CN108613945A - A method of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property - Google Patents
A method of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property Download PDFInfo
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- CN108613945A CN108613945A CN201810316462.2A CN201810316462A CN108613945A CN 108613945 A CN108613945 A CN 108613945A CN 201810316462 A CN201810316462 A CN 201810316462A CN 108613945 A CN108613945 A CN 108613945A
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- modified pitch
- soluble matter
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- tetrahydrofuran soluble
- tetrahydrofuran
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- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 title claims abstract description 146
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 230000003712 anti-aging effect Effects 0.000 title claims abstract description 41
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000002329 infrared spectrum Methods 0.000 title claims abstract description 25
- 230000032683 aging Effects 0.000 claims abstract description 83
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 claims abstract description 41
- 239000003245 coal Substances 0.000 claims abstract description 33
- 125000003375 sulfoxide group Chemical group 0.000 claims abstract description 33
- 238000012360 testing method Methods 0.000 claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 22
- 239000011159 matrix material Substances 0.000 claims abstract description 15
- 125000000524 functional group Chemical group 0.000 claims abstract description 11
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000012986 modification Methods 0.000 claims description 5
- 230000004048 modification Effects 0.000 claims description 5
- 239000002245 particle Substances 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 150000002240 furans Chemical class 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000002390 rotary evaporation Methods 0.000 claims description 2
- 238000003483 aging Methods 0.000 abstract description 45
- 239000010426 asphalt Substances 0.000 abstract description 42
- 238000000944 Soxhlet extraction Methods 0.000 abstract description 3
- 238000011156 evaluation Methods 0.000 abstract description 3
- 238000005265 energy consumption Methods 0.000 abstract description 2
- 101100227798 Arabidopsis thaliana THFS gene Proteins 0.000 abstract 7
- 239000011295 pitch Substances 0.000 description 124
- 230000001965 increasing effect Effects 0.000 description 21
- 230000035515 penetration Effects 0.000 description 10
- 230000033228 biological regulation Effects 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 8
- 239000010409 thin film Substances 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- 239000007788 liquid Substances 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- -1 Hydrogen furans Chemical class 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- 239000000654 additive Substances 0.000 description 4
- 230000000996 additive effect Effects 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 4
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000006227 byproduct Substances 0.000 description 3
- 238000010276 construction Methods 0.000 description 3
- 239000003431 cross linking reagent Substances 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 239000000284 extract Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- ZZIZZTHXZRDOFM-XFULWGLBSA-N tamsulosin hydrochloride Chemical compound [H+].[Cl-].CCOC1=CC=CC=C1OCCN[C@H](C)CC1=CC=C(OC)C(S(N)(=O)=O)=C1 ZZIZZTHXZRDOFM-XFULWGLBSA-N 0.000 description 3
- 230000003519 ventilatory effect Effects 0.000 description 3
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 2
- 230000003321 amplification Effects 0.000 description 2
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000002596 correlated effect Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000002708 enhancing effect Effects 0.000 description 2
- 150000002148 esters Chemical class 0.000 description 2
- 230000008676 import Effects 0.000 description 2
- 150000002576 ketones Chemical class 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 239000010117 shenhua Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 150000003462 sulfoxides Chemical class 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 125000003718 tetrahydrofuranyl group Chemical group 0.000 description 2
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 101100202447 Drosophila melanogaster sav gene Proteins 0.000 description 1
- 241000772415 Neovison vison Species 0.000 description 1
- 239000005864 Sulphur Substances 0.000 description 1
- 241000613130 Tima Species 0.000 description 1
- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000003679 aging effect Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 230000000191 radiation effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 229960002415 trichloroethylene Drugs 0.000 description 1
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Working-Up Tar And Pitch (AREA)
Abstract
The present invention relates to one kind being based on examination of infrared spectrum tetrahydrofuran soluble matter（Tetrahydrofuran soluble fraction, THFS）The method of modified pitch anti-aging property, includes the following steps：Test matrix pitch, coal directly-liquefied residue（Direct coal liquefaction residue, DCLR）Properties；1）Using Soxhlet extraction device using THF as extractant, DCLR is extracted；2）THFS to be obtained by extraction from DCLR prepares THFS modified pitch as modifying agent；3）Short ageing is simulated to THFS modified pitch；4）Using the functional group that infrared spectrometer test THFS modified pitch agings are forward and backward, the forward and backward carbonyl of ageing of asphalt and sulfoxide group peak area are calculated, its anti-aging property is analyzed using the forward and backward carbonyl of ageing of asphalt and sulfoxide group peak area ratio；5）Determine the optimum addition range of THFS.The evaluation method of the present invention is the anti-aging property of THFS modified pitch to be evaluated from microcosmic angle, and this method is simple, easy to operate, energy consumption is low.
