CN108169164A - It is a kind of that the method that trichloro ethylene is remained in recycling pitch is detected using FTIR - Google Patents
It is a kind of that the method that trichloro ethylene is remained in recycling pitch is detected using FTIR Download PDFInfo
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- CN108169164A CN108169164A CN201711407203.2A CN201711407203A CN108169164A CN 108169164 A CN108169164 A CN 108169164A CN 201711407203 A CN201711407203 A CN 201711407203A CN 108169164 A CN108169164 A CN 108169164A
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- XSTXAVWGXDQKEL-UHFFFAOYSA-N Trichloroethylene Chemical group ClC=C(Cl)Cl XSTXAVWGXDQKEL-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 229960002415 trichloroethylene Drugs 0.000 title claims abstract description 98
- UBOXGVDOUJQMTN-UHFFFAOYSA-N trichloroethylene Natural products ClCC(Cl)Cl UBOXGVDOUJQMTN-UHFFFAOYSA-N 0.000 title claims abstract description 98
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 title claims abstract description 57
- 238000004064 recycling Methods 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 38
- 238000002835 absorbance Methods 0.000 claims abstract description 122
- 238000001514 detection method Methods 0.000 claims abstract description 67
- 239000010426 asphalt Substances 0.000 claims abstract description 52
- 238000012360 testing method Methods 0.000 claims abstract description 51
- 239000000843 powder Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 239000000463 material Substances 0.000 claims description 23
- 230000008033 biological extinction Effects 0.000 claims description 5
- 239000000126 substance Substances 0.000 description 27
- 238000010438 heat treatment Methods 0.000 description 16
- 235000019738 Limestone Nutrition 0.000 description 12
- 238000013461 design Methods 0.000 description 12
- 239000006028 limestone Substances 0.000 description 12
- 238000005452 bending Methods 0.000 description 10
- 229910052500 inorganic mineral Inorganic materials 0.000 description 6
- 238000007689 inspection Methods 0.000 description 6
- 239000011707 mineral Substances 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 4
- 230000005484 gravity Effects 0.000 description 4
- 230000035515 penetration Effects 0.000 description 4
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 3
- 230000032683 aging Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000010998 test method Methods 0.000 description 3
- 150000001336 alkenes Chemical class 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 238000011017 operating method Methods 0.000 description 1
Classifications
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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
- G01N21/3563—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing solids; Preparation of samples therefor
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- 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)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The present invention provides a kind of methods for being detected using FTIR and trichloro ethylene being remained in recycling pitch, include the following steps：（1）Pure trichloro ethylene is detected using FTIR equipment, demarcates the position of its absorbance wave crest；（2）Original sample pitch is detected using FTIR equipment, demarcates the position of its absorbance wave crest；（3）Comparison（1）With（2）, determine that there are the beam locations of trichloro ethylene in detection pitch；（4）It will（2）In original sample asphalt and aggregate, miberal powder mixes and stirs to form asphalt；（5）Using rotary evaporator method, from（4）In asphalt in obtain recycling pitch；（6）Using FTIR equipment, detection（5）The absorbance of middle recycling pitch；（7）Comparison（2）Middle original sample pitch absorbance and（6）Middle recycling pitch absorbance,（3）Difference at determining beam location in the presence of difference, shows to remain trichloro ethylene in recycling pitch.The method of the present invention testing result is intuitively true and reliable, effectively avoids human error.
Description
Technical field
The present invention relates to a kind of recycling test methods of road engineering material more particularly to a kind of use FTIR to detect back
Receive the method that trichloro ethylene is remained in pitch.
Background technology
Applied of Asphalt Pavement Recycle Technique saves the valuable money such as building stones, pitch because its resourcebility is using old bitumen pavement material
Source, environmental protection reduce the advantages such as investment cost, more and more extensive to be built applied to the repair of highway in China asphalt pavement conserving
In if.The key of Applied of Asphalt Pavement Recycle Technique is the degree of aging of accurate evaluation Bituminous concrete surface, so as to instruct new pitch label or again
The selection of raw agent type, it is ensured that Bituminous concrete surface regenerates completely, and the surplus value of old bitumen pavement material is fully used.For evaluation
The degree of aging of Bituminous concrete surface need to recycle from old bitumen pavement material obtain Bituminous concrete surface first, secondly carry out Bituminous concrete surface performance and refer to
Target measures, and therefore, recycling obtains the premise that pure Bituminous concrete surface is its performance of accurate evaluation.
