CN1493877A - Method of evaluating polymer modified asphalt storage stability - Google Patents
Method of evaluating polymer modified asphalt storage stability Download PDFInfo
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- CN1493877A CN1493877A CNA021445400A CN02144540A CN1493877A CN 1493877 A CN1493877 A CN 1493877A CN A021445400 A CNA021445400 A CN A021445400A CN 02144540 A CN02144540 A CN 02144540A CN 1493877 A CN1493877 A CN 1493877A
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- modified asphalt
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Abstract
A method using microscope to evaluate the storage stability of polymer modified asphalt which is prepared from basic asphalt, thermoplastic rubber polymer containing SBS, SIS and SB, and the stabilizer playing the cross-linking and/or sulfurizing roles through chemical reaction features that a microscope is used to observe the quality of said modified asphalt.
Description
1, technical field
The invention belongs to the evaluation method of polymer modified asphalt character, relate in particular to a kind of evaluation method of polymer modified asphalt storage stability, particularly estimate the method for polymer modified asphalt storage stability (being compatibility) fast.
2, background technology
In order to improve the quality of road asphalt, prolong the serviceable life on road surface, at present, pitch is carried out modification with polymkeric substance, become a kind of efficient ways.Because it is bigger that high molecular polymer and pitch are compared molecular weight, density is less, add the difference of other properties, the two is difficult to dissolve each other, even adopt special equipment that polymkeric substance is ground or pulverizes, also be difficult to generally speaking form stabilising system, in case static with pitch, most of polymkeric substance can float and form the polymer phase that is rich in polymkeric substance, and the bottom then is the pitch phase based on pitch.For fear of the generation of lamination, at present, mainly adopt two kinds of methods.The one, processing modified at the construction field (site) pitch, the modified bitumen of producing mixes and stirs, paves the way with aggregate immediately.This method is had relatively high expectations with power to production equipment and production, and production cost is higher, and the unstable properties of modified bitumen is a kind of way of doing something against one's will in addition.Another kind method is by supplementary elements such as adding phase solvent, stabilizing agent or crosslinking chemicals, makes polymkeric substance and pitch reach compatible and not stratified purpose, and modified bitumen can carry out thermmal storage, is suitable for batch production production.
At above-mentioned second kind of method of producing modified bitumen, estimating its storage stability will be an important link.At present, its evaluation method mainly is the cylindrical container with unlike material, different-diameter and height, a certain amount of modified bitumen of packing into, through 48h or the thermmal storage of longer time, sample together with the container cooling of lowering the temperature, is made asphalt solidification, pitch is divided into three sections then, measure the softening point of the two sections pitches in upper and lower respectively, when upper and lower softening point difference is no more than a certain value, think that just storage stability is qualified.Otherwise, the bad and layering of the compatibility that shows polymkeric substance and pitch.Relatively typical method is the method for stipulating among the ASTMD5976-96.Although this method can be used for estimating the storage stability of modified bitumen, but also exist many shortcomings, such as, the time of test cost is long, and a sample needs 55h from start to end at least, and container is had relatively high expectations, certain ratio of height to diameter should be arranged, be convenient to operation again, test error is big, and the error of sample in processes such as cutting, heating and softening point analysis is inevitable.Therefore, can only finish the evaluation means in later stage as production with this method, and can have the purpose that regularly monitoring and adjustment are produced as the compatibility detection method in the production run.
3, summary of the invention
At the problems referred to above, the object of the present invention is to provide a kind of method of fast, accurately estimating polymer modified asphalt storage stability (being compatibility).
Content and method that the present invention is concrete comprise:
At first a small amount of modified bitumen is placed on the clean slide, put cover glass after, pitch is melted in heating, is depressed into thin and thick appropriateness and evenly, is cooled to room temperature then.Open the microscope light source switch, test piece is placed on the microscope stage, adjust the microscope enlargement factor at 4～1600 times, preferred 40～400 times, adjust focal length again, make it to observe till the distinct image.If the enough microscopic examinations of modified bitumen energy are to the dispersion situation or the structure of polymkeric substance, be finely dispersed two-phase, illustrate that then polymkeric substance is that physics is dispersed in the basic asphalt, perhaps not crosslinked mutually well, at this moment, storage Stability of Polymer Modified Asphalt will not reach requirement.On the contrary, if still can't see the disperse state or the structure of polymkeric substance in the modified bitumen when microscope is adjusted to clear picture, then illustrate polymkeric substance molten well by the effect of stabilizing agent or crosslinking chemical be a phase, at this moment, storage Stability of Polymer Modified Asphalt can reach requirement, promptly can not emanate and layering by polymkeric substance after the thermmal storage.
