continuous optical fiber, and all the grating areas are packaged by adopting a fine copper-plated stainless steel capillary tube;
each optical fiber is provided with a lead connector so as to be connected with the fiber grating demodulator conveniently;
the number of grating areas distributed on each optical fiber and the distance between adjacent gratings are set according to the test requirement of temperature rise, and the size range of each grating area is 5-8 mm;
the surface of the stainless steel capillary tube is plated with copper-zinc alloy, and the copper-zinc alloy is used for improving the interface strength between rubber and the stainless steel capillary tube in the forming process; the outer diameter of the stainless steel capillary tube is 0.5-1 mm, and the wall thickness is 0.2-0.4 mm;
(2) preparing materials: weighing various raw materials for preparing the graphene-butyl rubber composite material according to a formula;
(3) banburying: sequentially adding butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, alumina hollow microspheres, graphene paraffin oil and an anti-aging agent into an internal mixer within 30min, controlling the mixing temperature to be 70-100 ℃, internally mixing for 5-40 min, and discharging to obtain an internally mixed blend;
(4) adding a vulcanizing agent: adding the banburying blend into an open mill, adding an accelerant and sulfur, controlling the roll temperature to be 40-50 ℃, and mixing for 10-20 min;
(5) arrangement of fiber grating: according to specific temperature measurement requirements, arranging fiber gratings on a forming die with a groove reserved for an optical fiber lead wire, and leading the optical fiber lead wire out of the groove of the die lead wire;
(6) filling and coating: filling a prepared graphene-butyl rubber compound into a mold, and completely coating the fiber grating temperature sensor;
(7) and (3) vulcanization molding: placing a vulcanizing mold in a vulcanizing machine for high-temperature vulcanization molding, wherein rubber in the mold is in a viscous state at the initial stage of vulcanization, the stainless steel capillary tube internally sleeved with the fiber grating is tightly wrapped, and a strong chemical bond is formed between a rubber matrix and a copper coating on the surface of the stainless steel capillary tube in the vulcanization process, so that the interface strength between the rubber matrix and the stainless steel capillary tube is ensured;
(8) monitoring the dynamic temperature rise of the vibration reduction structural part: installing the molded butyl rubber vibration reduction structural part with the temperature sensor, and connecting an optical fiber lead with equipment such as an optical fiber coupler, an optical fiber grating demodulator, a computer processor and the like, wherein a light source can send out an optical signal, the optical signal can be transmitted to the optical fiber grating sensor, reflected after interaction between light and a grating and then transmitted to the optical fiber grating demodulator, and the change of the optical center wavelength is demodulated by the optical fiber grating demodulator; when the vibration reduction structural member bears dynamic load, the internal temperature of the structural member continuously rises along with the increase of the number of times of cyclic load, the fiber grating demodulator receives reflected light signals and identifies the change of the optical center wavelength, and the accurate temperature change is obtained through the conversion of the computer processor, so that the temperature change condition of the monitored point in the butyl rubber structural member is obtained.
The material theory of the invention is as follows: the graphene has excellent mechanical property, extremely high specific surface area and a topological structure with folds in nanometer size, so that the graphene has larger contact area and stronger binding force with rubber, thereby effectively improving the strength of the rubber and keeping the high flexibility of the rubber; the graphene sheet layer forms a micro-nano constraint layer in a butyl rubber matrix, and when the rubber material is subjected to vibration deformation, rubber molecules are subjected to shear deformation, so that a large loss factor and a wide damping function temperature range are generated; more importantly, the graphene has a remarkable enhancing effect on viscoelastic internal damping and heat conducting performance of the butyl rubber, and is beneficial to converting vibration and sound energy into heat energy to be dissipated when being transmitted into a rubber matrix, so that the butyl rubber nanocomposite containing the graphene has better vibration reduction and sound absorption performance and has better heat conductivity compared with a common rubber material.
The temperature measuring principle of the embedded fiber bragg grating temperature sensor is as follows: when the temperature of the environment where the fiber grating is located changes, the central wavelength of the reflected light of the grating changes under the actions of an elasto-optical effect, a thermo-optical effect, thermal expansion and the like; the offset of the optical center wavelength has a corresponding relation with the temperature variation; all grating areas in the fiber grating sensor are packaged by a stainless steel capillary tube plated with copper and then embedded in a vibration reduction rubber structural member, the grating areas are subjected to thermal expansion due to the temperature rise in the rubber structural member, an optical signal transmitted by a light source interacts with the fiber grating, reflected light enters a fiber grating demodulator through an optical fiber coupler, the fiber grating demodulator demodulates the change of the central wavelength of light, and the fiber grating demodulator is connected with a computer processor to obtain an accurate temperature digital signal and output and display the accurate temperature digital signal.