Description
Technical field
The invention belongs to technical field of buildings, are related to a kind of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch
The method of anti-aging property.
Background technology
In recent years, China mostly takes place frequently haze, and burning coal is one of the main arch-criminal for generating haze, therefore
It realizes that Coal Clean efficiently utilizes, builds cleaning low-carbon, safe and efficient modern energy system is of great significance.Coal liquefaction skill
Art is one of the effective means realized Coal Clean and efficiently utilized, and solid coal is converted to liquid combustion by chemical reaction process
Material, industrial chemicals and product are a kind of advanced clean coal technology, including two kinds of techniques of direct liquefaction and indirect liquefaction.Coal is straight
It is inevitable in direct coal liquefaction process to connect liquefied residue (direct coal liquefaction residue, DCLR)
The Main By product for accounting for feed coal total amount 30% that ground generates is the substance of a kind of high ash, high-sulfur, high charcoal and golf calorific value,
Containing useful components such as a large amount of asphaltenes, mink cell focus, tetrahydrofuran soluble matter, petroleum asphalt modified dose can be developed into.
King stockaded village rosy clouds etc. have rated modifying functions of the DCLR to bi tumenf orr oad, it was found that DCLR modified pitch can meet
Needle penetration is the standard of No. 50 pitch, and with the increase of DCLR volumes, the softening point of modified pitch gradually rises, needle penetration and
Ductility is in the trend continuously decreased.
Season etc. is macro using SHRP PG, needle penetration staging hierarchy, the analysis DCLR such as infrared spectrometer and bitumen blend
Performance and microstructure are seen, it is found that DCLR has good improvement result to the high-temperature behavior of pitch, but contain a large amount of four in DCLR
Hydrogen furans insoluble matter causes the cryogenic property of pitch to decline.
It is old to wait quietly, using benzaldehyde as crosslinking agent, being modified asphalt using the tetrahydrofuran soluble matter of DCLR,
The influence of THFS, the volume of crosslinking agent and blending temperature to asphalt performance is investigated.Studies have shown that the volume as THFS is
4%, modified effect is best when blending temperature is 170 DEG C, and benzaldehyde can make asphalt modification effect more as crosslinking agent addition
It is good.
Researcher mostly changes pitch from macroscopic perspective to study and characterize DCLR (including the TFHS obtained after extraction)
Property effect, but DCLR modified pitch, the especially anti-aging property of THFS modified pitch are but seldom related to.And it is anti-for pitch
Ageing properties, researchers have been carried out a large amount of research.
It is sudden and violent that Yao etc. is based on infrared spectrum (Fourier transform infrared spectrometer, FTIR) test
The pitch functional group being exposed in air and oxygen finds six functional groups (carboxylic acid, aldehyde, amide, acid in pitch containing carbonyl
Acid anhydride, ester and ketone), carboxylic acid and ketone are the main aged components in pitch, and content is related with the degree of oxidation of pitch, in pitch
Ester and aldehyde keep limited amount.
Lin Lu etc. chooses four kinds of different matrix pitches, to infrared spectrum before and after each ageing of asphalt in 1800-600cm-1
The comparison of the peak area size of oxygen-containing functional group can show that the variation after variety classes ageing of asphalt differs, and sulphur contains in range
Sulfoxide group peak area increases obviously after measuring higher ageing of asphalt, and carbonyl peak area increases after the lower ageing of asphalt of sulfur content
Obviously.
Lamontagne etc. has studied the aging character of different pitches thermo-oxidative ageing molecular configurational by infrared spectrometer,
Pitch is thought when being contacted with air, and the active group in strand and segment will pass through in conjunction with the oxygen molecule in air
Chemical reaction generates the very big molecule containing carbonyl, and then leads to ageing of asphalt.
Zhao Yongli etc. utilizes 1460cm using the aging character with infrared spectrum analysis SBS modified pitch-1The methyl at place
Peak area ratio is calculated on the basis of bending vibration absorption peak, quantitative analysis is carried out to it, the results showed that with the progress of aging, pitch
It is aoxidized so showing the increase of aging forward and backward carbonyl peak area ratio and sulfoxide group peak area ratio.
