CN107894407A - A kind of modified pitch SBS volume method for rapidly testing - Google Patents
A kind of modified pitch SBS volume method for rapidly testing Download PDFInfo
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- CN107894407A CN107894407A CN201711474731.XA CN201711474731A CN107894407A CN 107894407 A CN107894407 A CN 107894407A CN 201711474731 A CN201711474731 A CN 201711474731A CN 107894407 A CN107894407 A CN 107894407A
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- 238000000034 method Methods 0.000 title claims abstract description 60
- 238000012360 testing method Methods 0.000 title claims abstract description 46
- 238000002329 infrared spectrum Methods 0.000 claims abstract description 24
- 239000003607 modifier Substances 0.000 claims abstract description 20
- 239000011159 matrix material Substances 0.000 claims description 14
- 230000008569 process Effects 0.000 claims description 12
- 241001269238 Data Species 0.000 claims description 9
- 238000004458 analytical method Methods 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000012706 support-vector machine Methods 0.000 claims description 4
- 238000002790 cross-validation Methods 0.000 claims description 3
- 238000009499 grossing Methods 0.000 claims description 3
- 238000004321 preservation Methods 0.000 claims description 3
- 230000009467 reduction Effects 0.000 claims description 3
- 238000004611 spectroscopical analysis Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000000611 regression analysis Methods 0.000 claims 1
- 239000010426 asphalt Substances 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 5
- 238000000701 chemical imaging Methods 0.000 abstract description 2
- 238000010801 machine learning Methods 0.000 abstract description 2
- 239000011295 pitch Substances 0.000 description 63
- 238000005516 engineering process Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000001228 spectrum Methods 0.000 description 5
- 238000001514 detection method Methods 0.000 description 4
- 239000003381 stabilizer Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000010008 shearing Methods 0.000 description 3
- 238000003556 assay Methods 0.000 description 2
- 238000011088 calibration curve Methods 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000000799 fluorescence microscopy Methods 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 244000025254 Cannabis sativa Species 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
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- 239000002904 solvent Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012549 training Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
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Abstract
The invention discloses a kind of modified pitch SBS volume method for rapidly testing, preparation, ir data test, the pretreatment of infrared spectroscopic imaging, preferred, forecast model foundation, the application of forecast model for modeling wave band of SBS modified pitch samples.The modified pitch ir data obtained according to examination of infrared spectrum, forecast model is established with reference to machine learning algorithm, while the test of SBS volumes is rapidly completed, the accuracy of SBS asphalt modifiers volume prediction, the SBS volumes measure for the modified pitch that can be widely applied in all kinds of engineering projects can be ensured.
Description
Technical field
The present invention relates to SBS volume detection technique fields, the quick side of test of more particularly to a kind of modified pitch SBS volumes
Method.
Background technology
SBS modified pitch is using matrix pitch as raw material, adds a certain proportion of SBS modifier, good using SBS modifier
Good physical property does modification to pitch.SBS modified pitch is due to excellent high/low temperature pavement performance, in China's height
Using more and more common in grade pavement engineering.It is partially modified with the rise of the market competition and SBS modifier price of fierceness
Pitch supplier starts to use wrongful competitive method to obtain higher profit.In practical engineering application, either factory
The modified pitch of production or situ modified, the problem of " stealing " modifying agent using various methods, just progressively occur.Thus trigger
Performance of modified bitumen " discounting " phenomenon has been exposed through during a plurality of express highway pavement is constructed at home, and causes highway construction administration
The great attention of department.
At present, the technical specification in China defines the technical performance of finished product asphaltum.Research shows these technical performances
Also reduce and be deteriorated with SBS modifier volume really.But scientific and technological progress causes the loss of low-dosage SBS performance of modified bitumen to pass through
A certain amount of chemical " stabilizer " is filled to make up.Than being shown if any data, for 4.6% SBS modifier addition content, it is not added with
The softening point of modified pitch is 72 DEG C during chemical stabilizer, and during certain chemical stabilizer of admixture 0.2%, 0.4%, softening point is then
It is upgraded to 85 DEG C and 98 DEG C.Equally, low-temperature ductility also shows similar changing rule with part index numbers such as dynamic viscosities.It is true
On, a small amount of chemical stabilizer is filled in modified pitch, its initial purpose is the high temperature storage stability for solving modified pitch
Problem, that is, SBS is not isolated with matrix pitch when storing, but supplier was then carried out using its performance indications to modified pitch later
" name " is improved, and standard is not uniformly controlled for SBS volumes, and different SBS volumes can be to bituminous paving actual performance, especially
The improvement of durability produces different degrees of influence.Control in practical engineering application on modified pitch SBS contents is mainly led to
The supervision and management when strengthening modified pitch production are crossed, but effective analysis to modifier content at present and detection are not formed yet
Professional standard and specification.
