CN108467550A - A kind of butyl rubber nanocomposites and its dynamic heat build up detection method of graphene-containing - Google Patents
A kind of butyl rubber nanocomposites and its dynamic heat build up detection method of graphene-containing Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C08L23/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C08L23/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefins
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Abstract
The present invention provides a kind of butyl rubber nanocomposites and its dynamic heat build up detection method of graphene-containing.The butyl rubber nanocomposites of graphene-containing of the present invention greatly improve the damping capacity of butyl rubber, hence it is evident that improve the sound insulation property and heat-conductive characteristic of butyl rubber, with the incomparable advantage of conventional filler.The present invention proposes the butyl rubber dynamic heat build up detection method of graphene-containing simultaneously, by the fiber-optic grating sensor being implanted into inside butyl structures part, can with real time on-line monitoring rubber structure part during dynamic usage inside temperature change.Compared to the surface temperature detection method of current rubber structure part, the scheme tool of the real time on-line monitoring rubber structure part internal temperature has made marked progress.Material preparation of the present invention and temperature checking method are simple and reliable, applied widely, highly practical, have preferable economic benefit and social benefit.
Description
Technical field
The invention belongs to technical field of rubber material, be related to a kind of graphene-containing butyl rubber nanocomposites and its
Dynamic heat build up detection method.
Background technology
Worldwide problem of the vibration and noise as the present age, is prevalent in the every field of production and life.Many
In the measure of vibration and noise reducing, by the way that damping element and sound-absorbing material has been added in the machinery for being also easy to produce vibration, noise
As the most effective scheme of vibration and noise reducing.
Meet above-mentioned requirements and the high molecular material of excellent combination property is widely applied currently, many.These are high
Molecular material has viscoelastic and internal damping characteristics, this, which is conducive to will to damp and absorb sound, mechanism while being introduced into these materials, bright
It is aobvious to improve its vibration damping and sound absorbing performance.Butyl rubber (Isobutylene Isoprene Rubber, IIR) be by isobutene and
Isoprene carries out a kind of high score of function admirable of cationic polymerization generation under Friedel-Craft catalyst actions
Sub- material.The special molecular structure of butyl rubber so that friction and viscous loss are larger in it, so being vibration and noise reducing application neck
The preferred material in domain.
Graphene is a kind of carbon atom with sp2The monoatomic layer of hydridization arrangement is in the sheet two of the cellular arrangement of hexagonal annular
Crystal is tieed up, planar whether there is or not the multiple periodic structures of freight weight limit for graphene, there was only nanoscale perpendicular to the direction of plane, reason
There was only 0.335nm by thickness, is the Nano filling with macro-scale.The modulus of graphene may be up to 1TPa, and intensity reaches
130GPa, specific surface area is up to 2630m2.g-1, aspect ratio be more than 1000, be provided simultaneously with superelevation thermal conductivity (3000~
5000W.m-1.K-1) and electric conductivity (200000cm2.V-1.s-1).This imply that graphene to high molecular material in efficient enhancing and
There are prodigious potential advantages in terms of functionalization.It can be provided well for rubber mass using the excellent physical mechanical property of graphene
Sound absorption, damping and heat conductivility.
The dominant mechanism of vibration and noise reducing be utilize viscous interior friction of the high molecular material under dynamic load, will vibration and
Acoustic energy is converted into the energy dissipation of other forms, is generally converted to thermal energy, eventually leads to the Wen Sheng of damping structure part.So in conjunction with
The advantage of butyl rubber and graphene nano material respectively prepares a kind of butyl rubber nanocomposites of graphene-containing, can
To significantly improve the viscoelastic internal damping and heat conductivility of butyl rubber.