Maria de F á tima A.de S.Araujo etc. are by using infrared spectrum analysis SBS modified pitch ultraviolet
Degradation under radiation effects, and calculate carbonyl peak area, it is found that light degradation promotes oxidation process, increases the concentration of carbonyl.
It follows that researcher, which mostly uses greatly infra-red sepectrometry, has studied the anti-aging of matrix pitch, SBS modified pitch etc.
Performance, and for the anti-aging property of THFS modified pitch, researcher also seldom relates to.Therefore, it is necessary to develop a kind of base
In the method for examination of infrared spectrum THFS modified pitch anti-aging properties.
Invention content
For overcome the deficiencies in the prior art, the present invention is provided one kind and is changed based on examination of infrared spectrum tetrahydrofuran soluble matter
Property pitch anti-aging property method, this method is simple, easy to operate, energy consumption is low.
The present invention provides the following technical solutions：
A method of based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property, with tetrahydrofuran
Soluble matter (THFS) prepares tetrahydrofuran soluble matter modified pitch as modifying agent to matrix pitch modification, then can to tetrahydrofuran
Molten object modified pitch simulates short ageing, before then infrared spectrometer being used to test tetrahydrofuran soluble matter modified pitch aging,
Functional group afterwards calculates tetrahydrofuran soluble matter modified pitch aging forward and backward carbonyl and sulfoxide group peak area, utilizes tetrahydrochysene furan
The forward and backward carbonyl of soluble matter of muttering modified pitch aging and sulfoxide group peak area ratio analyze its anti-aging property, finally determine four
The optimum addition range of hydrogen furans soluble matter.
Component and content in THFS：Saturation point：0.3%；, fragrance point：3.1%, asphalitine：30.7% and colloid：
65.9%
The present invention selects the peak face of infrared spectrometer test THFS modified pitch carbonyl and sulfoxide group before and after short ageing
Product calculates the peak area ratio before and after carbonyl and sulfoxide group aging, and the ageing resistance of THFS modified pitch is evaluated from microcosmic angle
Can, to improving the utility value of DCLR or THFS and its reasonable development being had positive effect at asphalt modifier.
It is preferably in said program, the tetrahydrofuran soluble matter being obtained by extraction from coal directly-liquefied residue (DCLR)
(THFS) it is used as modifying agent.
It is preferably in any of the above-described scheme, including following steps are rapid：
Step 1：With tetrahydrofuran (THF) for extractant, coal directly-liquefied residue (DCLR) is extracted；
Step 2：The tetrahydrofuran soluble matter (THFS) being obtained by extraction from coal directly-liquefied residue (DCLR) is as modification
Agent prepares tetrahydrofuran soluble matter (THFS) modified pitch；
Step 3：Short ageing is simulated to tetrahydrofuran soluble matter (THFS) modified pitch；
Step 4：Using the function that infrared spectrometer test tetrahydrofuran soluble matter (THFS) modified pitch aging is forward and backward
Group calculates tetrahydrofuran soluble matter (THFS) modified pitch aging forward and backward carbonyl and sulfoxide group peak area, utilizes tetrahydrofuran
Soluble matter (THFS) modified pitch aging forward and backward carbonyl and sulfoxide group peak area ratio analyze its anti-aging property；
Step 5：Determine the optimum addition range of tetrahydrofuran soluble matter (THFS).
It is preferably in any of the above-described scheme, before being extracted to coal directly-liquefied residue (DCLR), test matrix drip
Green, coal directly-liquefied residue (DCLR) properties.
It is preferably in any of the above-described scheme, in step 1, before extraction, coal directly-liquefied residue (DCLR) will be ground
It is less than the particle of 2mm at grain size.
It is preferably in any of the above-described scheme, in step 1, the coal directly-liquefied residue (DCLR) after grinding is passed through
The square hole screen of 2.36mm is collected and is extracted less than 1.18mm, the DCLR particles more than 0.075mm.It can be with THF extractants more
Good contact so that extraction is more abundant.
It is preferably in any of the above-described scheme, in step 1, when extraction is extracted using Soxhlet extractor.It can basis
Extractant boiling point is different with environment temperature and adjusts heating temperature, and sample is impregnated and extracted repeatedly in extractive process, to reach
To rapid extraction purpose.Meanwhile when can recycle high extractant, the dosage for reducing extractant, extraction efficiency, saving automatically
Between.
It is preferably in any of the above-described scheme, in step 1, heating temperature when extraction is 70-90 DEG C.Extract at this temperature
It takes more fully.
It is preferably in any of the above-described scheme, in step 1, extraction process needs 20-25h, extraction more abundant.
