CN112194908A - Polyurethane and rock asphalt composite modified asphalt and preparation method thereof - Google Patents
Polyurethane and rock asphalt composite modified asphalt and preparation method thereof Download PDFInfo
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Abstract
The invention relates to polyurethane and rock asphalt composite modified asphalt and a preparation method thereof, belonging to the technical field of road modified asphalt cement. The asphalt comprises the following components in parts by weight: 1-5 parts of polyurethane modifier, 5-20 parts of rock asphalt and 85-100 parts of matrix asphalt. The optimal mixing amount of the polyurethane and the rock asphalt under the influence of various factors is determined by performing target optimization on the mixing amount of the polyurethane and the rock asphalt. The method has very important values for solving the damage phenomena of cracking, rutting and the like of the asphalt pavement under the natural environment and the driving load condition, prolonging the service life of the road, improving the integrity, smoothness and water tightness of the asphalt pavement and improving the durability and driving comfort of the asphalt pavement.
Description
Technical Field
The invention relates to polyurethane and rock asphalt composite modified asphalt and a preparation method thereof, belonging to the technical field of road modified asphalt cement.
Background
The technical performance of the existing single polymer composite modified asphalt is difficult to meet the severe use requirement of the current high-grade highway, and the polymer modifier is generally expensive, the production process is relatively complex, and the road building cost is increased. Moreover, the compatibility of the conventional polymer modifier with asphalt is poor, and the improvement effect on the asphalt is difficult to realize.
Polyurethane (PU) is a novel organic polymer material containing a repetitive-NHCOO-structural unit arrangement inside. At present, few research reports about the application of PU modified asphalt in the field of road engineering are reported at home and abroad, and the research on the preparation process of the PU modified asphalt and the road performance test of a mixture thereof are mainly focused. Because the thermoplastic PU is stable at normal temperature, but is easily decomposed into isocyanate and phenol when heated to 150 ℃, the bonding position in phenyl carbamate is not firmly bonded and is easily replaced by aliphatic amine or aliphatic alcohol, and the elasticity and the crosslinking degree of the original PU are reduced, so the high temperature resistance of the PU modified asphalt is influenced. Therefore, how to improve the high-temperature performance of the PU modified asphalt is a difficult problem which needs to be overcome at present.
Disclosure of Invention
The invention adds the polyurethane and the rock asphalt into the matrix asphalt to form the asphalt modified by the composite of the polyurethane and the rock asphalt, thereby fully playing the respective performance advantages, leading the asphalt modified by the composite of the polyurethane and the rock asphalt to have better high-temperature and low-temperature rheological properties and the like, solving the problems of cracks, rutting, loosening, frost heaving, slurry turning, sinking, cuddling, oil bleeding, cracking slurry pumping and the like of the matrix asphalt pavement, improving and prolonging the durability and the service life of the pavement.
The invention provides a polyurethane modifier, which comprises the following raw materials in parts by weight:
the invention preferably relates to the raw materials of the polyurethane modifier, which comprise the following components in parts by weight:
the invention also aims to provide a preparation method of the polyurethane modifier, which comprises the following steps: firstly, when the molecular weight of the poly-tetramethyl ether glycol is less than 2000, reacting the poly-butanediol adipate polyester glycol and the poly-tetramethyl ether glycol for 40-60min at the temperature of 110-120 ℃ under nitrogen according to the preset weight part; secondly, cooling the product obtained in the first step to 75-85 ℃, adding 75-85 ℃ 4,4' -diphenylmethane diisocyanate into the product obtained in the first step according to the predetermined weight part, and reacting for 0.3-0.5h at 75-85 ℃; thirdly, cooling the product obtained in the second step to 45-55 ℃, adding 1, 4-butanediol into the product obtained in the second step according to the predetermined weight part, uniformly mixing, and curing at 85-100 ℃ for 12-24 h.