In view of the viscous-elastic behaviour of rubber material itself, even if improving rubber material by adding graphene nano material
Heat conductivility, it is also difficult to avoid the heat of rubber structure part and serious temperature under dynamic load from rising phenomenon, this can be seriously affected
The performance of rubber damping structural member.It is therefore necessary to the heat shape of real time on-line monitoring rubber structure part in use
State, and then evaluate its Long-Term Properties.Currently, being to use to monitoring in real time more commonly used for rubber structure part heat state
The scheme of infrared thermal imagery can only be confined to structural member surface temperature when carrying out structural member temperature monitoring using the program, and to it
The monitoring of internal temperature is then helpless.But for the bigger structural member of size, internal temperature can be significantly hotter than table
Face temperature, so it is difficult to deducing the heat state inside rubber structure part by measurement structure part surface temperature.
In order to monitor heat and the warm liter situation inside rubbery sample, existing program is by being beaten on rubbery sample at present
Hole extend into needle-shaped temperature transducer inside rubbery sample and measures.104569041 A of Chinese patent CN disclose one
Kind compression heat generation detector, i.e., be improved existing Goodrich rubber compression heat generation testing machine, avoid existing testing machine
The drawbacks of sample core central temperature cannot real-time and accurately be measured.But it is inevitable in the measurement scheme of the compression test
Ground also needs to carry out tap operation to rubber structure part, destroys the structural intergrity of original rubber structure part, this will certainly lead
Cause the change of rubber structure part stress-strain state in loading procedure.Also, by the way of being punched on rubber structure part
When carrying out the measurement of Wen Sheng, a hole is often opened on rubber structure part, can only inside measurement structure part a point temperature, cannot
The temperature variations at the multiple positions in monitoring of structures part inside simultaneously.
Invention content
In order to overcome above-mentioned deficiency, a kind of graphene dispersion of present invention offer is preferable, simple for process and stability is good, easy
In the butyl rubber nanocomposites for the graphene-containing for realizing engineering；And for current rubber structure part in dynamic load
The shortcoming that lower internal temperature rise measures, while proposing the dynamic heat build up monitoring of the butyl rubber nanocomposites of graphene-containing
Method, by the fiber-optical grating temperature sensor being implanted into inside butyl structures part, before ensureing structural member integrality
Put, in real time monitor rubber structure part during dynamic usage inside temperature change.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of preparation side of the graphene of built-in fiber bragg grating temperature sensor-butyl rubber nanocomposites structural member
Method, including：
1) in advance there are arranging fiber grating on the molding die for the groove of fiber-optic wire, and by fiber-optic wire from
It is drawn in die wire groove；
2) the butyl rubber nanocomposites rubber compound of graphene-containing is filled into mold, and by optical fiber grating temperature
Sensor coats completely；
3) mold is subjected to high temperature vulcanized molding；
The grating region of the fiber grating is packaged with stainless steel capillary；
The butyl rubber nanocomposites of the graphene-containing are composed of the following raw materials in parts by weight：Butyl rubber raw rubber
100 parts, 3~8 parts of zinc oxide, 1~3 part of stearic acid, 10~30 parts of carbon black, 20~40 parts of hollow aluminum oxide microspheres, graphene stone
5~15 parts of wax oil, 1~4 part of anti-aging agent, 1~3 part of accelerating agent, 1~3 part of sulphur；
Wherein, graphene paraffin oil is the mixture of graphene and paraffin oil,
The anti-aging agent includes：2,2,4 trimethyl 1,2 dihydroquinoline polymer (anti-aging agent RD) and N- (1,3- diformazans
Base) butyl-N'- diphenyl-para-phenylene diamines (antioxidant D MPPD).
Existing rubber material is since tensile property is preferable, general seldom implantation fiber-optic grating sensor, in order to avoid in rubber
Sensor degradation or measurement result is made relatively large deviation occur in drawing process.In order to overcome the above problem, the application is using stainless
Steel wool tubule is packaged grating region, meanwhile, effectively increase butyl rubber using graphene doping and the adjustment of composition of raw materials
Glue mechanics and damping capacity, the fiber-optic grating sensor that ensure that implantation and basis material have good compatibility, experiment knot
Fruit shows：The accurate survey of structural member internal temperature rise under dynamic load may be implemented in the structural member prepared using the present processes
Amount.