It is preferably in any of the above-described scheme, in step 1, collects tetrahydrofuran soluble matter (THFS) solution, and further
In 80 DEG C of rotary evaporation 30-60min, tetrahydrofuran soluble matter (THFS) is obtained.
It is preferably in any of the above-described scheme, in step 2, when preparing tetrahydrofuran soluble matter (THFS) modified pitch, base
Matter pitch, which is heated to 120-160 DEG C, makes it be in flow regime.This temperature, matrix pitch can be completely melt, and uniform, mobility
It is good.
It is preferably in any of the above-described scheme, in step 3, when preparing tetrahydrofuran soluble matter (THFS) modified pitch, four
Hydrogen furans soluble matter (THFS) is heated to 140 DEG C -160 DEG C, is in molten condition.At this temperature, THFS can melt completely, and
It is even.
It is preferably in any of the above-described scheme, in step 3, when preparing tetrahydrofuran soluble matter (THFS) modified pitch, four
Hydrogen furans soluble matter (THFS) and matrix pitch are according to being that 4%-10% is blended in mass ratio.
Within the scope of 4-10%, chooses the THFS that additive amount is 4%, 6%, 8%, 10% and be added separately to matrix pitch
In, it is uniformly mixed, prepares several THFS modified pitch, test the technical indicator of above-mentioned 4 kinds of THFS modified pitch, ensure its technology
Index meets《Standard specification for construction and acceptance of highway asphalt pavement》Technical stipulation in relation to pitch in (JTG F40-2004).
It is preferably in any of the above-described scheme, in step 3, when preparing tetrahydrofuran soluble matter (THFS) modified pitch, altogether
Mixed object is in 150 DEG C of -170 DEG C of down cuts.Temperature is selected to be less than 150 DEG C, THFS modified pitch is excessively sticky to be unfavorable for testing；Temperature
Higher than 170 DEG C pitches are easy aging.Within this temperature range, matrix pitch can be sufficiently mixed with THFS, and be uniformly mixed.
It is preferably in any of the above-described scheme, the shear rate of boxshear apparatus is 4000-6000r/min.Under the rate, mixing
More uniformly, fully.
It is preferably in any of the above-described scheme, shear time 60-90min.It is because when shearing to select the time range
Between it is too short THFS modified pitch can be caused uneven, shear time be more than 90min can cause THFS performance of modified bitumen be deteriorated.
It is preferably in any of the above-described scheme, in step 3, tetrahydrofuran soluble matter (THFS) modified pitch is simulated short
Phase aging, using rotating thin film heated oven.
It being preferably in any of the above-described scheme, in step 3, the heating temperature of rotating thin film heated oven is 163 DEG C ±
0.5℃。
It is preferably in any of the above-described scheme, in step 3, rotating thin film heated oven preheats at 163 DEG C ± 0.5 DEG C
No less than 16h.
It is preferably in any of the above-described scheme, in step 3, the rotating speed of the toroidal frame of rotating thin film heated oven is 15r/
min±0.2r/min。
Be preferably in any of the above-described scheme, in step 3, rotating thin film heat when ventilatory capacity be 4000mL/min ±
200mL/min。
It is preferably in any of the above-described scheme, in step 3, tetrahydrofuran soluble matter (THFS) modified pitch is simulated in short term
Ageing time is 75-85min.
Reference may be selected in the aging condition of the present invention《Highway engineering pitch and Asphalt Mixture Experiment regulation》(JTG E20-
2011)。
It is preferably in any of the above-described scheme, in step 4, the functional group of tetrahydrofuran soluble matter (THFS) modified pitch
37 Fourier Transform Infrared Spectrometer of Tensor produced using German Bruker Optics is analyzed, scanning range is
4000-400cm-1Wave number, scanning times are 120 times, and the infrared waves for being 0.75 μm -1000 μm with wavelength carry out test specimen
Irradiation.
It is preferably in any of the above-described scheme, it is in step 4, tetrahydrofuran soluble matter (THFS) modified pitch sample is molten
In trichloro ethylene organic solvent, it is then applied to potassium bromide (KBr) salt on piece, it is after the solvent is volatilized, infrared using Fourier
Spectroanalysis instrument is tested, and required infrared spectrogram is obtained.
It is preferably in any of the above-described scheme, it, can be according to feature using the infrared spectrogram of the pitch in step 4
Position analysis carbonyl (C=O) functional group at peak (typically occurs in 1550-1800cm-1) and sulfoxide group (S=O) functional group is (usually
Appear in 1000-1200cm-1) with the variation of ageing process, indicate carbonyl (C=O) and sulfoxide (S using the size of absorbance
=O) base functional group concentration.
