C. HE et al.: EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE 661–667 EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE UPORABA VEZIVA NA OSNOVI EPOKSI SMOLE ZA ZAPOLNJEVANJE LUKENJ PRI VZDR@EVANJU PLO^NIKOV Chengping He 1 , Zhigang Wu 2 , Yu Huang 2 , Jiangang Yang *3 , Cong Liang 3 , Guanfa Zhang 3 1 Fujian Expressway Road and Bridge Construction Development Co., Ltd, Fuzhou, China 2 Fujian Province Expressway Maintenance Engineering Co., Ltd, Fuzhou, China 3 School of Civil Engineering and Architecture, East China Jiaotong University, Nanchang, China Prejem rokopisa – received: 2022-06-14; sprejem za objavo – accepted for publication: 2022-10-24 doi:10.17222/mit.2022.531 Aiming at the problems of asphalt pavement crack sealing and pothole repair materials, an epoxy-resin adhesive with high form- ing strength, good toughness and room-temperature curing was prepared. In addition to being used as a road filling sealant, the adhesive can also be used for preparing a cold patching mixture for pits. The properties of the epoxy-resin adhesive, the con- struction performance and road performance of the pouring sealant and cold patch were studied. The results showed that the early strength of the epoxy-resin adhesive was fast and high, the curing volume shrinkage was small, the low-temperature char- acteristics and tensile properties were good, and the toughness was excellent. As a pouring sealant, the epoxy-resin adhesive had excellent low-temperature bending resistance. The cold patching mixture based on the adhesive exhibited strong cohesiveness, good low-temperature crack resistance, and excellent high-temperature stability and water stability. This adhesive expands the application of epoxy resin in repairing cracks and pits of asphalt pavements, and is of great significance in promoting the devel- opment of the asphalt pavement maintenance technology. Keywords: pavement, epoxy resin, adhesive, construction V ~lanku je opisana priprava in lastnosti veziva na osnovi epoksidne smole za re{evanje problema tesnenja razpok in krpanja lukenj na asfaltiranih plo~nikih. Avtorji so pripravili vezivo z veliko trdnostjo, dobro `ilavostjo po oblikovanju in utrjevanju pri sobni temperaturi, ki ni uporabno samo kot polnilno tesnilo temve~ se lahko uporabi tudi kot hladna me{anica za krpanje jamic oziroma lukenj. Preu~evali so lastnosti izdelane epoksidne smole in njeno odpornost na obremenitve. Rezultati so pokazali, da se epoksidna smola hitro strdi in `e zelo hitro ima dobro trdnost ter tudi majhen skr~ek pri nizkih temperaturah. Izdelan material ima dobre natezne lastnosti in odli~no `ilavost ter kot polnilo odli~no odpornost proti upogibanju pri nizkih temperaturah. Hladna me{anica za krpanje razpok in lukenj ima tudi mo~no kohezivnost, odli~no visokotemperaturno stabilnost in vodoodpornost. Avtorji so poudarili, da razvito epoksidno vezivo {iri uporabnost epoksi smol tudi na podro~je gradbeni{tva oziroma na podro~je razvoja tehnologije vzdr`evanja asfaltiranih plo~nikov. Klju~ne besede: vzdr`evanje plo~nikov, epoksidna smola, vezivo, gradbeni{tvo 1 INTRODUCTION Asphalt is a temperature-sensitive material, which is brittle in winter and soft in summer. Under long-term im- pacts of the traffic load and natural environment, rutting disease is prone to occur in summer, and cracks, loose- ness, pits, and other diseases are prone to occur in win- ter. 1–3 If these cracks and pits are not repaired in time, the disease will further expand under the combined effect of heavy traffic and water, affecting driving comfort and road service life, 4 and seriously endangering driving safety. Therefore, the challenges of how to quickly and efficiently seal cracks and repair pits have become a long-term concern of an increasing number of research- ers. As crack sealing materials, we mainly use hot asphalt sealants, normal temperature asphalt sealants 5,6 and chemical sealants. 7,8 Hot asphalt sealants are prone to bond failure at high temperatures 9,10 and brittle fracture at low temperatures. 11 The aging performance of room- temperature asphalt sealants is poor. 5,12 The chemical sealant has a stable performance and it still has good per- formance after aging. Epoxy resin exhibits strong adhesion after curing and is widely used as an adhesive. Thermosetting epoxy resin has excellent chemical resistance and high bond strength. 13,14 The chemical crosslinking reaction product of a curing agent and epoxy resin shows good cohesion, which can significantly improve the high-temperature strength and deformation resistance of the adhesive. 15 There are many types of epoxy resins and curing agents. Through a reasonable material selection and formula de- sign, polymer materials meeting the requirements of dif- ferent conditions can be prepared. 