Preferably, it is composed of the following raw materials in parts by weight：100 parts of butyl rubber raw rubber, 3~5 parts of zinc oxide, stearic acid 1
~2 parts, 10~20 parts of carbon black, 20~30 parts of hollow aluminum oxide microspheres, 5~10 parts of graphene paraffin oil, 1~2.5 part of anti-aging agent,
1~2 part of accelerating agent, 1~2 part of sulphur.
Preferably, it is composed of the following raw materials in parts by weight：100 parts of butyl rubber raw rubber, 5~8 parts of zinc oxide, stearic acid 2
~3 parts, 20~30 parts of carbon black, 30~40 parts of hollow aluminum oxide microspheres, 10~15 parts of graphene paraffin oil, anti-aging agent 2.5~4
Part, 2~3 parts of accelerating agent, 2~3 parts of sulphur.
It is different from general graphene modified butyl rubber, using the butyl rubber of graphene-containing prepared by the raw material of the application
The advantage of glue nanocomposite also resides in：In sulfidation, the copper coating shape of rubber matrix and Stainless Steel Capillary pipe surface
At strong chemical bond, ensure that there is enough boundary strengths between the two.
Preferably, the graphene is multilayer chip graphene, and 2~20 microns of diameter, the number of plies is 2~50 layers；
Preferably, the paraffin oil, viscosity ranging from 5000~7000cps；
Preferably, a diameter of 0.4~1.5 micron of the hollow aluminum oxide microspheres, bulk density are 0.5~1.0g/
cm3。
The present invention also provides the preparation methods of the butyl rubber nanocomposites of above-mentioned graphene-containing, including：
1) graphene is mixed, at a certain temperature high-speed stirred with paraffin oil, obtains graphene paraffin oil；
2) mixing：By butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, hollow aluminum oxide microspheres, graphene paraffin oil
It is sequentially added in mixer with anti-aging agent, mixing discharges after a certain period of time, obtains mixing blend；
3) add vulcanizing agent：Mixing blend is added in open mill, accelerating agent, sulphur is added, is kneaded after a certain period of time, obtains
To the butyl rubber nanocomposites of graphene-containing.
Wherein, it is preferred that the degree of unsaturation of the butyl rubber raw rubber is not less than 1.75mol%；
Preferably, the carbon black is thermal cracking carbon black；
Preferably, the accelerating agent is the combination of one or both of following substances：Tetramethylthiuram disulfide, two sulphur
Change bisbenzothiazole.
The present invention also provides the butyl rubber nanocomposites of graphene-containing prepared by any above-mentioned method.
The present invention also provides graphene-butyl rubber nanometer of the built-in fiber bragg grating of any above-mentioned method preparation is multiple
Condensation material structural member.
The present invention also provides a kind of vibration-proof structure part dynamic temperature to rise monitoring system, including：It is light source, vibrating device, above-mentioned
Built-in fiber bragg grating graphene-butyl rubber nanocomposites structural member, fiber-optic wire and fiber coupler, optical fiber light
Grid (FBG) demodulator, computer processor；Wherein, the graphene of above-mentioned built-in fiber bragg grating-butyl rubber nanocomposites knot
Component setting is connected with fiber coupler on vibrating device, and by fiber-optic wire, the fiber coupler also respectively with light
Source is connected with fiber Bragg grating (FBG) demodulator, and the fiber Bragg grating (FBG) demodulator is connect with computer processor.
Beneficial effects of the present invention
(1) butyl rubber nanocomposites of graphene-containing of the present invention have been obviously improved the mechanics of butyl rubber
And damping capacity particularly due to the design feature of graphene itself, greatly improves sound absorption and the sound insulation property of butyl rubber
Can, with the incomparable advantage of conventional filler.