It is preferably in any of the above-described scheme, in step 4, carbonyl (C=O) takes 1599cm-1The absorption peak at place, sulfoxide group
(S=O) 1032cm is taken-1Absorption peak.
It is preferably in any of the above-described scheme, in step 4, tetrahydrochysene furan is calculated using infrared spectrum processing (OMNIC) software
The peak area of the forward and backward carbonyl of soluble matter of muttering (THFS) modified pitch aging (C=O) and sulfoxide group (S=O).
It is preferably in any of the above-described scheme, in step 4, by calculating different addition quantity tetrahydrofuran soluble matter (THFS)
The ratio of peak area and peak area before aging, obtains aging after the carbonyl (C=O) of modified pitch and sulfoxide (S=O) base aging
Forward and backward carbonyl (C=O) peak area ratio and sulfoxide group (S=O) area ratio.
It is preferably in any of the above-described scheme, in step 5, analyzes the carbonyl of tetrahydrofuran soluble matter (THFS) modified pitch
Existing correlativity between base (C=O) peak area ratio and sulfoxide group (S=O) area ratio and THFS volumes, utilizes correlation
Property coefficient evaluates the relationship between ageing of asphalt and THFS volumes.
It is preferably in any of the above-described scheme, in step 5, by analyzing different tetrahydrofuran soluble matter (THFS) volumes
The situation of change of the lower forward and backward carbonyl of modified pitch aging (C=O) peak area and sulfoxide group (S=O) area ratio judges tetrahydrochysene
The degree of aging of furans soluble matter (THFS) modified pitch determines best tetrahydrofuran soluble matter (THFS) volume model with this
It encloses.
The present invention is a kind of method based on examination of infrared spectrum THFS modified pitch anti-aging properties, and test THFS is modified
The forward and backward infrared spectrogram of ageing of asphalt obtains carbonyl 1599cm by OMNIC softwares-1With sulfoxide group 1032cm-1Peak face
Product calculates the forward and backward carbonyl of aging and sulfoxide group peak area ratio to evaluate the anti-aging of the modified pitch of different THFS additive amounts
Performance, so that it is determined that the optimum addition of THFS, it will be to THFS reasonable developments be of great significance at asphalt modifier.This hair
Bright evaluation method is the anti-aging property of THFS modified pitch to be evaluated from microcosmic angle, and this method is simple, easy to operate, consumption
It can be low.
The country for this new material of THFS modified pitch Study on Anti-ageing also simply by macro property index
Its ageing resistance is evaluated in test, the present invention passes through experimental study, it was demonstrated that is evaluated from microcosmic angle using infrared spectrum technology
The ageing resistance of this modified pitch is also reasonable.
Description of the drawings
Fig. 1 is an a kind of preferred reality of method based on examination of infrared spectrum THFS modified pitch anti-aging properties of the present invention
Apply the Soxhlet extractor of example；
Fig. 2 is the infrared spectrogram before and after the THFS modified pitch agings of embodiment illustrated in fig. 11；
Fig. 3 is the forward and backward carbonyl peak area of the 1THFS modified pitch agings of embodiment illustrated in fig. 1；
Fig. 4 is the forward and backward sulfoxide group peak area of the THFS modified pitch agings of embodiment illustrated in fig. 11；
Fig. 5 is SPI, VAI, RPR, RD of modified pitch under difference THFS volumes in embodiment 2 with the variation of THFS volumes.
Specific implementation mode
In order to further appreciate that the technical characteristic of the present invention, the present invention is explained in detail with reference to specific embodiment
It states.Embodiment only has illustrative effect to the present invention, without the effect of any restrictions, those skilled in the art
The modification for any unsubstantiality made on the basis of the present invention should all belong to the scope of protection of the present invention.
Embodiment 1：
This example selects the SK-90 matrix pitches of South Korea's import, according to《Highway engineering pitch and Asphalt Mixture Experiment rule
Journey》Pertinent regulations in (JTG E20-2011) have carried out correlated performance test to SK-90, and test result is shown in Table 1.
The performance of 1 SK-90 of table
As shown in Table 1, the properties for the SK-90 that this example is selected are satisfied by《Standard specification for construction and acceptance of highway asphalt pavement》
Associated specifications in (JTG F40-2004).