《Highway engineering pitch and Asphalt Mixture Experiment regulation》It is proposed from asphalt in (JTG E20-2011)
The method for recycling pitch, process are to dissolve old asphalt mixture using trichloro ethylene first, and Bituminous concrete surface is dissolved in three at this time
In vinyl chloride, so as to it is old gather materials detach；Secondly the mixed solution of distillation trichloro ethylene and Bituminous concrete surface, utilizes trichloro ethylene boiling point
Trichloro ethylene is evaporated, so as to recycle acquisition Bituminous concrete surface by the feature low compared with pitch from the mixed solution of the two.However from
Evaporating completely trichloro ethylene is not easy in the mixed solution of trichloro ethylene and Bituminous concrete surface, and is seen at present with experimental implementation person's naked eyes
Whether examine, which has trichloro ethylene vapour to coagulate recycling and be used as, judges that it evaporates whether complete standard is very coarse, often results in returning for acquisition
Residual fraction trichloro ethylene in pitch is received, influences to recycle the purity of pitch, causes Bituminous concrete surface Aging level evaluation inaccurate.
Invention content
The present invention provides a kind of methods for being detected using FTIR and trichloro ethylene being remained in recycling pitch, have been put forward for the first time pair
Recycle the detection method that trichloro ethylene is remained in pitch.
The present invention is realized using following scheme：
The present invention is a kind of to detect the method that trichloro ethylene is remained in recycling pitch using FTIR, including following operating procedure：
(1) using FTIR equipment, the absorbance of pure trichloro ethylene is detected, calibration trichloro ethylene absorbance presents apparent
The beam location of wave crest；
(2) using FTIR equipment, the absorbance of original sample pitch is detected, the wave number of apparent wave crest is presented in calibration pitch absorbance
Position；
(3) beam location of trichloro ethylene absorbance wave crest detected in comparison (1), with the original sample pitch detected in (2)
The beam location of absorbance wave crest determines that there are the beam locations of trichloro ethylene in detection pitch；
(4) by (2) original sample asphalt and aggregate, miberal powder mixes and stirs and to form asphalt；
(5) using rotary evaporator method, recycling pitch is obtained from the asphalt in (4)；
(6) the recycling pitch in (5) is prepared into sample, using FTIR equipment, the absorbance of detection recycling pitch；
(7) the original sample pitch absorbance of comparison (2) detection and the recycling pitch absorbance of (6) detection, in the inspection that (3) determine
There are the differences at the beam location of trichloro ethylene in survey pitch, in the presence of difference, show to remain trichlorine in recycling pitch
Ethylene.
As preference, a kind of detect the method that trichloro ethylene is remained in recycling pitch using FTIR, tested in (1)
Wave-number range is 600-4000cm-1, detection output valve is absorbance.
As preference, a kind of detect the method that trichloro ethylene is remained in recycling pitch using FTIR, tested in (2)
Wave-number range is 600-4000cm-1, detection output valve is absorbance.
As preference, a kind of detect the method that trichloro ethylene is remained in recycling pitch using FTIR, collect in (4)
Material, miberal powder and original sample pitch mass percent be：The miberal powder of 4~8wt%, the original sample pitch of 3~6wt%, remaining is to gather materials,
Its gross mass meets 100%.
As preference, a kind of detect the method that trichloro ethylene is remained in recycling pitch using FTIR, tested in (6)
Wave-number range is 600-4000cm-1, detection output valve is absorbance.
Wherein, original sample pitch is bi tumenf orr oad or modified pitch, gathers materials and commonly uses material of building the road for limestone or basalt
Material, miberal powder are limestone mineral powder, and the design level of asphalt is matched often uses bituminous pavement design grading for AC or SMA.