(2) it is excellent that graphene nano material is utilized in the butyl rubber nanocomposites of graphene-containing of the present invention
Heat conductivility, so that the heat conductivility of the butyl rubber nanocomposites structural member of preparation is dramatically increased, bearing dynamic carry
When lotus, the Wen Sheng of vibration-proof structure part is obviously reduced, and is conducive to the durability for improving vibration isolation rubber structural member.
(3) temperature of graphene of the present invention-butyl rubber vibration-proof structure part rises monitoring method in guarantee rubber structure
On the basis of part integrality, the thermal history inside rubber can be accurately measured, whether further can determine whether rubber structure part
It destroys, achievees the purpose that structural member usage situation health monitoring.This is existing at present or widely applied monitoring scheme institute
Incomparable, heretofore described method advantage protrudes, and tool has made marked progress.
(4) monitoring method for the material preparation method and dynamic Wen Sheng that the present invention uses, easy to operate, measuring stability
Good, convenient for engineering production, and adaptation is wide, has preferable economic benefit and social benefit.
Description of the drawings
The accompanying drawings which form a part of this application are used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its explanation do not constitute the improper restriction to the application for explaining the application.
Fig. 1 is graphene-butyl rubber nanocomposites of the present invention containing embedded optical fiber grating sensor
The diagrammatic cross-section of structural member.
Wherein, the stainless steel capillary of 101- copper coatings, 102- fiber-optical grating temperature sensors, 103- graphenes-fourth
Base rubber nano composite material structural member, 104- fiber grating leads.
Fig. 2 is that graphene-butyl rubber nanocomposites dynamic heat build up monitors schematic diagram.
Wherein, 201- light sources, 202- fiber couplers, 203- samples are fixed and loading device, 204- graphenes-butyl rubber
Glue nanocomposite structural member, 205- fiber-optical grating temperature sensors, 206- computer processors, 207- fiber grating demodulations
Instrument.
Fig. 3 is the finite element modelling result cloud atlas in rubber structure part temperature field under dynamic load.
Specific implementation mode
It is noted that following detailed description is all illustrative, it is intended to provide further instruction to the application.Unless another
It indicates, all technical and scientific terms used herein has usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific implementation mode, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or combination thereof.
With reference to specific embodiment, the present invention is described further.
The technical scheme is that：
The butyl rubber nanocomposites of graphene-containing are butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, oxidation
The mixture of aluminium tiny balloon, graphene paraffin oil, anti-aging agent, accelerating agent and sulphur, the mass fraction of each component in being formulated
Than for：100 parts of butyl rubber raw rubber, 3~8 parts of zinc oxide, 1~3 part of stearic acid, 10~30 parts of carbon black, hollow aluminum oxide microspheres
20~40 parts, 5~15 parts of graphene paraffin oil, 1~4 part of anti-aging agent, 1~3 part of accelerating agent, 1~3 part of sulphur.
The graphene paraffin oil is the homogeneous mixture of graphene and paraffin oil.
The anti-aging agent includes：2,2,4 trimethyl 1,2 dihydroquinoline polymer (anti-aging agent RD) and N- (1,3- bis-
Methyl) butyl-N'- diphenyl-para-phenylene diamines (antioxidant D MPPD).
The graphene is multilayer chip graphene, and 2~20 microns of diameter, the number of plies is 2~50 layers.
The paraffin oil, viscosity ranging from 5000~7000cps；If paraffin oil viscosity is excessive, graphene with
When paraffin oil starts mixing, it is difficult to stir evenly, graphene is reunited serious；If the viscosity very little of paraffin oil, in graphene
After being dispersed with stirring with paraffin oil, reassembled standing short period graphene；By repetition test, paraffin is chosen
Oily 5000~7000cps of viscosity is preferred.