16,17 Wang et al. 18 pre- pared super-viscosity epoxy grouting, and their results show that super-low-viscosity epoxy grouting materials can be used to repair microcracks in construction. Modesti et al. 19 found that an epoxy resin sealant can ef- Materiali in tehnologije / Materials and technology 56 (2022) 6, 661–667 661 UDK 678.686:693.78 ISSN 1580-2949 Original scientific article/Izvirni znanstveni ~lanek MTAEC9, 56(6)661(2022) *Corresponding author's e-mail: 2851@ecjtu.edu.cn (Jiangang Yang) fectively restore the overall mechanical properties of concrete. Liu et al. 20 prepared a new epoxy polymer- modified-asphalt cold patching mixture, and found that the cold patching mixture has a good repair effect in winter and rainy seasons. Pedram et al. 21 found that a mixture with a high epoxy-resin content exhibits excel- lent mechanical properties and durability. Therefore, ep- oxy resin is an ideal pavement-crack filling and pot- hole-repair material. In this paper, an epoxy-resin adhesive with high strength, good toughness and normal temperature curing was developed. The adhesive can not only be used as a road filling sealant but can also be used to prepare a cold patching mixture for pits. The properties of the adhesive were examined with viscosity and curing degree tests, and the bonding performance of the sealant repair struc- ture was studied with a low-temperature beam bending test. The construction and road performance of the cold patch were studied using construction workability, high-temperature rutting, low-temperature bending and freeze-thaw splitting tests. 2 EXPERIMENTAL PART 2.1 Materials 2.1.1 Epoxy-resin adhesive In this paper, bisphenol A type E-44 epoxy resin was selected as the epoxy-resin material. DMP-3-800LC poly mercaptan was selected as the curing agent. Active dilu- ent butanediol diglycidyl was selected as the diluent. Polyurethane prepolymer was selected as the toughening agent. Tertiary amine accelerator DMP30 was selected as the accelerator. The epoxy-resin adhesive was mixed at normal temperature. The mass proportions of (E-44 ep- oxy resin : curing agent : diluent : toughening agent : ac- celerator) were (100 : 55 : 50 : 20 : 3). 2.1.2 Aggregate and filler The coarse aggregate used in the test was limestone gravel, the fine aggregate was manufactured sand, and the filler was limestone powder without agglomerations, clean and dry after grinding. The aggregates and mineral powder all met the requirements of JTG F40-2004. 2.1.3 Mineral gradation This study was based on the AC-10 grading design; the grading curve is shown in Figure 1. 2.2 Methods 2.2.1 Mixing process of the cold patching mixture The main preparation steps were as follows. Firstly, the adhesive was prepared in the above proportions. Then the coarse aggregate was placed in a mixing pot and mixed with the prepared adhesive at room tempera- ture for 180 s so that the binder fully covered the aggre- gate surface. Finally, the fine aggregate was poured into the mixing pot and stirred for 300 s to obtain an ep- oxy-resin cold patching mixture for trench repair. The content of the adhesive was 2 %. Their stirring was done at 360 min –1 and the temperature was 25 °C. 2.2.2 Viscosity test The viscosity-test reference standard was T 2794-2013. The equipment included a dV-II + Pro rotary viscometer produced by Brook Company from the United States, and the test temperature was 25 °C. 2.2.3 Curing degree and curing volume shrinkage test The extraction method (T 2576-2016) was used to determine the curing degree of the adhesive. For the cur- ing volume shrinkage test, we first used a disposable sy- ringe to slowly and evenly inject the adhesive into a 5 mL small glass measuring cylinder. After curing at 25 °C for 7 d, the adhesive was placed in a 60 °C oven for 1 h. When it was cooled to room temperature, volume V of the adhesive cured in the measuring cylinder was re- corded. The curing-shrinkage formula is shown in Equa- tion (1). = − × 5 5 100 V % (1) 2.2.4 Glass transition temperature test A 200 F3 differential scanning calorimeter produced by Niche Company from Germany was used in the ex- periment. Firstly, the furnace temperature was raised to 60 °C at the rate was 10 °C/min. Then, the furnace tem- perature was cooled from 60 °C to –60 °C at the same rate for 3 min. Finally, the furnace temperature was raised from –60 °C to 60 °C at the rate of 10 °C/min. The sample weight was about 5–10 mg. The inflection point of the curve data during the second heating process was selected as the glass transition temperature T g . 