Used instrument and equipment mainly comprises microscope, microslide and cover glass.Used microscope can be an ordinary optical microscope, also can be fluorescence, polarizing microscope etc., first-selected ordinary optical microscope.Used microscope light source can be transmitted light, also can be reflected light etc., first-selected transmitted light.Used microscope enlargement factor is 4～1600 times, and microslide and cover glass are the commercially available universal product.
The present invention is applicable to the modified bitumen of various high molecular polymers and stabilizing agent or crosslinking chemical production, is particularly useful for the pitch that SBS (styrene-butadiene-styrene block copolymer), SIS (styrene-isoprene block copolymer), SB (styrene-butadiene diblock copolymer) or SBR (styrene-butadiene rubber) etc. contain the polymer modification of conjugated diolefine hydrocarbon structure.The inventive method is suitable for estimating polymer modified asphalt storage stability (being compatibility), not only required instrument of this method and equipment are single, and easy and simple to handle, flexible, save time (1～5min can go out the result), laborsaving, visual result, accurately and reliably, can be used as the monitoring means in the production run, be convenient in time pinpoint the problems, solve as early as possible.
4, description of drawings
Fig. 1, the 2nd, the microscopic examination figure of 1 two kinds of samples of the embodiment of the invention, Fig. 3, the 4th, the microscopic examination figure of 2 two kinds of samples of the embodiment of the invention, Fig. 5, the 6th, the microscopic examination figure of 3 two kinds of samples of the embodiment of the invention can know the difference of finding out qualified samples and failed test sample from figure.
5, embodiment
To be further detailed the present invention by embodiment below.
Embodiment 1
Mixed 60 minutes with High shear device at 180 ℃ with 4% SBS with basic asphalt, make polymer modified asphalt A, with the SBS of basic asphalt and 4% and 0.5% stabilizing agent (containing dimorpholinyl disulfide 35%, massicot 50%, carbon black 15%), make polymer modified asphalt B, observe respectively with ordinary optical microscope (transmitted light), wherein enlargement factor is 100 times, and observations is seen Fig. 1 and Fig. 2.The separation test that carries out with the method among the ASTMD5976-96 the results are shown in Table 1.Can find out that from Fig. 1 and Fig. 2 and table 1 can obviously find out the disperse state (shinny part) of polymkeric substance in the image that obtains with microscopic modified bitumen A, it is fine compatible to illustrate that polymkeric substance and basic asphalt do not have, its storage stability is defective.Upper and lower softening point difference is greater than 2 ℃ behind separation test with the method for stipulating among the ASTMD5976-96 for this sample, and storage stability is defective.The unanimity as a result of two kinds of method gained.And in the image of modified bitumen B, can't see the dispersion situation (for a uniform phase) of polymkeric substance.Polymerization and basic asphalt compatibility that this modified bitumen sample is described are fine, and its storage stability is qualified.Upper and lower softening point difference is less than 2 ℃ behind separation test for this sample, and storage stability is qualified.The result of two kinds of method gained is also in full accord.
Embodiment 2
Mixed 60 minutes with High shear device at 180 ℃ with 6% SBS with basic asphalt, make polymer modified asphalt C, with the SBS of basic asphalt and 6% and 0.5% stabilizing agent (containing dimorpholinyl disulfide 35%, massicot 50%, carbon black 15%), make polymer modified asphalt D, with observing respectively with the method for embodiment 1, wherein enlargement factor is 400 times, and observations is seen Fig. 3 and Fig. 4.The separation test that carries out with the method among the ASTMD5976-96 the results are shown in Table 1.Can find out from Fig. 3 and Fig. 4 and table 1, can obviously find out the disperse state (shinny part) of polymkeric substance in the image that obtains with microscopic modified bitumen C, illustrate that polymkeric substance and basic asphalt compatibility are bad, its storage stability does not reach requirement, upper and lower softening point difference is greater than 2 ℃ behind separation test with the method for stipulating among the ASTMD5976-96 for this sample, and storage stability is defective.The unanimity as a result of two kinds of method gained.And in the image of modified bitumen D, can't see the dispersion situation (being a phase) of polymkeric substance.The compatibility that this modified bitumen sample polymer and basic asphalt are described is good, and its storage stability is qualified.This sample upper and lower softening point difference behind separation test illustrates that less than 2 ℃ storage stability is qualified.The result of two kinds of method gained is also in full accord.