The beneficial functional of the present invention is：
Due to the stretching vibration of the out-of-plane bending vibration and-C-Cl chemical bonds of-C-H chemical bonds, FTIR in trichloro ethylene
It will be in wave number 750-1000cm in detection process-1In the range of show apparent absorbance wave crest；Due to-C-H chemical bonds in pitch
In-plane bending vibration, the stretching vibration of-C-H chemical bonds and the skeletal vibration of-C-C chemical bonds, will in FTIR detection process
In wave number 1500cm-1、2800cm-1Nearby show apparent absorbance wave crest, and in 750-1000cm-1In the range of, pitch chemistry
There is not wave crest in the absorbance of key.With reference to absorbance wave crest size and chemical bond concentration Bouguer law in a linear relationship, work as drip
When containing trichloro ethylene in blueness, due to the introducing of-C-Cl chemical bonds, pitch can be caused in wave number 750-1000cm-1In the range of
Absorbance changes, and judges remaining trichloro ethylene in recycling pitch accordingly.
In the present invention, using FTIR detection methods, detection process rapidly and efficiently, detection data have good uniformity and
Stability, testing result is accurately and reliably and with distinct comparativity.
In the present invention, it is that limestone or basalt often use road-making material to gather materials, and miberal powder is limestone mineral powder, and original sample pitch is
Bi tumenf orr oad or modified pitch, test method are not limited by experiment material, and with general applicability.Asphalt
Design level is matched often uses bituminous pavement design grading for AC or SMA, and test method is not limited by mixture gradation type, and is had
General applicability.
In the present invention, original sample pitch absorbance is detected, and compared with trichloro ethylene absorbance using FTIR, is demarcated
The beam location of notable difference is presented in pitch and trichloro ethylene absorbance wave crest, so that it is determined that there are three chloroethenes in detection pitch
The beam location of alkene.
In the present invention, the absorbance of recycling pitch and original sample pitch is detected using FTIR, by comparing the absorbance of the two,
Remaining three chloroethene in pitch is recycled in the difference at beam location in the detection pitch determined there are trichloro ethylene, judgement
Alkene, forms whether the trichloro ethylene based on high accuracy testing inspection evaporates complete criterion, with conventional using artificial
The roughness standard whether naked-eye observation has trichloro ethylene vapour to coagulate recycling is compared, and criterion is intuitive, and eliminates human error
It influences, judging result is accurately and reliably.
The method of the present invention have it is easy to operate, rapidly and efficiently, be easily achieved, be easy to grasp with promote, testing result it is straight
See true and reliable, effective the advantages of avoiding human error.
Description of the drawings
Fig. 1 is the absorbance detection result of 1 trichloro ethylene of embodiment；
Fig. 2 is the absorbance detection result of 1 original sample SBS modified pitch of embodiment；
Fig. 3 is that embodiment 1 determines that there are the beam locations of trichloro ethylene in detection SBS modified pitch；
Fig. 4 is the absorbance detection result that embodiment 1 recycles SBS modified pitch；
Fig. 5 is that embodiment 1 recycles the absorbance of SBS modified pitch and the absorbance comparison of original sample SBS modified pitch；
Fig. 6 is the absorbance detection result of 2 trichloro ethylene of embodiment；
Fig. 7 is the absorbance detection result of 2 original sample SBS modified pitch of embodiment；
Fig. 8 is that embodiment 2 determines that there are the beam locations of trichloro ethylene in detection SBS modified pitch；
Fig. 9 is the absorbance detection result that embodiment 2 recycles SBS modified pitch；
Figure 10 is that embodiment 2 recycles the absorbance of SBS modified pitch and the absorbance comparison of original sample SBS modified pitch；
Figure 11 is the absorbance detection result of 3 trichloro ethylene of embodiment；
Figure 12 is the absorbance detection result of 3 original sample SBS modified pitch of embodiment；
Figure 13 is that embodiment 3 determines that there are the beam locations of trichloro ethylene in detection SBS modified pitch；