The invention also aims to provide a preparation method of the polyurethane modifier, which comprises the following steps: firstly, when the molecular weight of the poly-tetramethyl ether glycol is more than or equal to 2000, diluting the poly-tetramethyl ether glycol with dimethylformamide, and reacting the poly-butylene adipate polyester glycol and the poly-tetramethyl ether glycol for 40-60min at the temperature of 110-120 ℃ under nitrogen according to the preset weight part; secondly, cooling the product obtained in the first step to 75-85 ℃, adding 75-85 ℃ 4,4' -diphenylmethane diisocyanate into the product obtained in the first step according to the predetermined weight part, and reacting for 0.3-0.5h at 75-85 ℃; thirdly, cooling the product obtained in the second step to 45-55 ℃, adding 1, 4-butanediol into the product obtained in the second step according to the predetermined weight part, uniformly mixing, and curing at 85-100 ℃ for 12-24 h.
The invention also aims to provide asphalt compositely modified by the polyurethane modifier and rock asphalt, which comprises the following components in parts by weight:
1-5 parts of polyurethane modifier
5-20 parts of rock asphalt
85-100 parts of matrix asphalt.
The invention also aims to provide a preparation method of the asphalt, which comprises the following steps: firstly, adding a polyurethane modifier into 135-DEG C-145-DEG C matrix asphalt according to a predetermined weight part, and shearing for 0.5-1.5h at the speed of 1500-DEG C3000 r/min; secondly, heating the product obtained in the step I to 140 ℃ and 150 ℃, and shearing for 0.5-1h at 4000 ℃ and 5000 r/min; thirdly, adding the rock asphalt into the product obtained in the second step according to the predetermined weight part, adjusting the temperature to 135-140 ℃, and shearing for 0.3-0.5h at 2000-2500 r/min.
The invention has the beneficial effects that:
the optimal mixing amount of the polyurethane and the rock asphalt under the influence of various factors is determined by performing target optimization on the mixing amount of the polyurethane and the rock asphalt. The method has very important values for solving the damage phenomena of cracking, rutting and the like of the asphalt pavement under the natural environment and the driving load condition, prolonging the service life of the road, improving the integrity, smoothness and water tightness of the asphalt pavement and improving the durability and driving comfort of the asphalt pavement.
The invention can efficiently and rapidly prepare the polyurethane/rock asphalt composite modified asphalt, simplifies the production process, reduces the production energy consumption, can effectively solve the problems of poor interface compatibility of the modifier and the matrix asphalt and the like, and improves the performance of the matrix asphalt.
Drawings
In the drawing of figure 14 of the present invention,
FIG. 1 is a chart of the infrared spectrum of the polyurethane modifier prepared in example 1;
FIG. 2 is a TG plot of the polyurethane modifier prepared in example 1;
FIG. 3 is a DSC plot of the polyurethane modifier prepared in example 1;
FIG. 4 is an infrared spectrum of the polyurethane modifier prepared in example 2;
FIG. 5 is a TG plot of the polyurethane modifier prepared in example 2;
FIG. 6 is a DSC plot of the polyurethane modifier prepared in example 2;
FIG. 7 is a plot of DSR test results for base asphalt versus asphalt prepared in example 3;
FIG. 8 is a graph of the S value results of BBR testing of base asphalt and asphalt prepared in example 3;
FIG. 9 is a graph of the results of the BBR test for base asphalt versus asphalt prepared in example 3;
FIG. 10 is a graph of time-unrecoverable strain at 64 ℃ for a base asphalt versus asphalt prepared in example 3;
FIG. 11 is a plot of DSR test results for base asphalt versus asphalt prepared in example 4;
FIG. 12 is a graph of the S value results of BBR testing of base asphalt and asphalt prepared in example 4;
FIG. 13 is a graph of the results of the BBR test for base asphalt versus asphalt prepared in example 4;
FIG. 14 is a graph of time-unrecoverable strain at 64 ℃ for a base asphalt versus asphalt prepared in example 4.
Detailed Description
The following non-limiting examples are presented to enable those of ordinary skill in the art to more fully understand the present invention and are not intended to limit the invention in any way.
Example 1
A preparation method of a polyurethane modifier comprises the following steps:
when the molecular weight of the poly-tetramethyl ether glycol is less than 2000, reacting X parts of poly-butanediol adipate polyester glycol and X parts of poly-tetramethyl ether glycol in parts by weight under nitrogen at the temperature of 110 ℃ for 40-60min, wherein the flow rate of the nitrogen is 20mL/min, and the stirring speed is 200 rpm;
secondly, cooling the product obtained in the first step to 80 ℃, adding 21.39 parts by weight of 4,4' -diphenylmethane diisocyanate melted at 80 ℃ into the product obtained in the first step, reacting for 0.3-0.5h at 80 ℃, and stirring at 200 rpm;
and thirdly, cooling the product obtained in the second step to 50 ℃, adding 3.67 parts of 1, 4-butanediol into the product obtained in the second step according to the parts by weight, uniformly mixing, curing at 100 ℃ for 24 hours, and stirring at 400 rpm.