Graphene paraffin oil prepare the step of be：According to quality parts ratio 20:100~50:100 by graphene and paraffin oil
It being sequentially placed into container, is then stirred using high speed rotation blender at a temperature of 30~70 DEG C, rotating speed is 200~1200rpm,
0.5~5h is stirred, 0.5h is stood without reassembling or deposited phenomenon, obtains uniformly mixed graphene paraffin oil.
The degree of unsaturation of the butyl rubber raw rubber is not less than 1.75mol%.
The carbon black is thermal cracking carbon black.
A diameter of 0.4~1.5 micron of the hollow aluminum oxide microspheres, bulk density are 0.5~1.0g/cm3。
The accelerating agent is the combination of one or both of following substances：Tetramethylthiuram disulfide (accelerating agent
TMTD), dibenzothiazyl disulfide (altax).
The dynamic heat build up of graphene-butyl rubber nanocomposites vibration-proof structure part monitors system, is in butyl rubber
Before structural member sulfidization molding, it is implanted into fiber-optic grating sensor inside structural member, after molding, forms optical fiber built-in grating temperature
The butyl structures part of sensor.
It is as follows that the specific preparation of graphene-butyl rubber nanocomposites structural member and temperature rise monitoring step：
(1) preparation of fiber-optical grating temperature sensor：According to the demand that rubber structure part internal temperature is tested, every continuous
Optical fiber on be distributed several grating regions, and all grating regions are packaged using very thin copper facing stainless steel capillary；
Pigtail splice is attached on every optical fiber, in order to be connected with fiber Bragg grating (FBG) demodulator；
The distance between grating region quantity and adjacent gratings for being distributed on every optical fiber are needed according to the test of Wen Sheng
It asks and is configured, the size range of each grating region is 5~8mm；
The Stainless Steel Capillary pipe surface is coated with ormolu, improving rubber and Stainless Steel Capillary in forming process
Boundary strength between pipe；0.5~1mm of outer diameter, the 0.2~0.4mm of wall thickness of stainless steel capillary；
(2) dispensing：The various raw materials for preparing graphene-butyl rubber composite material are weighed by formula；
(3) mixing：By butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, hollow aluminum oxide microspheres, graphene paraffin oil
It being sequentially added in mixer in 30min with anti-aging agent, control melting temperature is 70~100 DEG C, is discharged after 5~40min of mixing,
Obtain mixing blend；
(4) add vulcanizing agent：Mixing blend is added in open mill, accelerating agent, sulphur is added, control roller temperature is 40~50
DEG C, it is kneaded 10~20min；
(5) arrangement of fiber grating：According to specific thermometric demand, in advance there are the groove for fiber-optic wire at
Fiber grating is arranged on pattern tool, and fiber-optic wire is drawn from die wire groove；
(6) mold filling and cladding：The rubber compound of graphene-butyl rubber well prepared in advance is filled into mold, and will
Fiber-optical grating temperature sensor coats completely；
(7) sulfidization molding：Sulfurizing mould is placed on vulcanizer and carries out high temperature vulcanized molding, in initial vulcanization step, mold
Rubber be in viscous state, and by the stainless steel capillary tight of inner sleeve fiber grating, in sulfidation, rubber matrix
Strong chemical bond is formed with the copper coating of Stainless Steel Capillary pipe surface, ensures boundary strength between the two；
(8) vibration-proof structure part dynamic temperature rises monitoring：By the butyl rubber vibration-proof structure after molding with temperature sensor
Part is installed, and fiber-optic wire is connected with equipment such as fiber coupler, fiber Bragg grating (FBG) demodulator, computer processors, wherein light
Source can send out optical signal, and optical signal can be transferred to fiber-optic grating sensor and pass through between light and grating the back reflection that interacts,
It is transferred to fiber Bragg grating (FBG) demodulator again, the variation of center wavelength of light is demodulated by fiber Bragg grating (FBG) demodulator；When vibration-proof structure part is held
When by dynamic load, structural member internal temperature is constantly increased with the increase of cyclic loading number, and fiber Bragg grating (FBG) demodulator receives
Reflected light signal and the variation for identifying center wavelength of light, and convert to obtain accurate temperature change by computer processor, i.e.,
Obtain the temperature variations of butyl structures part inside point monitored.