The DCLR that this example is selected is that Baotou Coal Chemical Branch of Shenhua Coal to Liquid and Chemical Co., Ltd. is direct in coal
The by-product generated in liquefaction process, appearance are in black powder.According to《Highway engineering pitch and Asphalt Mixture Experiment rule
Journey》Relevant regulations in (JTG E20-2011) test the performance of DCLR, and test result is shown in Table 2.
2 DCLR performances of table
As shown in Table 2, DCLR needle penetrations, ductility are very small under room temperature, illustrate that DCLR is harder crisp, cryogenic property is poor.
This example selects tetrahydrofuran (THF) solvent of the Xuzhou City of Jiangsu Province bio tech ltd Suo Tong supply,
For colourless transparent liquid, molecular formula C4H8O, the product are mainly used for extracting a kind of middle polarity extractant when DCLR.It utilizes
Soxhlet extraction device extracts DCLR using THF as extractant, and device Soxhlet extractor schematic diagram is as shown in Figure 1, wherein 1-
Condenser pipe, 2-extraction tubes, 3-siphon pipes, 4-5-extraction flasks of connecting tube.
According to《Highway engineering pitch and Asphalt Mixture Experiment regulation》Relevant regulations in (JTG E20-2011), measure
The density of THFS is 1.14g/cm3, softening point is 150 DEG C, and performance is shown in Table 3.
The performance of 3 THFS of table
As shown in Table 3, compared with DCLR, the penetration index and ductility value of THFS increase, and softening point reduces, and illustrates to DCLR
After being extracted, obtained THFS softens, ductility enhancing.
It is separately added into the THFS that additive amount is 4.0%, 6.0%, 8.0%, 10.0% in matrix pitch, prepares THFS and changes
Property pitch, and short ageing is simulated to THFS modified pitch using rotary thin film in drying oven, according to 163 DEG C of heating temperature, annular
Frame rotating speed is set to 15r/min, and ventilatory capacity when heating is that 4000mL/min simulates short ageing, ageing time 75min.
Using Fourier Transform Infrared Spectrometer, test THFS modified pitch before ageing, after infrared spectrogram such as Fig. 2
It is shown, it is modified using the forward and backward carbonyl of ageing of asphalt and sulfoxide group functional group peak area ratio size evaluation different addition quantity THFS
The anti-aging property of pitch.
By OMNIC processing softwares, be calculated THFS modified pitch before ageing, rear 1599cm-1Locate carbonyl and
1032cm-1The peak area ratio for locating sulfoxide group, is shown in Fig. 3.
The forward and backward carbonyl peak area of the 4 adulteration modified ageings of asphalt of difference THFS of table
The forward and backward sulfoxide group peak area of the 5 adulteration modified ageings of asphalt of difference THFS of table
By Fig. 3, Fig. 4 and table 4, table 5 are understood：
(1) due to the aging of pitch, the carbonyl content in THFS modified pitch increases, and shows as the increasing of carbonyl peak area
Greatly, the forward and backward carbonyl peak area of 0%THFS modified pitch (SK-90 pitches) aging increases to 0.014 by 0.008, improves
75.00%, illustrate that aging makes the carbonyl concentration of pitch be continuously increased.It is modified under different THFS volumes compared to SK-90 pitches
The increasing degree of the forward and backward peak area of ageing of asphalt increases with the increase of THFS volumes.Meanwhile the carbonyl concentration after ageing of asphalt
It is apparently higher than increasing degree of the carbonyl concentration before ageing of asphalt with THFS volumes with the increasing degree of THFS volumes.This is mainly
Because the aging of pitch makes some C=C in pitch be broken and reacts with oxygen to generate carbonyl, under heat and oxygen effect, reaction
It can continue to carry out.
(2) THFS addition and being continuously increased with volume, the carbonyl peak area ratio of pitch be continuously increased, illustrating to drip
Green anti-aging property is constantly reducing.Meanwhile being continuously increased with THFS volumes, the carbonyl peak area ratio and THFS of pitch
There is good linear relationships, relative coefficient to be up to 0.9888 between volume, illustrates the addition of THFS and volume is higher, drip
Green anti-aging property is poorer.
(3) THFS addition and being continuously increased with volume, the sulfoxide group peak area after ageing of asphalt be apparently higher than pitch
Sulfoxide group peak area before aging illustrates that aging makes the sulfoxide group concentration of pitch be continuously increased.Compared to SK-90 pitches, no
Increasing degree with the forward and backward peak area of modified pitch aging under THFS volumes increases with the increase of THFS volumes.Meanwhile pitch
The sub- peak base concentration that sub- peak base concentration after aging is apparently higher than before ageing of asphalt with the increasing degree of THFS volumes is mixed with THFS
The increasing degree of amount.This is primarily due to ageing of asphalt and makes organic R-S-R functional groups that hot oxygen reaction occur at high temperature, with oxygen
Solid/liquid/gas reactions generate R-S=O-R sulfoxide groups.