In recent years, the SBS asphalt modifier volume determination techniques method that in the market occurs includes fractionation, differential thermal point
Analysis method, fluorescence microscopy.Wherein, more contact volatile harmful solvent, operation week can be utilized in fractionation experiment
Phase is grown, and detection SBS contents are higher to test operation level requirement, the precision for holding measure is difficult in practical engineering application, no
Beneficial to the large-scale promotion of engineer applied；Requirement of the differential thermal experiment equally to equipment is higher, test period length, and experimentation cost compared with
It is high；Fluorescence microscopy also has very high requirement to equipment, and the data processing in later stage is also required to take a long time.It is red
The conventional method of external spectrum technical testing SBS contents is first to carry out lot of experiments to establish standard curve, then passes through standard curve meter
The modifier content of unknown pitch is calculated, but due to the modified pitch matrix used in different engineering projects, asphalt type, SBS types
Vary, therefore, test every time will establish a standard curve in advance.So by summarizing modified pitch SBS containing measurement
Fixed various methods understand that various measuring technology precision, accuracy are uneven, and how repdocutbility and applicability need further
Research, also neither one normative reference is followed or judged as user and manager.
Therefore, how to provide a kind of applicability is extensively, using easily modified pitch SBS volumes method for rapidly testing sheet
Art personnel technical problem urgently to be resolved hurrily.
The content of the invention
Infrared spectrum technology measure SBS contents method the most frequently used at present is used to pass through SBS and drip for calibration curve method
Blue or green Correlative characteristic peaks establish a standard curve with the change of SBS volumes, recycle standard curve that unknown SBS pitches are calculated
Modifier content.The problem of calibration curve method is present is will be again through experiment drafting standard for different modified pitch
Curve, it is that Specification Curve of Increasing process Consideration is single to also have some drawbacks, related to SBS assays in material spectrum
Many important informations can all neglect.
In view of this, it is an object of the invention to provide a kind of modified pitch SBS volume method for rapidly testing, according to infrared
The SBS ir datas of spectrum test establish forecast model, while the test of SBS volumes is rapidly completed, can ensure SBS
The accuracy of asphalt modifier volume prediction, the SBS volumes for the SBS modified pitch that can be widely applied in all kinds of engineering projects are surveyed
It is fixed.Its concrete scheme is as follows to achieve the above object：
A kind of modified pitch SBS volume method for rapidly testing, comprises the following steps：
Step 1, prepare multigroup SBS modified pitch sample；
Step 2, examination of infrared spectrum is carried out respectively to multigroup SBS modified pitch sample, obtains SBS infrared spectrums
Data；
Step 3, the SBS ir datas are pre-processed；
Step 4, the relation of pretreated SBS infrared spectrums characteristic peak and SBS volumes is analyzed, and combine coefficient correlation
Method screening Modelling feature section；
Step 5, establish forecast model；
Step 6, the SBS volumes of unknown SBS modified pitch sample are predicted according to the forecast model.
Preferably, in the step 1：Several matrix pitch and SBS modifier are selected, is prepared using different SBS volumes
Multigroup SBS modified pitch sample.
Preferably, the step 2 specifically includes：
1) using the infrared spectrum of transmission beam method test modified pitch；
2) will the SBS modified pitch sample heating after uniformly be applied on KBr chip, smearing thickness be 0.4mm~
0.5mm, room temperature is cooled to, is tested using infrared spectrometer, export SBS infrared spectrograms, it is infrared that preservation obtains the SBS
Spectroscopic data.
Preferably, the temperature conditionss that the SBS modified pitch sample heats in constant temperature oven are 165 DEG C~175 DEG C.
Preferably, the working environment of the infrared spectrometer is：25 DEG C ± 5 DEG C of temperature, humidity are not more than 60%.
Preferably, in order to ensure test accuracy, scanning times are arranged to 32 times, and scanning resolution is arranged to 0.5cm-1。
Preferably, the method pre-processed to the SBS ir datas includes but is not limited to first derivative and Fu
In leaf roll product smoothing method.