The present invention materialogy principle be：Graphene has excellent mechanical property, high specific surface area, in nanometer ruler
The topological structure for having fold on very little makes it have the contact area of bigger and stronger binding force with rubber, to effectively improve rubber
Glue intensity and the high-flexibility for maintaining rubber itself；Graphene sheet layer forms " micro-nano constraint in butyl rubber matrix
Layer ", rubber material occur vibration deformation when, rubber molecule bear it is shear-deformable, to generate larger fissipation factor and compared with
Wide damping function temperature range；Importantly, graphene all has significantly the viscoelastic internal damping and heat conductivility of butyl rubber
Humidification, be conducive to vibration and acoustic energy and be converted into form of thermal energy dissipation when being transmitted in rubber matrix so that graphene-containing
Butyl rubber nanocomposites have preferable vibration damping and sound absorbing performance, and with compared to General Purpose Rubber material it is better
Thermal conductivity.
The temperature-measurement principle of interplantation fiber-optical grating temperature sensor is：When the temperature change of fiber grating local environment, bullet
The effects that luminous effect, thermo-optic effect, thermal expansion, causes the center wavelength variation of optical grating reflection light；The offset of center wavelength of light with
Temperature variation has correspondence；All grating regions are encapsulated by copper-plated stainless steel capillary in fiber-optic grating sensor,
It is then embedded in inside vibration isolation rubber structural member, causes grating region to thermally expand because of rubber structure part internal temperature rise, passed by light source
It interacting between defeated next optical signal and fiber grating, reflected light enters fiber Bragg grating (FBG) demodulator by fiber coupler, by
It demodulates the variation of center wavelength of light, and fiber Bragg grating (FBG) demodulator connects computer processor, obtains accurate temperature digital signal
And export display.
Examples 1 to 3 and comparative example 1：
Table 1 is the quality parts ratio of the rubber compounding of the embodiment of the present invention 1~3 and comparative example 1, butyl rubber raw rubber used
Degree of unsaturation be 1.75mol%；A diameter of 5 microns of graphene in graphene paraffin oil used, the number of plies are 5 layers, paraffin oil
Viscosity be 5000cps；In the preparation process of graphene paraffin oil, the quality parts ratio of graphene and paraffin oil is 20:
100, at a temperature of 50 DEG C, the rotating speed of high speed rotation blender is 800rpm, mixing time 0.5h.
The specific preparation of graphene-butyl rubber nanocomposites structural member described in Examples 1 to 3 and comparative example 1
And temperature liter monitoring step is as follows：
(1) preparation of fiber-optical grating temperature sensor：As desired, 103 inside center of test cylindrical rubber structural member
The temperature change state of point carves a grating region 102 in advance on a continuous optical fiber 104, and not using very thin copper facing
Rust steel wool tubule 101 is packaged grid region, Stainless Steel Capillary pipe outside diameter 0.7mm, wall thickness 0.2mm.
(2) dispensing：The various raw materials for preparing graphene-butyl rubber composite material are weighed by formula in table 1.
(3) mixing：By butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, hollow aluminum oxide microspheres, graphene paraffin oil
It being sequentially added in mixer in 30min with anti-aging agent, control smelting temperature is 70~100 DEG C, is discharged after 5~40min of mixing,
Obtain mixing blend.
(4) add vulcanizing agent：Mixing blend is added in open mill, accelerating agent, sulphur is added, control roller temperature is 40~50
DEG C, it is kneaded 10~20min.
(5) arrangement of fiber grating：Thermometric requirement according to step (1), in advance, there are for fiber-optic wire
Groove molding die on arrange fiber grating, and fiber-optic wire interface is drawn from die wire groove.