(4) THFS addition and being continuously increased with volume, the sulfoxide group area ratio of pitch be continuously increased, illustrating to drip
Green anti-aging property is constantly reducing.Meanwhile being continuously increased with THFS volumes, the sub- peak base area ratio and THFS of pitch
There is good linear relationships, relative coefficient to be up to 0.9146 between volume, illustrates the addition of THFS and volume is higher, drip
Green anti-aging property is poorer.
(5) from figure 3, it can be seen that 4%, 6%, 8%, the forward and backward carbonyl peak of its aging of the modified pitch of 10%THFS volumes
Area increases 75.00%, 81.25%, 94.74% and 104.76% respectively.From fig. 4, it can be seen that when THFS volumes are more than
When 6%, the sulfoxide group area increasing degree for representing bitumen blowing product significantly increases, and sulfoxide group area is more apparent than increasing degree
Increase, illustrates that the anti-aging property of THFS pitches at this time drastically declines.In conclusion recommending THFS the optimum mix amounts that should control
Within 6%.
Embodiment 2：
This example selects the SK-90 matrix pitches of South Korea's import, according to《Highway engineering pitch and Asphalt Mixture Experiment rule
Journey》Pertinent regulations in (JTG E20-2011) have carried out correlated performance test to SK-90, and test result is shown in Table 6.
The performance of 6 SK-90 of table
As shown in Table 6, the properties for the SK-90 that this example is selected are satisfied by《Standard specification for construction and acceptance of highway asphalt pavement》
Associated specifications in (JTG F40-2004).
The DCLR that this example is selected is that Baotou Coal Chemical Branch of Shenhua Coal to Liquid and Chemical Co., Ltd. is direct in coal
The by-product generated in liquefaction process, appearance are in black powder.According to《Highway engineering pitch and Asphalt Mixture Experiment rule
Journey》Relevant regulations in (JTG E20-2011) test the performance of DCLR, and test result is shown in Table 7.
7 DCLR performances of table
As shown in Table 7, DCLR needle penetrations, ductility are very small under room temperature, illustrate that DCLR is harder crisp, cryogenic property is poor.
This example selects tetrahydrofuran (THF) solvent of the Xuzhou City of Jiangsu Province bio tech ltd Suo Tong supply,
For colourless transparent liquid, molecular formula C4H8O, the product are mainly used for extracting a kind of middle polarity extractant when DCLR.It utilizes
Soxhlet extraction device extracts DCLR using THF as extractant, and device Soxhlet extractor schematic diagram is as shown in Figure 1, wherein 1-
Condenser pipe, 2-extraction tubes, 3-siphon pipes, 4-5-extraction flasks of connecting tube.
According to《Highway engineering pitch and Asphalt Mixture Experiment regulation》Relevant regulations in (JTG E20-2011), measure
The density of THFS is 1.14g/cm3, softening point is 150 DEG C, and performance is shown in Table 8.
The performance of 8 THFS of table
As shown in Table 8, compared with DCLR, the penetration index and ductility value of THFS increase, and softening point reduces, and illustrates to DCLR
After being extracted, obtained THFS softens, ductility enhancing.
It is separately added into the THFS that additive amount is 4.0%, 6.0%, 8.0%, 10.0% in matrix pitch, prepares THFS and changes
Property pitch.
This experiment studies THFS modified pitch anti-aging properties the macro property based on asphalt material.
Short ageing is simulated to THFS modified pitch using rotary thin film in drying oven, according to 163 DEG C of heating temperature, toroidal frame
Rotating speed is set to 15r/min, and ventilatory capacity when heating is that 4000mL/min simulates short ageing, ageing time 75min.To aging
Front and back THFS modified pitch carries out testing performance index, includes mainly：Softening point, viscosity, needle penetration and ductility, and calculate soft
Change point increment (SPI, SPI=T2-T1, wherein T1And T2The respectively forward and backward softening point of ageing of asphalt, DEG C), viscosity ageing index
(VAI, VAI=(η2-η1)/η1, wherein η1And η2Respectively 135 DEG C of forward and backward viscositys of ageing of asphalt, Pa.s), residual needle penetration
Than (RPR, RPR=P2/P1× 100%, wherein P1And P2The respectively forward and backward needle penetration of ageing of asphalt, 0.1mm) and residual prolong
Degree (RD, RD are the ductility after ageing of asphalt, cm).