Preferably, in the step 4, the selection for modeling wave band is chemically tied based on langbobier law with SBS characteristic peaks
The relation of structure angle comprehensive analysis infrared spectrum characteristic peak and SBS volumes, and screen to obtain Modelling feature with reference to correlation coefficient process
Section.
Preferably, the Modelling feature section is 680cm-1~1050cm-1。
Preferably, the step 5 specifically includes：
Recurrence, which is carried out, from SVMs establishes the forecast model；
Dimensionality reduction is carried out using PCA；
The accuracy of the forecast model is tested using five folding cross validations.
Preferably, the modified pitch SBS modifier developed according to a kind of modified pitch SBS volumes method for rapidly testing
Volume fast testing system.
A kind of modified pitch SBS volume method for rapidly testing disclosed by the invention, it is infrared according to the SBS of examination of infrared spectrum
Spectroscopic data establishes forecast model, can cover nearly all common modified pitch information, including bitumen base, modifying agent and
Volume ratio etc., applicability is more extensive, and application is more convenient, and user need to only import the ir data that test obtains, you can
It is rapidly completed the test of SBS volumes.The present invention using infra-red sepectrometry relative to existing detection method, no matter in applicability, accurate
Property, suffer from clear superiority in terms of economy, testing efficiency.The foundation of machine learning method is combined on this basis is based on infrared spectrum
The SBS content prediction models of data, can strengthen the applicability of model by the unified Modeling of a variety of SBS modified pitch, and machine
The effective information of ir data can be preferably collected in device learning algorithm modeling process by principal component analysis technology, is made
Theoretical more science, the predictive ability of model is more accurate.
The present invention effectively can be supervised effectively to SBS modified pitch market, prevent the improper of pitch supplier from trying to gain
Profit, make its market specifications, regularization, positive role is played to the social and economic benefits for creating good.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to embodiment or existing
There is the required accompanying drawing used in technology description to be briefly described, it should be apparent that, drawings in the following description are only this
The embodiment of invention, for those of ordinary skill in the art, on the premise of not paying creative work, can also basis
The accompanying drawing of offer obtains other accompanying drawings；
Fig. 1 is a kind of schematic flow sheet of modified pitch SBS volume method for rapidly testing disclosed by the invention；
Fig. 2 is the SBS infrared spectrograms that SBS contents disclosed in the embodiment of the present invention are 5%；
Fig. 3 is SBS infrared spectrograms after the disclosed pretreatment of the embodiment of the present invention；
Fig. 4 is the coefficient correlation curve map of infrared spectrum disclosed in the embodiment of the present invention and SBS volumes；
Fig. 5 is SVM prediction result schematic diagram disclosed in the embodiment of the present invention.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete
Site preparation describes, it is clear that described embodiment is only part of the embodiment of the present invention, rather than whole embodiments.It is based on
Embodiment in the present invention, those of ordinary skill in the art are obtained every other under the premise of creative work is not made
Embodiment, belong to the scope of protection of the invention.
Shown in Figure 1, the invention discloses a kind of modified pitch SBS volume method for rapidly testing, including SBS to be modified drip
The preparation of blue or green sample, ir data test, the pretreatment of infrared spectroscopic imaging, modeling wave band it is preferred, forecast model
Establish, the application of forecast model, specific implementation step is as follows：
S1：Prepare multigroup SBS modified pitch sample；
1) the 70# matrix pitches of six kinds of different oil sources of preparation, two kinds of SBS modifiers (star-like BM4302 and line style YH791),
It is respectively 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, 5.5%, 6% to select SBS volumes, prepares 6*2*9=108 groups
Sample, every group of sample carry out five groups of parallel tests, 540 groups of corresponding datas, i.e. SBS modified pitch infrared spectrum and SBS are obtained
The corresponding data of volume；
2) prepared by sample：SBS modified pitch is prepared in high-speed shearing machine laboratory, it is necessary to ensure that SBS modifier is sheared
It is can be uniformly distributed in after meeting certain requirements in matrix pitch, so as to develop into the SBS modified pitch for meeting actual requirement.Often
, it is necessary to which rotating speed and mixing time to high-speed shearing machine propose certain requirement in group sample preparation, first 2kg matrix should be dripped
Green grass or young crops proportionally puts into SBS modifier after stirring, and to make SBS be uniformly blended into matrix pitch, high-speed shearing machine turns to be set to
6000r/min, mixing time 1 hour, 170 DEG C of matrix pitch heating-up temperature, 175 DEG C of modified asphalt-stirring process.