(6) mold filling and cladding：The rubber compound of graphene-butyl rubber well prepared in advance is filled into mold, and will
Fiber-optical grating temperature sensor coats completely.
(7) sulfidization molding：Sulfurizing mould is placed on vulcanizer and is vulcanized, 140 DEG C, time 30min of curing temperature, such as
This can obtain butyl rubber sample；And the rubber in initial vulcanization step, mold is in viscous state, not by inner sleeve fiber grating
Become rusty steel wool tubule tight, and in sulfidation, the copper coating on rubber matrix and 101 surface of stainless steel capillary, which is formed, to be strengthened
Key is learned, ensures boundary strength between the two.
(8) vibration-proof structure part dynamic temperature rises monitoring：Cylindrical butyl rubber after molding with temperature sensor is subtracted
The structural member 204 that shakes is mounted on vibrating device 203, and by fiber grating lead 104 and light source 201, fiber Bragg grating (FBG) demodulator
207, the equipment such as fiber coupler 202, computer processor 206 connect, wherein light source 201 can send out optical signal, optical signal meeting
It is transferred to fiber-optic grating sensor 205 and passes through between light and grating the back reflection that interacts, then be transferred to fiber grating demodulation
Instrument 207 demodulates the variation of center wavelength of light by it；When vibration, cylindrical vibration-proof structure part 204 is (i.e.：Graphene-butyl
Rubber nano composite material structural member) dynamic load is born, structural member internal temperature constantly rises with the increase of cyclic loading number
Height, fiber Bragg grating (FBG) demodulator receive continually changing reflected light signal and demodulate the variation of center wavelength of light, and by calculating
The processing of machine processor 206 obtains accurate temperature change and rises situation to get the temperature to butyl structures part inside center point.
The butyl rubber sample of preparation is tested for the property, test result is shown in Table 1.
The composition quality parts ratio and its performance test results of 1 Examples 1 to 3 of table and comparative example 1
As it can be seen that in terms of the fissipation factor for characterizing material damping damping property, Examples 1 to 3 is all higher than comparison
Example 1.In terms of acoustic absorptivity, Examples 1 to 3 is all apparently higher than comparative example 1, equally, comparing embodiment 1~3 and right
Ratio 1 it is found that addition different quality number graphene nano material the thermal coefficient of butyl rubber is had it is different degrees of
Promoted, and from dynamic load cycle 300 times when the raised result of fiber-optical grating temperature sensor monitoring temperature can be seen that and add
After adding graphene nano material, in the case where increasing material loss factor, the temperature at structural member center does not dramatically increase,
Reflect the special result of graphene paraffin oil.
In terms of the temperature monitoring at cylindrical butyl structures part center, the Wen Sheng that is monitored by scheme of the present invention
As a result with finite element modelling Comparative result it is found that relative error control between the two can prove the present invention within 10%
The accuracy of the scheme.
Finally it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not limited to this hair
It is bright, although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still
It can modify to the technical solution recorded in previous embodiment, or equivalent replacement is carried out to which part.It is all in this hair
Within bright spirit and principle, any modification, equivalent replacement, improvement and so on should be included in protection scope of the present invention
Within.Above-mentioned, although the foregoing specific embodiments of the present invention is described with reference to the accompanying drawings, not to the scope of the present invention
Limitation, those skilled in the art should understand that, based on the technical solutions of the present invention, those skilled in the art are not required to
Make the creative labor the various modifications or changes that can be made still within protection scope of the present invention.