Figure 14 is the absorbance detection result that embodiment 3 recycles SBS modified pitch；
Figure 15 is that embodiment 3 recycles the absorbance of SBS modified pitch and the absorbance comparison of original sample SBS modified pitch；
Figure 16 is the absorbance detection result of 4 trichloro ethylene of embodiment；
Figure 17 is the absorbance detection result of 4 original sample SBS modified pitch of embodiment；
Figure 18 is that embodiment 4 determines that there are the beam locations of trichloro ethylene in detection SBS modified pitch；
Figure 19 is the absorbance detection result that embodiment 4 recycles SBS modified pitch；
Figure 20 is that embodiment 4 recycles the absorbance of SBS modified pitch and the absorbance comparison of original sample SBS modified pitch.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
Embodiment 1
The present invention is a kind of to detect the method that trichloro ethylene is remained in recycling pitch using FTIR, includes the following steps：
(1) using FTIR equipment, pure trichloro ethylene is detected in test wave number 600-4000cm-1In the range of extinction
The beam location of apparent wave crest, the result is shown in Figure 1 is presented in degree, calibration trichloro ethylene absorbance.
In trichloro ethylene, due to the stretching vibration of the out-of-plane bending vibration and-C-Cl chemical bonds of-C-H chemical bonds so that
Its FTIR testing result is in wave number 836cm-1、928cm-1Place has apparent absorbance wave crest.
(2) using FTIR equipment, detection original sample pitch is in test wave number 600-4000cm-1In the range of absorbance, calibration
The beam location of apparent wave crest is presented in pitch absorbance.Original sample pitch uses SBS modified pitch, and testing performance index result is shown in
Table 1, FTIR testing results are shown in Fig. 2.
Table 1SBS performance of modified bitumen index test results
| Needle penetration 25 DEG C (0.1mm) | Softening point (DEG C) | Ductility 5 DEG C (cm) |
| 46.7 | 81.6 | 31.0 |
In SBS modified pitch, due to the in-plane bending vibration ,-C-H chemical bonds of-C-H chemical bonds stretching vibration and-
The skeletal vibration of C-C chemical bonds so that its FTIR testing result is in wave number 1455cm-1、2850cm-1、2920cm-1Place has bright
Aobvious absorbance wave crest.
(3) beam location of trichloro ethylene absorbance wave crest detected in comparison (1), with the original sample pitch detected in (2)
The beam location of absorbance wave crest determines as a result to see Fig. 3 there are the beam location of trichloro ethylene in detection pitch.
The beam location of comparison trichloro ethylene absorbance wave crest, the beam location with SBS modified pitch absorbance wave crests, two
The beam location of person's absorbance wave crest is different.According to Bouguer law, when containing trichloro ethylene in SBS modified pitch, SBS is modified
Pitch is in wave number 836cm-1、928cm-1Neighbouring absorbance will change, and determine 836cm-1、928cm-1It is modified for detection SBS
There are the beam locations of trichloro ethylene in pitch.
(4) by (2) original sample asphalt and aggregate, miberal powder mixes and stirs and to form asphalt.Original sample pitch is modified drip for SBS
Blueness is gathered materials using limestone, and the test result of relative density is shown in Table 2.
2 relative density of aggregate result of the test of table
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 |
| Bulk specific gravity | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.757 | 2.746 | 2.728 |
| Apparent relative density | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.718 | 2.713 | 2.701 |
Miberal powder uses limestone mineral powder, and the bitumen aggregate ratio of asphalt is 4.2%, and design level, which is matched, is shown in Table 3.
The design level of 3 asphalt of table is matched
Mixing and stirring detailed process is：It the gathering materials of heating, pitch is added in into indoor small first mixes and 90s is mixed and stirred in pot, secondly will
The miberal powder addition of heating, which is mixed, mixes and stirs 90s in pot, the temperature of the heating aggregate is 180 DEG C, and the temperature of heated asphalt is 165 DEG C,
The temperature for heating miberal powder is 180 DEG C, and it is 175 DEG C to mix and stir temperature.