2.2.5 Tensile strength and elongation at break test A tensile specimen was prepared according to the test method of T 2567-2008. After curing at 25 °C for 7 d, the prepared dumbbell-shaped tensile sealant specimen C. HE et al.: EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE 662 Materiali in tehnologije / Materials and technology 56 (2022) 6, 661–667 Figure 1: Mineral gradation curves was placed in an oven at 60 °C for 1 h and then tested with the CMT5105 universal test. The test temperature was –10 °C and the tensile rate was 10 mm/min. 2.2.6 High-temperature rutting test According to the rutting test method of T 0719-2011, a rutting plate specimen was formed, and its dimensions were (300 × 300 × 50) mm. The specimen was cured in a 25 °C environment box for 28 d. The test temperature was 60 °C, the wheel pressure was 0.7 MPa; the rutting deformation data were recorded for 45 min and 60 min. 2.2.7 Low-temperature beam bending test According to the test specification of the T 0715-2011 low-temperature bending-test method, a rutting plate specimen was formed and kept in the 25 °C environment box for 28 d. After that, the rut plate was cut into a prism beam specimen, with dimensions of (250 ×30 × 35) mm; it was placed in a freezing solution with a constant tem- perature of –The test temperature was –10 °C and the loading rate was 50 mm/min. 2.2.8 Marshall immersion test According to the test specification of the T 0709-2011 Marshall immersion stability test, the epoxy-resin adhe- sive cold patching mixture was double sidedly com- pacted 75 times to form Marshall specimens with a di- ameter of 101.6 mm and height of 63.5 mm. The specimens were cured in the 25 °C environment box for 28 d. After curing, the bulk density and porosity parame- ters of the Marshall specimens were tested, and the Mar- shall stability was tested after two groups of specimens were placed in a flume with a constant temperature of 60 °C for 30 min and 48 h. 2.2.9 Freeze-thaw splitting test According to the test procedure of the T 0729-2011 freeze-thaw splitting test, the specimens were cured in the 25 °C environment box for 28 d. After curing, the first group of specimens was kept at room temperature; the second group of specimens was placed in a plastic bag after vacuum saturation, and 10 mL of water was added to the specimens; then the bag was placed into a refrigerator at a constant temperature of –18 °C for 16 h. After taking out the specimens, they were removed from the plastic bag and placed into a water tank with a con- stant temperature of 60 °C. After a dwell time of 24 h, the specimens were taken out and both groups of speci- mens were placed in a water tank with a constant tem- perature of 25 °C for 2 h. The splitting rate was 50 mm/min. 3 RESULTS AND DISCUSSION 3.1 Epoxy resin adhesive properties 3.1.1 Viscosity According to the requirements of T 1041-2007, the operation time of a sealant should be more than 30 min. In the actual construction process, the permeability of the adhesive was closely related to the viscosity. The vis- cosity was in a reasonable range of 1000–2000 mPa·s, which did not affect the permeability of the cracks. Therefore, the period from the initial adhesive viscosity to 2000 mPa·s was defined as the operable time in this paper. Considering that the adhesive was produced at room temperature, the viscosity test temperature was 25 °C; the viscosity of the adhesive changed as shown in Figure 2. Figure 2 shows that the initial viscosity of the adhe- sive is not more than 2000 mPa·s as it remains in a rea- sonable range of 1000–2000 mPa·s, indicating that the adhesive has good perfusion for asphalt pavement cracks. The viscosity of the adhesive increases with the curing time, and the viscosity increases rapidly after about 2 h, indicating that the adhesive can reach the gel state earlier and form the initial strength in the construc- tion process. In addition, the viscosity of the adhesive exceeds 2000 mPa·s at 53.1 min, meeting the require- ment of the operating time exceeding 30 min, so the ad- hesive has good pour viscosity. 3.1.2 Curing degree and curing volume shrinkage In this part, the curing degree and curing volume shrinkage of the adhesive were tested at 25 °C. The test samples were tensile specimens formed by curing. The test results are shown in Table 1. Table 1: Test results for the curing degree and volume shrinkage of the adhesive Degree of cure (%) Volume shrinkage (%) 95.19 1.6 When the curing degree is greater than 95 %, it can be considered that the epoxy resin is completely cured, indicating that the adhesive has been completely cured and the cured product has good aging resistance and C. HE et al.: EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE Materiali in tehnologije / Materials and technology 56 (2022) 6, 661–667 663 Figure 2: Change in the adhesive viscosity with time long-term performance. The volume shrinkage of the ad- hesive was within 2 %, indicating that the internal stress generated by the adhesive in the curing process was small, having little effect on the tensile properties and adhesion properties of the cured adhesive. 