Analysis of mechanism
As can be seen from FIG. 1, at 2956cm-1And 2817cm-1Respectively belongs to CH when strong absorption peaks appear2And CH3The stretching vibration; 1722cm-1The occurrence of a strong absorption peak at this position is probably the result of C ═ O stretching vibration in the ester carbonyl group or C ═ O stretching vibration in the amide I bond; 1538cm-1The position is the deformation vibration of N-H in the amide II; 1380cm-1Is in the home CH3The symmetric deformation vibration of (2); 1149 and 1058cm-1Absorption peak of C-O-C in the belonging aliphatic bond; 816 and 712cm-1The absorption peak in the range is-CH bending vibration on the benzene ring. The expected product was prepared in example 1 by infrared spectroscopy.
Subsequently, the molecular weight of the polyurethane modifier was 157362 by gel chromatography, and the content of C element was measured by an element analyzer: 66.880%, content of H element: 3.593%, and the content of N element: 1.711%, and the content of O element: 27.816 percent.
The measured value of the hard segment content calculated by elemental analysis is substituted into formula I:
m in formula Ins2000, the relative molecular mass of the monomer is 262, and n is calculated to be 8; when Ch 19.31 is calculated, Mnh 478.62 and the relative molecular mass of the hard segment is 340, then the measured number-average relative molecular mass value of m 3 binding can be calculated, and therefore it can be concluded that the polyurethane modifier prepared in example 1 has the following possible structural formula ii:
thermal performance
As can be seen from FIGS. 2 to 3, T of the polyurethane modifier prepared in example 15%And T10%328.1 ℃ and 336.2 ℃ respectively, and a glass transition temperature TgIt was-47.92 ℃.
Mechanical property detection
The mechanical property test results of the polyurethane modifier prepared in example 1 are shown in table 1:
TABLE 1
Example 2
A preparation method of a polyurethane modifier comprises the following steps:
when the molecular weight of the poly-tetramethyl ether glycol is more than or equal to 2000, using dimethylformamide to prepare a mixture of the poly-tetramethyl ether glycol and the dimethylformamide according to a molar ratio of 1: 30, diluting the polytetramethylene ether glycol, and reacting X parts of polybutylene adipate polyester glycol and X parts of polytetramethylene ether glycol under nitrogen at the flow rate of 20mL/min at the temperature of 110 ℃ for 40-60min at the stirring speed of 200 rpm;
secondly, cooling the product obtained in the first step to 80 ℃, adding X parts of 4,4' -diphenylmethane diisocyanate at 80 ℃ into the product obtained in the first step according to the parts by weight, reacting for 0.3-0.5h at 80 ℃, and stirring at 200 rpm;
and thirdly, cooling the product obtained in the second step to 50 ℃, adding X parts of 1, 4-butanediol into the product obtained in the second step according to the parts by weight, uniformly mixing, curing at 100 ℃ for 24 hours, and stirring at 400 rpm.
Analysis of mechanism
As can be seen from FIG. 4, at 2948cm-1And 2853cm-1The strong absorption peak is respectively represented by-CH2and-CH 3; 1728cm-1The absorption peak appears at 1700cm when the stretching vibration of C ═ O in the home ester carbonyl group or the stretching vibration of C ═ O in the amide I bond is larger than 20 percent-1A new peak appears when C is equal to O in the attributive isocyanurate trimer (another 1408--1Where the peak also belongs to the isocyanurate trimer); 1520 and 1560cm-1The point is deformation vibration of N-H in the amide II; 1227 + 1233cm-1The absorption peak is deformation vibration of-OH; 1060-1150cm-1The absorption peak of C-O-C in the aliphatic bond is at 1110-1080cm-1The peak appearing in the range acts as the stretching vibration of C-O in the home ether group; and 816 and 712cm-1The peaks in the range are all bending vibrations of-CH on the benzene ring.