Evaluate the anti-aging property of THFS modified pitch jointly using above-mentioned SPI, VAI, RPR, RD.
Fig. 5 is SPI, VAI, RPR, RD of modified pitch under different THFS volumes with the variation of THFS volumes.It can by Fig. 5
Know：
(1) addition of THFS and being continuously increased with volume, the SPI and VAI of pitch are gradually increased, and RPR and RD are gradual
It reduces, illustrates that the anti-aging property of THFS modified pitch is constantly being deteriorated.Meanwhile SPI, VAI and RPR and THFS volumes of pitch
Between there is good linear relationships, relative coefficient to be all higher than 0.8.Relative to SK-90 pitches, when 4%THFS is added,
RD drastically declines, and has dropped 77.5%, and the correlation between RD and THFS volumes is poor.
(2) SPI, VAI, RPR, RD value of THFS modified pitch variation degree in different THFS volumes section are poor
It is different.It is less than as SPI, VAI of pitch are respectively less than 20%, the RPR ranges of decrease in the amplification of THFS volumes section (0-4% or 4%-6%)
2%；But when THFS volumes increase to 8% from 6%, SPI, VAI of pitch are sharply increased, amplification is respectively 29.6%,
54.8%, the RPR range of decrease increase to 5.5% from 0.6%, illustrate when THFS volumes be more than 6% when, THFS modified pitch it is anti-aging
Performance drastically declines.In conclusion recommending THFS volumes that should control within 6%.
Claims (10)
1. a kind of method based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property, can with tetrahydrofuran
Molten object prepares tetrahydrofuran soluble matter modified pitch as modifying agent to matrix pitch modification, then is modified to tetrahydrofuran soluble matter
Pitch simulates short ageing, the function for then using infrared spectrometer test tetrahydrofuran soluble matter modified pitch aging forward and backward
Group calculates tetrahydrofuran soluble matter modified pitch aging forward and backward carbonyl and sulfoxide group peak area, utilizes tetrahydrofuran soluble matter
The forward and backward carbonyl of modified pitch aging and sulfoxide group peak area ratio analyze its anti-aging property, finally determine that tetrahydrofuran can
The optimum addition range of molten object.
2. the side as described in claim 1 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：The tetrahydrofuran soluble matter being obtained by extraction from coal directly-liquefied residue is as modifying agent.
3. as claimed in claim 1 or 2 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：It is rapid including following steps：
Step 1：Using tetrahydrofuran as extractant, coal directly-liquefied residue is extracted；
Step 2：For the tetrahydrofuran soluble matter being obtained by extraction from coal directly-liquefied residue as modifying agent, preparing tetrahydrofuran can
Molten object modified pitch；
Step 3：Short ageing is simulated to tetrahydrofuran soluble matter modified pitch；
Step 4：Using the functional group that infrared spectrometer test tetrahydrofuran soluble matter modified pitch aging is forward and backward, tetrahydrochysene is calculated
The forward and backward carbonyl of furans soluble matter modified pitch aging and sulfoxide group peak area, it is old using tetrahydrofuran soluble matter modified pitch
Change forward and backward carbonyl and sulfoxide group peak area ratio analyzes its anti-aging property；
Step 5：Determine the optimum addition range of tetrahydrofuran soluble matter.
4. the side as claimed in claim 3 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：Before being extracted to coal directly-liquefied residue, test matrix pitch, coal directly-liquefied residue items
Energy.
5. the side as claimed in claim 4 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, before extraction, the particle that grain size is less than 2mm will be ground into coal directly-liquefied residue.
6. the side as claimed in claim 5 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, by the coal directly-liquefied residue after grinding by the square hole screen of 2.36mm, collection is less than
1.18mm, the coal directly-liquefied residue particle more than 0.075mm are extracted.
7. the side as claimed in claim 3 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, when extraction, is extracted using Soxhlet extractor.
8. the side as claimed in claim 7 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, heating temperature when extraction is 70-90 DEG C.
9. the side as claimed in claim 8 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, extraction process needs 20-25h.
10. the side as claimed in claim 9 based on examination of infrared spectrum tetrahydrofuran soluble matter modified pitch anti-aging property
Method, it is characterised in that：In step 1, tetrahydrofuran soluble matter solution is collected, and further in 80 DEG C of rotary evaporation 30-60min,
Obtain tetrahydrofuran soluble matter.
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