S2：Examination of infrared spectrum is carried out to multigroup SBS modified pitch sample using transmission beam method respectively, it is red to obtain SBS
External spectrum data；
1) SBS modified pitch samples are heated to 165 DEG C~175 DEG C in constant temperature oven, SBS modified pitch sample is in equal
Uniform flow is dynamic, thick liquid nano；
2) using tablet press machine to be pressed into pure powder KBr, thickness is uniform, clear transparent crystal microchip is standby；
3) infrared spectrometer operation sequence starts, and setting operation condition is stand-by, working environment：25 DEG C ± 5 DEG C of temperature, it is wet
Degree is not more than 60%；
4) the SBS modified pitch sample is uniformly applied on the KBr chip, smearing thickness be 0.4mm~
0.5mm, room temperature is cooled to, be positioned in infrared spectrometer fixture, fixture is put into infrared spectrograph sample room, using transmission beam method
The infrared spectrum of modified pitch, output SBS infrared spectrograms to computer are tested, preservation obtains the SBS ir datas.
S3：SBS ir datas are pre-processed；The method of pretreatment includes but is not limited in first derivative and Fu
Leaf roll accumulates smoothing method.
S4：After based on Lambert-Beer laws and SBS the characteristic peaks chemically pretreatment of structural point comprehensive analysis
SBS infrared spectrums characteristic peak and SBS volumes relation, and combine correlation coefficient process and screen optimal Modelling feature section；
According to Lambert-Beer laws, under identical testing conditions, SBS characteristic absorptions peak area substantially with its content
It is directly proportional, the relevant information corresponding to SBS contents is necessarily included in modified pitch infrared spectrum.
Due to full section middle infrared spectrum (4000cm-1~400cm-1) in include more system noise, therefore utilize full spectrum
It is modeled effect and bad.Numerous characteristic peaks are included in SBS modified pitch infrared spectrums, also not all characteristic peak all and
SBS volumes are related, so best modeled wave band must be screened, in the present embodiment, it is contemplated that SBS characteristic peaks are 699cm-1、
910cm-1、966cm-1, it is as follows in conjunction with correlation coefficient process, its concrete methods of realizing：
SBS infrared signature peak is 699cm-1, 910cm-1, 966cm-1, with reference to correlation coefficient process, calculate infrared spectrum number
According to collection and the coefficient correlation of SBS volume data, 540 groups of samples are obtained after experiment altogether, if ir data integrates as matrix X, then
Have
In formula, line number m is test sample amount, is herein 540, and columns n is the collection capacity of ir data, itself and selection
Modeling section, infrared spectrum frequency acquisition is relevant.
SBS volumes column matrix is Y, is had
Any one row and Y coefficient correlation in matrix X are asked for, is had
The ir data collection of full section and the coefficient correlation of SBS content column matrix are obtained, it is real for the present invention referring to accompanying drawing 4
Apply the coefficient correlation curve map of infrared spectrum disclosed in example and SBS volumes.Can be according to coefficient correlation collection of illustrative plates, it is determined that final modeling
Section is 680cm-1~1050cm-1。
S5：Establish forecast model；Forecast model carries out recurrence foundation from SVMs (SVR), using principal component point
The method for analysing (PCA) carries out dimensionality reduction, and the kernel function of SVMs is Quadratic Kernel, is surveyed using five folding cross validations
The accuracy of trial and error procedure.
All 540 groups of test datas build the coefficient of determination R of forecast model2=0.991, root-mean-square error RMSE=0.11,
Because the present embodiment discloses the forecast model obtained using six kinds with the data set of label difference oil sources pitch, predicted value with
Fine difference between actual value comes from the difference of different oil sources, is such as individually modeled with a kind of data set of oil sources pitch, SBS mixes
Measure forecast model coefficient of determination R20.998 can be reached, have been provided with very high precision of prediction.
It is SVM prediction result schematic diagram, prediction result and reality disclosed in the embodiment of the present invention referring to accompanying drawing 5
SBS volumes match, and ensure that the degree of accuracy of SBS volumes prediction.
S6：The SBS volumes of unknown SBS modified pitch sample are predicted according to the forecast model.
The forecast model trained is exported into workspace, it is i.e. predictable unknown using the ir data newly inputted
The SBS volumes of SBS modified pitch samples.