(5) using rotary evaporator method, recycling pitch is obtained from the asphalt in (4).
(6) the recycling pitch in (5) is prepared into sample, using FTIR equipment, detection recycling pitch is in test wave number 600-
4000cm-1In the range of absorbance, testing result is shown in Fig. 4.
(7) the original sample pitch absorbance of comparison (2) detection and the recycling pitch absorbance of (6) detection, in the inspection that (3) determine
There are the differences at the beam location of trichloro ethylene, comparing result in survey pitch to see Fig. 5.
The absorbance of SBS modified pitch is recycled compared with the absorbance of original sample SBS modified pitch, in wave number 836cm-1、
928cm-1Nearby there are apparent wave crest, therefore recycle in SBS modified pitch and remain trichloro ethylene.
Embodiment 2
The present invention is a kind of to detect the method that trichloro ethylene is remained in recycling pitch using FTIR, includes the following steps：
(1) using FTIR equipment, pure trichloro ethylene is detected in test wave number 600-4000cm-1In the range of extinction
Degree, calibration trichloro ethylene absorbance are presented the beam location of apparent wave crest, as a result see Fig. 6.
In trichloro ethylene, due to the stretching vibration of the out-of-plane bending vibration and-C-Cl chemical bonds of-C-H chemical bonds so that
Its FTIR testing result is in wave number 836cm-1、928cm-1Place has apparent absorbance wave crest.
(2) using FTIR equipment, detection original sample pitch is in test wave number 600-4000cm-1In the range of absorbance, calibration
The beam location of apparent wave crest is presented in pitch absorbance.Original sample pitch uses SBS modified pitch, and testing performance index result is shown in
Table 4, FTIR testing results are shown in Fig. 7.
Table 4SBS performance of modified bitumen index test results
| Needle penetration 25 DEG C (0.1mm) | Softening point (DEG C) | Ductility 5 DEG C (cm) |
| 46.7 | 81.6 | 31.0 |
In SBS modified pitch, due to the in-plane bending vibration ,-C-H chemical bonds of-C-H chemical bonds stretching vibration and-
The skeletal vibration of C-C chemical bonds so that its FTIR testing result is in wave number 1455cm-1、2850cm-1、2920cm-1Place has bright
Aobvious absorbance wave crest.
(3) beam location of trichloro ethylene absorbance wave crest detected in comparison (1), with the original sample pitch detected in (2)
The beam location of absorbance wave crest determines as a result to see Fig. 8 there are the beam location of trichloro ethylene in detection pitch.
The beam location of comparison trichloro ethylene absorbance wave crest, the beam location with SBS modified pitch absorbance wave crests, two
The beam location of person's absorbance wave crest is different.According to Bouguer law, when containing trichloro ethylene in SBS modified pitch, SBS is modified
Pitch is in wave number 836cm-1、928cm-1Neighbouring absorbance will change, and determine 836cm-1、928cm-1It is modified for detection SBS
There are the beam locations of trichloro ethylene in pitch.
(4) by (2) original sample asphalt and aggregate, miberal powder mixes and stirs and to form asphalt.Original sample pitch is modified drip for SBS
Blueness is gathered materials using limestone, and the test result of relative density is shown in Table 5.
5 relative density of aggregate result of the test of table
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 |
| Bulk specific gravity | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.757 | 2.746 | 2.728 |
| Apparent relative density | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.718 | 2.713 | 2.701 |
Miberal powder uses limestone mineral powder, and the bitumen aggregate ratio of asphalt is 4.2%, and design level, which is matched, is shown in Table 6.
The design level of 6 asphalt of table is matched
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 | 16 |
| Pass through quality percentage (%) | 6 | 8 | 12 | 18 | 24 | 36 | 48 | 70 | 95 | 100 |
Mixing and stirring detailed process is：It the gathering materials of heating, pitch is added in into indoor small first mixes and 90s is mixed and stirred in pot, secondly will
The miberal powder addition of heating, which is mixed, mixes and stirs 90s in pot, the temperature of the heating aggregate is 180 DEG C, and the temperature of heated asphalt is 165 DEG C,
The temperature for heating miberal powder is 180 DEG C, and it is 175 DEG C to mix and stir temperature.