Examples 1-3 and comparative example 1:
table 1 shows the mass part ratio of the rubber formulas of examples 1-3 and comparative example 1, and the unsaturation degree of the used raw butyl rubber is 1.75 mol%; the diameter of graphene in the used graphene paraffin oil is 5 micrometers, the number of layers is 5, and the viscosity of the paraffin oil is 5000 cps; in the preparation process of the graphene paraffin oil, the mass part ratio of graphene to paraffin oil is 20:100, the rotating speed of a high-speed rotary stirrer is 800rpm at the temperature of 50 ℃, and the stirring time is 0.5 h.
The specific preparation and temperature rise monitoring steps of the graphene-butyl rubber nanocomposite structural member described in the embodiments 1-3 and the comparative example 1 are as follows:
(1) preparing a fiber grating temperature sensor: according to the requirement, the temperature change state of the central point in the cylindrical rubber structural part 103 is tested, a grating area 102 is carved on a continuous optical fiber 104 in advance, and a fine copper-plated stainless steel capillary 101 is adopted to package the grating area, wherein the outer diameter of the stainless steel capillary is 0.7mm, and the wall thickness is 0.2 mm.
(2) Preparing materials: weighing various raw materials for preparing the graphene-butyl rubber composite material according to the formula in the table 1.
(3) Banburying: adding butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, alumina hollow microspheres, graphene paraffin oil and an anti-aging agent into an internal mixer in sequence within 30min, controlling the internal mixing temperature to be 70-100 ℃, and discharging after internal mixing for 5-40 min to obtain an internal mixing blend.
(4) Adding a vulcanizing agent: and adding the banburying blend into an open mill, adding an accelerant and sulfur, controlling the roll temperature to be 40-50 ℃, and mixing for 10-20 min.
(5) Arrangement of fiber grating: and (2) according to the temperature measurement requirement in the step (1), arranging the fiber bragg grating on the forming die with the groove for the fiber lead wire reserved in advance, and leading out the fiber lead wire interface from the die lead wire groove.
(6) Filling and coating: filling the prepared graphene-butyl rubber compound into a mold, and completely coating the fiber grating temperature sensor.
(7) And (3) vulcanization molding: placing the vulcanization mold on a vulcanizing machine for vulcanization at the vulcanization temperature of 140 ℃ for 30min, thus obtaining a butyl rubber sample; in the initial stage of vulcanization, the rubber in the mold is in a viscous state, the stainless steel capillary tube internally sleeved with the fiber grating is tightly wrapped, and in the vulcanization process, the rubber matrix and the copper plating layer on the surface of the stainless steel capillary tube 101 form a strong chemical bond, so that the interface strength between the rubber matrix and the stainless steel capillary tube is ensured.
(8) Monitoring the dynamic temperature rise of the vibration reduction structural part: mounting a molded cylindrical butyl rubber vibration reduction structural part 204 with a temperature sensor on a vibration device 203, and connecting a fiber grating lead wire 104 with equipment such as a light source 201, a fiber grating demodulator 207, a fiber coupler 202, a computer processor 206 and the like, wherein the light source 201 can send out an optical signal which is transmitted to the fiber grating sensor 205, reflected after interaction between light and grating, transmitted to the fiber grating demodulator 207 and demodulated to change of the light center wavelength; when the vibration is carried out, the cylindrical vibration reduction structural member 204 (namely, the graphene-butyl rubber nanocomposite structural member) bears dynamic load, the internal temperature of the structural member is continuously increased along with the increase of the number of times of cyclic load, the fiber grating demodulator receives a continuously changed reflected light signal and demodulates the change of the central wavelength of light, the reflected light signal is processed by the computer processor 206, and the accurate temperature change is obtained, namely the temperature increase condition of the central point in the butyl rubber structural member is obtained.
The prepared butyl rubber sample was subjected to a performance test, and the test results are shown in table 1.
TABLE 1 composition parts by mass ratio of examples 1 to 3 and comparative example 1 and performance test results thereof
As can be seen, the loss factors for characterizing the damping and vibration-damping performance of the material are higher in examples 1-3 than in comparative example 1. In the aspect of sound absorption coefficient, examples 1 to 3 are all significantly higher than that of comparative example 1, and similarly, it can be seen from comparison between examples 1 to 3 and comparative example 1 that the thermal conductivity of butyl rubber is improved to different extents by adding different mass parts of graphene nano materials, and it can be seen from the result of temperature increase monitored by the fiber grating temperature sensor when the dynamic load is circulated for 300 times, after the graphene nano materials are added, the temperature at the center of the structural member is not significantly increased under the condition of increasing the loss factor of the material, and the special effect of the graphene paraffin oil is reflected.