The foregoing description shows that further method of the present invention is compared with known method, unanimity as a result, but method of the present invention has advantage easily and efficiently, be any other method can not compare.Therefore, application can be increased work efficiency greatly in real work.
Embodiment 3
Press the method for embodiment 1, just change SBS into SIS, content is 4%, obtains sample E, F, and microscopic examination result (amplifying 600 times) and experimental result are seen Fig. 5,6 and table 1.
Table 1
| Embodiment | ????????1 | ?????????2 | ???????????3 | |||
| The modified bitumen sample | ??A | ??B | ??C | ??D | ??E | ??F |
| SBS(SIS)，m％ | ??4 | ??4 | ??6 | ??6 | ??4 | ??4 |
| Pen. (25 ℃), 1/10mm | ??95 | ??103 | ??73 | ??77 | ??76 | ??77 |
| Softening point, ℃ | ??56.0 | ??53.8 | ??74.5 | ??75.0 | ??61.7 | ??62.3 |
| Ductility (5 ℃), cm | ??68 | ??83 | ??41 | ??41 | ??42 | ??59 |
| Separation test (163 ℃, 48h): softening point is poor, ℃ | ??28.9 | ??0.2 | ??20.5 | ??0.5 | ??8.7 | ??0 |
| Method of the present invention: can see distribution of polymer | Energy | Not | Energy | Not | Energy | Not |
| Storage stability | Defective | Qualified | Defective | Qualified | Defective | Qualified |
Claims (7)
1, a kind of method of estimating the polymer modified asphalt storage stability, it is characterized in that adopting the microscopic examination method to judge the pitch storage stability, at first polymer modified asphalt is placed on the slide, put cover glass after, heating melt to be pressed pitch even, be cooled to room temperature then, in enlargement factor is that 4～1600 microscopically is observed, if image is homodisperse two-phase, then the storage stability of sample is defective, if image is a phase, then the storage stability of sample is qualified.
2,, it is characterized in that described microscope enlargement factor is 40～400 times according to the method for the described evaluation polymer modified asphalt of claim 1 storage stability.
3,, it is characterized in that described microscope is optical microscope, fluorescent microscope or polarizing microscope according to the method for claim 1 or 2 described evaluation polymer modified asphalt storage stabilities.
4,, it is characterized in that described microscope light source is transmitted light or reflected light according to the method for the described evaluation polymer modified asphalt of claim 3 storage stability.
5,, it is characterized in that described polymer modified asphalt is the modified bitumen with high molecular polymer and stabilizing agent or crosslinking chemical production according to the method for the described evaluation polymer modified asphalt of claim 1 storage stability.
6,, it is characterized in that described polymer modified asphalt is the pitch that contains the polymer modification of conjugated diolefine hydrocarbon structure according to the method for claim 1 or 5 described evaluation polymer modified asphalt storage stabilities.