(5) using rotary evaporator method, recycling pitch is obtained from the asphalt in (4).
(6) the recycling pitch in (5) is prepared into sample, using FTIR equipment, detection recycling pitch is in test wave number 600-
4000cm-1In the range of absorbance, testing result is shown in Fig. 9.
(7) the original sample pitch absorbance of comparison (2) detection and the recycling pitch absorbance of (6) detection, in the inspection that (3) determine
There are the differences at the beam location of trichloro ethylene, comparing result in survey pitch to see Figure 10.
The absorbance of SBS modified pitch is recycled compared with the absorbance of original sample SBS modified pitch, in wave number 836cm-1、
928cm-1Nearby there are apparent wave crest, therefore recycle in SBS modified pitch and remain trichloro ethylene.
Embodiment 3
The present invention is a kind of to detect the method that trichloro ethylene is remained in recycling pitch using FTIR, includes the following steps：
(1) using FTIR equipment, pure trichloro ethylene is detected in test wave number 600-4000cm-1In the range of extinction
The beam location of apparent wave crest, the result is shown in Figure 11 is presented in degree, calibration trichloro ethylene absorbance.
In trichloro ethylene, due to the stretching vibration of the out-of-plane bending vibration and-C-Cl chemical bonds of-C-H chemical bonds so that
Its FTIR testing result is in wave number 836cm-1、928cm-1Place has apparent absorbance wave crest.
(2) using FTIR equipment, detection original sample pitch is in test wave number 600-4000cm-1In the range of absorbance, calibration
The beam location of apparent wave crest is presented in pitch absorbance.Original sample pitch uses SBS modified pitch, and testing performance index result is shown in
Table 7, FTIR testing results are shown in Figure 12.
Table 7SBS performance of modified bitumen index test results
| Needle penetration 25 DEG C (0.1mm) | Softening point (DEG C) | Ductility 5 DEG C (cm) |
| 46.7 | 81.6 | 31.0 |
In SBS modified pitch, due to the in-plane bending vibration ,-C-H chemical bonds of-C-H chemical bonds stretching vibration and-
The skeletal vibration of C-C chemical bonds so that its FTIR testing result is in wave number 1455cm-1、2850cm-1、2920cm-1Place has bright
Aobvious absorbance wave crest.
(3) beam location of trichloro ethylene absorbance wave crest detected in comparison (1), with the original sample pitch detected in (2)
The beam location of absorbance wave crest determines that there are the beam location of trichloro ethylene, the result is shown in Figure 1s 3 in detection pitch.
The beam location of comparison trichloro ethylene absorbance wave crest, the beam location with SBS modified pitch absorbance wave crests, two
The beam location of person's absorbance wave crest is different.According to Bouguer law, when containing trichloro ethylene in SBS modified pitch, SBS is modified
Pitch is in wave number 836cm-1、928cm-1Neighbouring absorbance will change, and determine 836cm-1、928cm-1It is modified for detection SBS
There are the beam locations of trichloro ethylene in pitch.
(4) by (2) original sample asphalt and aggregate, miberal powder mixes and stirs and to form asphalt.Original sample pitch is modified drip for SBS
Blueness is gathered materials using limestone, and the test result of relative density is shown in Table 8.
8 relative density of aggregate result of the test of table
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 |
| Bulk specific gravity | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.757 | 2.746 | 2.728 |
| Apparent relative density | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.718 | 2.713 | 2.701 |
Miberal powder uses limestone mineral powder, and the bitumen aggregate ratio of asphalt is 4.2%, and design level, which is matched, is shown in Table 9.