To verify the accuracy of forecast model of the present invention, 10 groups of embodiments are disclosed directly below：
Two groups of SBS modified pitch samples are reconfigured in laboratory, modified drip is configured using the method test of the present invention
Blue or green modifier content, concrete outcome are shown in Table 1.
The laboratory SBS assay results of table 1
From result, within ± 0.1%, method of testing provides very high the test result error of two groups of samples
Measuring accuracy.
Forecast model according to training writes a set of modified pitch SBS modifier volume fast testing system, and user is only
The ir data that test obtains need to be imported, you can be rapidly completed the test of SBS volumes, this great market promotion prospect.
A kind of modified pitch SBS volume method for rapidly testing provided by the present invention is described in detail above, this
Apply specific case in text to be set forth the principle and embodiment of the present invention, the explanation of above example is only intended to
Help to understand method and its core concept of the invention；Meanwhile for those of ordinary skill in the art, the think of according to the present invention
Think, in specific embodiments and applications there will be changes, in summary, this specification content should not be construed as pair
The limitation of the present invention.
Herein, such as first and second or the like relational terms be used merely to by an entity or operation with it is another
One entity or operation make a distinction, and not necessarily require or imply between these entities or operation any this reality be present
Relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to the bag of nonexcludability
Contain, so that process, method, article or equipment including a series of elements not only include those key elements, but also including
The other element being not expressly set out, or also include for this process, method, article or the intrinsic key element of equipment.
In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that including the key element
Process, method, other identical element also be present in article or equipment.
Claims (8)
- A kind of 1. modified pitch SBS volume method for rapidly testing, it is characterised in that：Comprise the following steps：Step 1, prepare multigroup SBS modified pitch sample；Step 2, examination of infrared spectrum is carried out respectively to multigroup SBS modified pitch sample, obtains SBS ir datas；Step 3, the SBS ir datas are pre-processed；Step 4, the relation of pretreated SBS infrared spectrums characteristic peak and SBS volumes is analyzed, and combine correlation coefficient process and sieve Select Modelling feature section；Step 5, establish forecast model；Step 6, the SBS volumes of unknown SBS modified pitch sample are predicted according to the forecast model.
- A kind of 2. modified pitch SBS volume method for rapidly testing according to claim 1, it is characterised in that the step In one：The pitch and SBS modifier of several matrix are selected, multigroup SBS modified pitch sample is prepared using different SBS volumes This.
- A kind of 3. modified pitch SBS volume method for rapidly testing according to claim 1, it is characterised in that the step Two specifically include：1) using the infrared spectrum of transmission beam method test modified pitch；2) will the SBS modified pitch sample heating after uniformly be applied on KBr chip, smearing thickness be 0.4mm~ 0.5mm, room temperature is cooled to, is tested using infrared spectrometer, export SBS infrared spectrograms, it is infrared that preservation obtains the SBS Spectroscopic data.
- 4. a kind of modified pitch SBS volume method for rapidly testing according to claim 1, it is characterised in that to the SBS The method that ir data is pre-processed includes but is not limited to first derivative and Fourier's convolution smoothing method.
- A kind of 5. modified pitch SBS volume method for rapidly testing according to claim 1, it is characterised in that the step In four, the selection for modeling wave band is based on langbobier law and SBS characteristic peaks, chemically structural point comprehensive analysis infrared spectrum The relation of characteristic peak and SBS volumes, and screen to obtain Modelling feature section with reference to correlation coefficient process.
- A kind of 6. modified pitch SBS volume method for rapidly testing according to claim 5, it is characterised in that the modeling Characteristic interval is 680cm-1~1050cm-1。
- A kind of 7. modified pitch SBS volume method for rapidly testing according to claim 1, it is characterised in that the step Five specifically include：Regression analysis is carried out from algorithm of support vector machine, establishes the forecast model；Data Dimensionality Reduction is carried out using PCA；The accuracy of the forecast model is tested using five folding cross validations.
- 8. a kind of modified pitch SBS volume method for rapidly testing according to any one of claim 1-7, its feature exist In quickly being tested according to the modified pitch SBS modifier volume that a kind of modified pitch SBS volumes method for rapidly testing is developed System.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110186866A (en) * | 2019-06-05 | 2019-08-30 | 交通运输部公路科学研究所 | A kind of method of determining SBS modified pitch degradation amount |
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| CN101876634A (en) * | 2010-06-22 | 2010-11-03 | 长安大学 | Method for testing mixing amount of styrene-butadiene-styrene modified asphalt modifier |
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