3.1.3 Glass transition temperature When using the low-temperature evaluation method of polymer materials, glass transition temperature T g is also commonly used to characterize the low-temperature performance of materials. Amorphous polymer materials undergo three different states: from low temperature to high temperature, from the glass state to the glass-rubber state, and then to the rubber state. When an adhesive is below the glass transition temperature, it is prone to brit- tle fracture under load. The glass transition temperature of our adhesive was tested with differential scanning cal- orimetry (DSC) to evaluate the low-temperature charac- teristics of the adhesive. The test result shows that the glass transition temper- ature of the adhesive was –18.1 °C, meeting the require- ments of the rubber state at low temperatures in winter. 3.1.4 Tensility An adhesive must have a certain tensile strength to sustain the expansion and shrinkage trend of cracks with temperature changes. Due to a decrease in the nighttime temperature or sudden drop in the temperature, the adhe- sive may also be subjected to the tensile stress caused by crack expansion. Therefore, the test curing temperature was 25 °C, and the measurement temperature was –10 °C. The tensile properties of the adhesive were tested during the molding process at room temperature. The results are shown in Figure 3. As shown in Figure 3, at the beginning of curing, the growth rate of the tensile strength of the adhesive was very obvious. Especially, the growth rate was the fastest in the first three days, reaching 3.69 MPa on the 3 rd day. After 15 d of curing, the tensile strength increased slowly, reaching 5.83 MPa on the 28 th day, and the over- all tensile strength was large. At the beginning of the re- action, the elongation at the break of the adhesive gradu- ally increased with the extension of the reaction time; ba- sically, within 1–2 days, the elongation at break reached a maximum of 133.12 %. As the reaction continued, the elongation at break decreased gradually with the exten- sion of the curing time, having a good negative correla- tion with the tensile strength. However, the overall elon- gation at break was higher than 121 %, exhibiting an excellent tensile deformation ability. In summary, the ad- hesive has good tensile properties. 3.2 Bending bonding properties of the adhesive for fill- ing seams In order to study the flexural-tensile adhesion perfor- mance of the adhesive and the crack wall-filling repair structure, an AC-13 graded asphalt mixture was used to prepare beam specimens for a low-temperature bending test. After bending fracture, the beam was separated from a 5-mm spacing, sealed with the adhesive on three sides, and poured with the adhesive on the unsealed sur- face. After molding at 25 °C for 7 d, it was placed in a 60 °C oven for 1 h. The repaired beams were tested un- der low-temperature bending. The results are shown in Table 2. Table 2: Results for the flexural strength Strength index Specimen types Value Flexural-tensile strength (MPa) Undamaged speci- men 10.36 Bending bond strength (MPa) Damage repair speci- men 8.63 Bending tensile-strength ratio (%) 83.3 It can be seen from Table 2 that the flexural-tensile bond strength of the beam repaired with the adhesive re- covered 83.3 % of the flexural-tensile bond strength of the undamaged specimen; its recovery degree is high, in- dicating that the low-temperature flexural-tensile resis- tance of the adhesive and the crack wall-filling repair structure is strong. 3.3 Cold patching mixture performance of the ep- oxy-resin adhesive 3.3.1 Cohesiveness Following the JTG F40-2004 rolling sieve cohesion test method, 800 g of a cold patching mixture, uniformly mixed at room temperature, was put into a Marshall test model and placed into a (0, 10, 20 and 30) °C environ- ment box for 4 h, respectively. After taking it out, both sides were compacted five times and demolded. After that the specimen was put into a standard sieve, stood up and rolled back 20 times. The damage rate of the speci- men was determined. The test results are shown in Ta- ble 3. C. HE et al.: EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE 664 Materiali in tehnologije / Materials and technology 56 (2022) 6, 661–667 Figure 3: Formation of the adhesive tensile strength Table 3: Rolling