7,, it is characterized in that described polymer modified asphalt is the pitch of SBS, SIS, SB or SBR modification according to the method for the described evaluation polymer modified asphalt of claim 6 storage stability.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02144540 CN1219212C (en) | 2002-11-02 | 2002-11-02 | Method of evaluating polymer modified asphalt storage stability |
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| CN 02144540 CN1219212C (en) | 2002-11-02 | 2002-11-02 | Method of evaluating polymer modified asphalt storage stability |
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| CN1219212C CN1219212C (en) | 2005-09-14 |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105445316A (en) * | 2015-11-13 | 2016-03-30 | 长安大学 | Device and method for testing thermal storage stability of modified asphalt |
| CN105547921A (en) * | 2016-01-04 | 2016-05-04 | 西北民族大学 | Modified asphalt storage stability standard viscosity detection method |
| CN105807036A (en) * | 2016-03-29 | 2016-07-27 | 西安公路研究院 | Determination and evaluation method for emulsified bitumen storage stability |
| CN105928849A (en) * | 2016-04-26 | 2016-09-07 | 长安大学 | Method for evaluating storage stability of penetrated oil layer emulsified asphalt |
| CN110132876A (en) * | 2019-06-05 | 2019-08-16 | 山西省交通科技研发有限公司 | A method of SBS polymer modified pitch hot storage stability is measured based on infrared spectrum technology |
| CN110426318A (en) * | 2019-08-15 | 2019-11-08 | 哈尔滨工业大学 | A kind of evaluation asphalt surface hot fills class base joint grouting glue storage stability test device and test method |
| CN110489858A (en) * | 2019-08-14 | 2019-11-22 | 南京林业大学 | Pitch and SBS Compatibility Evaluation method based on molecular dynamics simulation |
| CN112129731A (en) * | 2020-08-12 | 2020-12-25 | 山东省交通科学研究院 | Method and tool for rapidly detecting storage stability of polymer modified asphalt |
| CN112881226A (en) * | 2019-11-29 | 2021-06-01 | 中石油克拉玛依石化有限责任公司 | Method and experimental device for evaluating storage stability of emulsified asphalt |
| CN114428077A (en) * | 2020-09-30 | 2022-05-03 | 中国石油化工股份有限公司 | Method for analyzing rubber particles in polymer material |
| CN114428076A (en) * | 2020-09-29 | 2022-05-03 | 中国石油化工股份有限公司 | Storage stability judging method and quality control method of polymer modified asphalt |
-
2002
- 2002-11-02 CN CN 02144540 patent/CN1219212C/en not_active Expired - Lifetime
Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105445316A (en) * | 2015-11-13 | 2016-03-30 | 长安大学 | Device and method for testing thermal storage stability of modified asphalt |
| CN105445316B (en) * | 2015-11-13 | 2019-03-01 | 长安大学 | A kind of modified pitch hot storage stability test device and method |
| CN105547921A (en) * | 2016-01-04 | 2016-05-04 | 西北民族大学 | Modified asphalt storage stability standard viscosity detection method |
| CN105807036A (en) * | 2016-03-29 | 2016-07-27 | 西安公路研究院 | Determination and evaluation method for emulsified bitumen storage stability |
| CN105807036B (en) * | 2016-03-29 | 2017-11-14 | 西安公路研究院 | A kind of evaluation of measuring method of emulsified asphalt storage stability |
| CN105928849A (en) * | 2016-04-26 | 2016-09-07 | 长安大学 | Method for evaluating storage stability of penetrated oil layer emulsified asphalt |
| CN110132876A (en) * | 2019-06-05 | 2019-08-16 | 山西省交通科技研发有限公司 | A method of SBS polymer modified pitch hot storage stability is measured based on infrared spectrum technology |
| CN110489858A (en) * | 2019-08-14 | 2019-11-22 | 南京林业大学 | Pitch and SBS Compatibility Evaluation method based on molecular dynamics simulation |
| CN110426318A (en) * | 2019-08-15 | 2019-11-08 | 哈尔滨工业大学 | A kind of evaluation asphalt surface hot fills class base joint grouting glue storage stability test device and test method |
| CN112881226A (en) * | 2019-11-29 | 2021-06-01 | 中石油克拉玛依石化有限责任公司 | Method and experimental device for evaluating storage stability of emulsified asphalt |
| CN112129731A (en) * | 2020-08-12 | 2020-12-25 | 山东省交通科学研究院 | Method and tool for rapidly detecting storage stability of polymer modified asphalt |
| CN112129731B (en) * | 2020-08-12 | 2024-01-23 | 山东省交通科学研究院 | Rapid detection method and detection tool for storage stability of polymer modified asphalt |
| CN114428076A (en) * | 2020-09-29 | 2022-05-03 | 中国石油化工股份有限公司 | Storage stability judging method and quality control method of polymer modified asphalt |
| CN114428077A (en) * | 2020-09-30 | 2022-05-03 | 中国石油化工股份有限公司 | Method for analyzing rubber particles in polymer material |
| CN114428077B (en) * | 2020-09-30 | 2024-04-19 | 中国石油化工股份有限公司 | Method for analyzing rubber particles in polymer material |
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| CN1219212C (en) | 2005-09-14 |
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