Claims (10)
1. a kind of preparation side of the graphene of built-in fiber bragg grating temperature sensor-butyl rubber nanocomposites structural member
Method, which is characterized in that including：
1) in advance there are arranging fiber grating on the molding die for the groove of fiber-optic wire, and by fiber-optic wire from mold
It is drawn in lead groove；
2) the butyl rubber nanocomposites rubber compound of graphene-containing is filled into mold, and by fiber grating temperature sensor
Device coats completely；
3) mold is subjected to high temperature vulcanized molding；
The grating region of the fiber grating is packaged with stainless steel capillary；
The butyl rubber nanocomposites of the graphene-containing are composed of the following raw materials in parts by weight：Butyl rubber raw rubber 100
Part, 3~8 parts of zinc oxide, 1~3 part of stearic acid, 10~30 parts of carbon black, 20~40 parts of hollow aluminum oxide microspheres, graphene paraffin oil
5~15 parts, 1~4 part of anti-aging agent, 1~3 part of accelerating agent, 1~3 part of sulphur；
Wherein, graphene paraffin oil is the mixture of graphene and paraffin oil.
2. the method as described in claim 1, which is characterized in that the butyl rubber nanocomposites of the graphene-containing are by such as
The raw material of lower parts by weight forms：100 parts of butyl rubber raw rubber, 3~5 parts of zinc oxide, 1~2 part of stearic acid, 10~20 parts of carbon black,
20~30 parts of hollow aluminum oxide microspheres, 5~10 parts of graphene paraffin oil, 1~2.5 part of anti-aging agent, 1~2 part of accelerating agent, sulphur 1
~2 parts.
3. the method as described in claim 1, which is characterized in that the butyl rubber nanocomposites of the graphene-containing are by such as
The raw material of lower parts by weight forms：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 hollow aluminum oxide microspheres, 10~15 parts of graphene paraffin oil, 2.5~4 parts of anti-aging agent, 2~3 parts of accelerating agent, sulphur 2
~3 parts.
4. the method as described in claim 1, which is characterized in that the graphene is multilayer chip graphene, and diameter 2~20 is micro-
Rice, the number of plies are 2~50 layers；
Or the paraffin oil, viscosity ranging from 5000~7000cps；
Or a diameter of 0.4~1.5 micron of the hollow aluminum oxide microspheres, bulk density are 0.5~1.0g/cm3。
5. the method as described in claim 1, which is characterized in that the system of the butyl rubber nanocomposites of the graphene-containing
Preparation Method is as follows：
1) graphene is mixed, at a certain temperature high-speed stirred with paraffin oil, obtains graphene paraffin oil；
2) mixing：By butyl rubber raw rubber, zinc oxide, stearic acid, carbon black, hollow aluminum oxide microspheres, graphene paraffin oil and prevent
Old agent is sequentially added in mixer, and mixing discharges after a certain period of time, obtains mixing blend；
3) add vulcanizing agent：Mixing blend is added in open mill, accelerating agent, sulphur is added, is kneaded after a certain period of time, is contained
The butyl rubber nanocomposites of graphene.
6. method as claimed in claim 5, which is characterized in that the degree of unsaturation of the butyl rubber raw rubber is not less than
1.75mol%.
7. method as claimed in claim 5, which is characterized in that the carbon black is thermal cracking carbon black.
8. method as claimed in claim 5, which is characterized in that the accelerating agent is the group of one or both of following substances
It closes：Tetramethylthiuram disulfide, dibenzothiazyl disulfide.
9. the nano combined material of graphene-butyl rubber of built-in fiber bragg grating prepared by any methods of claim 1-8
Expect structural member.
10. a kind of vibration-proof structure part dynamic temperature rises monitoring system, including：It is light source, vibrating device, built-in described in claim 9
The graphene of fiber grating-butyl rubber nanocomposites structural member, fiber-optic wire and fiber coupler, fiber grating demodulation
Instrument, computer processor；Wherein, the graphene of the built-in fiber bragg grating-butyl rubber nanocomposites structural member is set
Set on vibrating device, and be connected with fiber coupler by fiber-optic wire, the fiber coupler also respectively with light source and light
Fine grating demodulation instrument connection, the fiber Bragg grating (FBG) demodulator are connect with computer processor.
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