The design level of 9 asphalt of table is matched
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 | 16 |
| Pass through quality percentage (%) | 6 | 8 | 12 | 18 | 24 | 36 | 48 | 70 | 95 | 100 |
Mixing and stirring detailed process is：It the gathering materials of heating, pitch is added in into indoor small first mixes and 90s is mixed and stirred in pot, secondly will
The miberal powder addition of heating, which is mixed, mixes and stirs 90s in pot, the temperature of the heating aggregate is 180 DEG C, and the temperature of heated asphalt is 165 DEG C,
The temperature for heating miberal powder is 180 DEG C, and it is 175 DEG C to mix and stir temperature.
(5) using rotary evaporator method, recycling pitch is obtained from the asphalt in (4).
(6) the recycling pitch in (5) is prepared into sample, using FTIR equipment, detection recycling pitch is in test wave number 600-
4000cm-1In the range of absorbance, testing result is shown in Figure 14.
(7) the original sample pitch absorbance of comparison (2) detection and the recycling pitch absorbance of (6) detection, in the inspection that (3) determine
There are the differences at the beam location of trichloro ethylene, comparing result in survey pitch to see Figure 15.
The absorbance of SBS modified pitch is recycled compared with the absorbance of original sample SBS modified pitch, in wave number 836cm-1、
928cm-1Nearby there are apparent wave crest, therefore recycle in SBS modified pitch and remain trichloro ethylene.
Embodiment 4
The present invention is a kind of to detect the method that trichloro ethylene is remained in recycling pitch using FTIR, includes the following steps：
(1) using FTIR equipment, pure trichloro ethylene is detected in test wave number 600-4000cm-1In the range of extinction
The beam location of apparent wave crest, the result is shown in Figure 16 is presented in degree, calibration trichloro ethylene absorbance.
In trichloro ethylene, due to the stretching vibration of the out-of-plane bending vibration and-C-Cl chemical bonds of-C-H chemical bonds so that
Its FTIR testing result is in wave number 836cm-1、928cm-1Place has apparent absorbance wave crest.
(2) using FTIR equipment, detection original sample pitch is in test wave number 600-4000cm-1In the range of absorbance, calibration
The beam location of apparent wave crest is presented in pitch absorbance.Original sample pitch uses SBS modified pitch, and testing performance index result is shown in
Table 10, FTIR testing results are shown in Figure 17.
Table 10SBS performance of modified bitumen index test results
| Needle penetration 25 DEG C (0.1mm) | Softening point (DEG C) | Ductility 5 DEG C (cm) |
| 46.7 | 81.6 | 31.0 |
In SBS modified pitch, due to the in-plane bending vibration ,-C-H chemical bonds of-C-H chemical bonds stretching vibration and-
The skeletal vibration of C-C chemical bonds so that its FTIR testing result is in wave number 1455cm-1、2850cm-1、2920cm-1Place has bright
Aobvious absorbance wave crest.
(3) beam location of trichloro ethylene absorbance wave crest detected in comparison (1), with the original sample pitch detected in (2)
The beam location of absorbance wave crest determines that there are the beam location of trichloro ethylene, the result is shown in Figure 1s 8 in detection pitch.
The beam location of comparison trichloro ethylene absorbance wave crest, the beam location with SBS modified pitch absorbance wave crests, two
The beam location of person's absorbance wave crest is different.According to Bouguer law, when containing trichloro ethylene in SBS modified pitch, SBS is modified
Pitch is in wave number 836cm-1、928cm-1Neighbouring absorbance will change, and determine 836cm-1、928cm-1It is modified for detection SBS
There are the beam locations of trichloro ethylene in pitch.
(4) by (2) original sample asphalt and aggregate, miberal powder mixes and stirs and to form asphalt.Original sample pitch is modified drip for SBS
Blueness is gathered materials using limestone, and the test result of relative density is shown in Table 11.
11 relative density of aggregate result of the test of table
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 |
| Bulk specific gravity | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.757 | 2.746 | 2.728 |
| Apparent relative density | 2.639 | 2.685 | 2.690 | 2.698 | 2.716 | 2.734 | 2.718 | 2.713 | 2.701 |
Miberal powder uses limestone mineral powder, and the bitumen aggregate ratio of asphalt is 4.2%, and design level, which is matched, is shown in Table 12.