Subsequently, the molecular weight of the polyurethane modifier was 157362 by gel chromatography, and the content of C element was measured by an element analyzer: 66.88 percent, and the content of H element: 3.593%, and the content of N element: 1.711%, and the content of O element: 27.816 percent.
The measured value of the hard segment content calculated by elemental analysis is substituted into formula III:
m in the formula III ns20000, the relative molecular mass of the monomer is 90, and n 22 can be obtained through calculation; calculated as ChWhen equal to 21.39, Mnh478.62, the relative molecular mass of the hard segment chain is 340, and the measured number-average relative molecular mass value of m-4 binding can be calculated, thus concluding that the possible structural formula of the polyurethane modifier prepared in example 2 is as shown in formula IV:
thermal performance
As can be seen from FIGS. 5-6, T of the polyurethane modifier prepared in example 25%And T10%324.7 ℃ and 340.7 ℃ respectively, and a glass transition temperature TgIt was-52.6 ℃.
Mechanical property detection
The mechanical property test results of the polyurethane modifier prepared in example 2 are shown in table 2:
TABLE 2
Example 3
A preparation method of asphalt compositely modified by polyurethane modifier and rock asphalt comprises the following steps:
adding 5 parts by weight of the polyurethane modifier prepared in example 1 into 100 parts by weight of matrix asphalt at 135 ℃, and shearing at 2000r/min for 0.5 h;
secondly, heating the product obtained in the first step to 140 ℃, and shearing for 1h at 5000 r/min;
thirdly, adding 15 parts of rock asphalt into the product obtained in the second step by weight, adjusting the temperature to 135-140 ℃ and shearing for 0.5h at 2500 r/min.
High temperature rheology
The high-temperature rheological properties of the matrix asphalt and the polyurethane/rock asphalt composite modified asphalt are shown in fig. 7, and the comparison shows that the high-temperature rheological property of the polyurethane/rock asphalt composite modified asphalt is obviously superior to that of the matrix asphalt.
Low temperature rheology
The high-temperature rheological properties of the matrix asphalt and the polyurethane/rock asphalt composite modified asphalt are shown in figures 8-9, and the comparison shows that the low-temperature rheological property of the polyurethane/rock asphalt composite modified asphalt is obviously superior to that of the matrix asphalt.
Multi stress creep test
The PU composite modified asphalt multi-stress creep test is carried out by adopting DSR. The test strictly conforms to the test standard of AASHTOMP19-10 (2013). The test conditions were: under the stress-recovery mode of DSR, the PU composite modified asphalt sample (aged by RTFOT for a short time) is loaded for 1s and then unloaded for 9s, and the temperature of the whole test is controlled to be constant at 64 ℃. During the test, the sample was first stressed at 1.0kPa, the cycle was repeated 10 times, the stress was then increased to 3.2kPa, and the cycle was continued 10 times, and finally the strain recovery ratio (R) and the unrecoverable creep compliance (Jnr) were measured, and the results are shown in FIG. 10 and Table 3.
TABLE 3
As can be seen from fig. 10 and table 3, the polyurethane/rock asphalt composite has an improved resistance to permanent deformation of the asphalt. The R and the Jnr are obtained through test measurement and calculation, and the strain recovery rate of the composite modified asphalt is obviously improved compared with that of the matrix asphalt, and meanwhile, the polyurethane/rock asphalt composite modified asphalt has more excellent permanent deformation resistance compared with the matrix asphalt.
Example 4
A preparation method of asphalt compositely modified by polyurethane modifier and rock asphalt comprises the following steps:
adding 5 parts by weight of the polyurethane modifier prepared in the example 2 into 100 parts by weight of matrix leaching at 140 ℃, and shearing at 2000r/min for 0.5 h;
secondly, heating the product obtained in the first step to 145 ℃, and shearing for 1h at 5000 r/min;
thirdly, adding 10 parts of rock asphalt into the product obtained in the second step by weight, adjusting the temperature to 140 ℃, and shearing for 0.5h at 2500 r/min.
High temperature rheology
The high-temperature rheological properties of the matrix asphalt and the polyurethane/rock asphalt composite modified asphalt are shown in fig. 11, and the comparison shows that the high-temperature rheological properties of the polyurethane/rock asphalt composite modified asphalt are obviously superior to those of the matrix asphalt.