In the aspect of temperature monitoring at the center of the cylindrical butyl rubber structural part, the temperature rise result monitored by the scheme of the invention is compared with the finite element simulation result, the relative error between the temperature rise result and the finite element simulation result is controlled within 10 percent, and the accuracy of the scheme of the invention can be proved.
It should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and the present invention is not limited thereto, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or equivalents thereof. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (9)
1. A preparation method of a graphene-butyl rubber nanocomposite structural member with a built-in fiber grating temperature sensor is characterized by comprising the following steps:
1) arranging fiber gratings on a forming die with a groove for a fiber lead wire reserved in advance, and leading the fiber lead wire out of the groove of the die lead wire;
2) filling the butyl rubber nano composite material rubber compound containing graphene into a mould, and completely coating the fiber grating temperature sensor;
3) carrying out high-temperature vulcanization molding on the mold;
the grating area of the fiber grating is packaged by a stainless steel capillary tube with a copper-plated surface;
in the vulcanization process, the rubber and the copper plating layer on the surface of the stainless steel capillary tube form a strong chemical bond;
the graphene-containing butyl rubber nanocomposite material is prepared from the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 3-8 parts of zinc oxide, 1-3 parts of stearic acid, 10-30 parts of carbon black, 20-40 parts of alumina hollow microspheres, 5-15 parts of graphene paraffin oil, 1-4 parts of an anti-aging agent, 1-3 parts of a promoter and 1-3 parts of sulfur;
wherein the graphene paraffin oil is a mixture of graphene and paraffin oil;
the graphene is multilayer flaky graphene, the diameter of the graphene is 2-20 micrometers, and the number of layers is 2-50;
the viscosity range of the paraffin oil is 5000-7000 cps;
the diameter of the alumina hollow microsphere is 0.4-1.5 microns, and the bulk density is 0.5-1.0 g/cm3。
2. The method of claim 1, wherein the graphene-containing butyl rubber nanocomposite is composed of the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 3-5 parts of zinc oxide, 1-2 parts of stearic acid, 10-20 parts of carbon black, 20-30 parts of alumina hollow microspheres, 5-10 parts of graphene paraffin oil, 1-2.5 parts of an anti-aging agent, 1-2 parts of an accelerator and 1-2 parts of sulfur.
3. The method of claim 1, wherein the graphene-containing butyl rubber nanocomposite is composed of the following raw materials in parts by weight: 100 parts of butyl rubber raw rubber, 5-8 parts of zinc oxide, 2-3 parts of stearic acid, 20-30 parts of carbon black, 30-40 parts of alumina hollow microspheres, 10-15 parts of graphene paraffin oil, 2.5-4 parts of an anti-aging agent, 2-3 parts of a promoter and 2-3 parts of sulfur.
4. The method of claim 1, wherein the graphene-containing butyl rubber nanocomposite is prepared by:
1) mixing graphene and paraffin oil, and stirring at a high speed at a certain temperature of 30-70 ℃ to obtain graphene paraffin oil, wherein the rotating speed of the high-speed stirring is 200-1200 rpm;
2) banburying: sequentially adding butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, alumina hollow microspheres, graphene paraffin oil and an anti-aging agent into an internal mixer, and discharging after internal mixing for a certain time to obtain an internal mixing blend; the certain time is 5-40 min;
3) adding a vulcanizing agent: adding the banburying blend into an open mill, adding an accelerant and sulfur, and mixing for a certain time to obtain a butyl rubber nano composite material containing graphene; the certain time is 10-20 min.
5. The process of claim 4, wherein the raw butyl rubber has an unsaturation level of not less than 1.75 mol%.
6. The method of claim 4, wherein said carbon black is a thermally cracked carbon black.
7. The method of claim 4, wherein the promoter is one or a combination of the following: tetramethylthiuram disulfide, dibenzothiazyl disulfide.
8. The graphene-butyl rubber nanocomposite structure with built-in fiber grating prepared by the method of any one of claims 1 to 7.
9. A dynamic temperature rise monitoring system for a vibration damping structure, comprising: a light source, a vibration device, the graphene-butyl rubber nanocomposite structural component with the built-in fiber grating of claim 8, a fiber lead and a fiber coupler, a fiber grating demodulator, a computer processor; the graphene-butyl rubber nanocomposite structural component with the built-in fiber grating is arranged on a vibration device and connected with a fiber coupler through a fiber lead, the fiber coupler is further connected with a light source and a fiber grating demodulator respectively, and the fiber grating demodulator is connected with a computer processor.
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