The design level of 12 asphalt of table is matched
| Grain size (mm) | 0.075 | 0.15 | 0.3 | 0.6 | 1.18 | 2.36 | 4.75 | 9.5 | 13.2 | 16 |
| Pass through quality percentage (%) | 6 | 8 | 12 | 18 | 24 | 36 | 48 | 70 | 95 | 100 |
Mixing and stirring detailed process is：It the gathering materials of heating, pitch is added in into indoor small first mixes and 90s is mixed and stirred in pot, secondly will
The miberal powder addition of heating, which is mixed, mixes and stirs 90s in pot, the temperature of the heating aggregate is 180 DEG C, and the temperature of heated asphalt is 165 DEG C,
The temperature for heating miberal powder is 180 DEG C, and it is 175 DEG C to mix and stir temperature.
(5) using rotary evaporator method, recycling pitch is obtained from the asphalt in (4).
(6) the recycling pitch in (5) is prepared into sample, using FTIR equipment, detection recycling pitch is in test wave number 600-
4000cm-1In the range of absorbance, testing result is shown in Figure 19.
(7) the original sample pitch absorbance of comparison (2) detection and the recycling pitch absorbance of (6) detection, in the inspection that (3) determine
There are the differences at the beam location of trichloro ethylene, comparing result in survey pitch to see Figure 20.
The absorbance of SBS modified pitch is recycled compared with the absorbance of original sample SBS modified pitch, in wave number 836cm-1、
928cm-1Nearby there are apparent wave crest, therefore recycle in SBS modified pitch and remain trichloro ethylene.
Claims (5)
1. a kind of detect the method that trichloro ethylene is remained in recycling pitch using FTIR, it is characterised in that：Including operating step as follows
Suddenly：
（1）Using FTIR equipment, the absorbance of pure trichloro ethylene is detected, apparent wave crest is presented in calibration trichloro ethylene absorbance
Beam location；
（2）Using FTIR equipment, the absorbance of original sample pitch is detected, the wave number position of apparent wave crest is presented in calibration pitch absorbance
It puts；
（3）Comparison（1）The beam location of the trichloro ethylene absorbance wave crest of middle detection, with（2）The original sample pitch extinction of middle detection
The beam location of wave crest is spent, determines that there are the beam locations of trichloro ethylene in detection pitch；
（4）It will（2）In original sample asphalt and aggregate, miberal powder mixes and stirs to form asphalt；
（5）Using rotary evaporator method, from（4）In asphalt in obtain recycling pitch；
（6）It will（5）In recycling pitch prepare sample, using FTIR equipment, the absorbance of detection recycling pitch；
（7）Comparison（2）The original sample pitch absorbance of detection and（6）The recycling pitch absorbance of detection,（3）Determining detection drip
There are the differences at the beam location of trichloro ethylene in blueness, in the presence of difference, show to remain trichloro ethylene in recycling pitch.
2. a kind of method that residual trichloro ethylene in recycling pitch is detected using FTIR according to claim 1, feature
It is：It is described（1）Middle test wave number ranging from 600-4000cm-1, detection output valve is absorbance.
3. a kind of method that residual trichloro ethylene in recycling pitch is detected using FTIR according to claim 1, feature
It is：It is described（2）Middle test wave number ranging from 600-4000cm-1, detection output valve is absorbance.
4. a kind of method that residual trichloro ethylene in recycling pitch is detected using FTIR according to claim 1, feature
It is：It is described（4）In gather materials, the mass percent of miberal powder and original sample pitch is：The original sample drip of the miberal powder, 3 ~ 6wt% of 4 ~ 8wt%
Blueness, to gather materials, gross mass meets 100% for remaining.
5. a kind of method that residual trichloro ethylene in recycling pitch is detected using FTIR according to claim 1, feature
It is：It is described（6）Middle test wave number ranging from 600-4000cm-1, detection output valve is absorbance.
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