Low temperature rheology
The high-temperature rheological properties of the matrix asphalt and the polyurethane/rock asphalt composite modified asphalt are shown in figures 12-13, and the comparison shows that the low-temperature rheological property of the polyurethane/rock asphalt composite modified asphalt is obviously superior to that of the matrix asphalt.
Multi stress creep test
The PU composite modified asphalt multi-stress creep test is carried out by adopting DSR. The test strictly conforms to the test standard of AASHTOMP19-10 (2013). The test conditions were: under the stress-recovery mode of DSR, the PU composite modified asphalt sample (aged by RTFOT for a short time) is loaded for 1s and then unloaded for 9s, and the temperature of the whole test is controlled to be constant at 64 ℃. During the test, the sample was first stressed at 1.0kPa, the cycle was repeated 10 times, the stress was then raised to 3.2kPa, and the cycle was continued 10 times, and finally the strain recovery ratio (R) and the unrecoverable creep compliance (Jnr) were measured, and the results are shown in FIG. 14 and Table 4.
TABLE 4
As can be seen from the combination of fig. 14 and table 4, the polyurethane/rock asphalt composite has an improved resistance to permanent deformation of the asphalt. The R and the Jnr are obtained through test measurement and calculation, and the strain recovery rate of the composite modified asphalt is obviously improved compared with that of the matrix asphalt, and meanwhile, the polyurethane/rock asphalt composite modified asphalt has more excellent permanent deformation resistance compared with the matrix asphalt.
Claims (6)
3. a process for producing the polyurethane modifier according to claim 1 or 2, characterized in that: the preparation method comprises the following steps:
firstly, when the molecular weight of the poly-tetramethyl ether glycol is less than 2000, reacting the poly-butanediol adipate polyester glycol and the poly-tetramethyl ether glycol for 40-60min at the temperature of 110-120 ℃ under nitrogen according to the preset weight part;
secondly, cooling the product obtained in the first step to 75-85 ℃, adding 75-85 ℃ 4,4' -diphenylmethane diisocyanate into the product obtained in the first step according to the predetermined weight part, and reacting for 0.3-0.5h at 75-85 ℃;
thirdly, cooling the product obtained in the second step to 45-55 ℃, adding 1, 4-butanediol into the product obtained in the second step according to the predetermined weight part, uniformly mixing, and curing at 85-100 ℃ for 12-24 h.
4. A process for producing the polyurethane modifier according to claim 1 or 2, characterized in that: the preparation method comprises the following steps:
firstly, when the molecular weight of the poly-tetramethyl ether glycol is more than or equal to 2000, diluting the poly-tetramethyl ether glycol with dimethylformamide, and reacting the poly-butylene adipate polyester glycol and the poly-tetramethyl ether glycol for 40-60min at the temperature of 110-120 ℃ under nitrogen according to the preset weight part;
secondly, cooling the product obtained in the first step to 75-85 ℃, adding 75-85 ℃ 4,4' -diphenylmethane diisocyanate into the product obtained in the first step according to the predetermined weight part, and reacting for 0.3-0.5h at 75-85 ℃;
thirdly, cooling the product obtained in the second step to 45-55 ℃, adding 1, 4-butanediol into the product obtained in the second step according to the predetermined weight part, uniformly mixing, and curing at 85-100 ℃ for 12-24 h.
5. An asphalt modified by compounding the polyurethane modifier according to claim 1 or 2 with rock asphalt, wherein: the asphalt comprises the following components in parts by weight:
1-5 parts of polyurethane modifier
5-20 parts of rock asphalt
85-100 parts of matrix asphalt.
6. A process for producing asphalt according to claim 5, characterized in that: the preparation method comprises the following steps:
firstly, adding a polyurethane modifier into 135-DEG C-145-DEG C matrix asphalt according to a predetermined weight part, and shearing for 0.5-1.5h at the speed of 1500-DEG C3000 r/min;
secondly, heating the product obtained in the step I to 140 ℃ and 150 ℃, and shearing for 0.5-1h at 4000 ℃ and 5000 r/min;
thirdly, adding the rock asphalt into the product obtained in the second step according to the predetermined weight part, adjusting the temperature to 135-140 ℃, and shearing for 0.3-0.5h at 2000-2500 r/min.
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