sieve test results Temperature (°C) 01 02 03 0 Failure rate (%) 6.53 4.79 5.43 4.52 Normative value (%) 40 It can be seen from Table 3 that the damage rate of the specimen at each temperature is less than 10 %, which is much lower than the standard value. It can be seen that the cold patching mixture has good cohesive- ness, and particles can be bonded to each other as a whole through the adhesive without falling off. 3.3.2 Construction workability In this study, an improved empirical method was used to evaluate the workability of the epoxy-based cold patching mixture. The test used temperatures of (0, 10, 20 and 30) °C to study the construction workability of the cold filling mixture at different temperatures. 500 g of the cold patch mixture of was weighed and mixed evenly at room temperature. The mixture was loaded into plastic bags and placed in environmental boxes at (0, 10, 20 and 30) °C for 4 h. After 4-h storage at each tempera- ture, the cold patching mixture could be kneaded into clusters; the higher the temperature, the better was the clustering effect, indicating that the cold patch had good compactness. The agglomerated mixture could be easily patted and dispersed by beating it with a wooden stick; basically, it had no large aggregate and good porosity. The lower the temperature after the mixture was agglom- erated, the better it could be dispersed into blocks in a short time without any external force. The block mixture could be patted and dispersed. The test shows that when the temperature is low, the porosity of the cold patching mixture is better; when the temperature is high, the com- pressibility of the cold patching mixture is better. 3.4 Road performance of the cold patching mixture 3.4.1 High-temperature stability The pavement temperature is high in summer, and the asphalt pavement is deformed under the repeated actions of temperature and load. If deformation continues to ac- cumulate, it will cause rutting, congestion and other dis- eases, affecting the traffic safety and reducing the com- fort and road service performance. Therefore, it was necessary to test the high-temperature stability of the cold patching mixture. The test results are shown in Ta- ble 4. Table 4: Rutting test results for the pavement cold patch mixture 45-min de- flection (mm) 60-min de- flection (mm) Dynamic stability (times/mm) Specification require- ment (times/mm) Common asphalt mixture Modified SMA mixture 0.209 0.223 83200 1000 3000 It can be seen from Table 4 that the dynamic stability of the cold patching mixture reaches 83200 times/mm, which is much higher than the requirement for the dy- namic stability of the modified SMA mixture, which is not less than 3000 times/mm as specified in the Techni- cal Specification for Highway Asphalt Pavement Con- struction (JTG F40-2004). Therefore, the high-tempera- ture stability of the epoxy-resin cold patching mixture is good. 3.4.2 Low-temperature crack resistance Transverse cracks of asphalt pavement are mostly caused by low-temperature cracking of asphalt. There- fore, pavement cold patching materials must have low-temperature crack resistance to ensure that a re- paired pavement has a certain deformation resistance to avoid low-temperature shrinkage cracks. To study the low-temperature crack resistance of cold patching pre- pared with the epoxy-resin adhesive, a low-temperature bending test was used to evaluate its low-temperature performance provided by the bending tensile strength and bending tensile strain. The test results are shown in Table 5. Table 5: Low-temperature bending test results Failure load (kN) Mid-span deflection (mm) Flexural- tensile strength (MPa) Flexural- ten- sile strain Stiffness modulus (MPa) 2524 0.487 20.32 2876 × 10 –6 7598 It can be seen from Table 5 that the bending strain was2876×10 –6 , meeting the requirements of the Tech- nical Specification for Highway Asphalt Pavement Con- struction (JTG F40-2004), stipulating that the bending strain of an ordinary asphalt mixture in a cold winter re- gion should not be less than 2600 × 10 –6 . The above re- sults indicate that the epoxy-resin pavement cold patch- ing mixture is suitable for most regions. 3.4.3 Water stability of the cold water feed The stability of the cold water feed was evaluated with the Marshall Immersion test and freeze-thaw split- ting test. The results of the Marshall Immersion test are shown in Table 6, and the results of the freeze-thaw splitting test are shown in Table 7. Table 6: Volume indicators and Marshall Immersion results Bulk density (g/cm 3 ) Percent- age of void (%) MS (kN) MS1 (kN) MS 0 (%) Norma- tive value (%) 2.455 1.387 100.43 95.78 95.37 80 In Table 6, MS is the Marshall stability of the speci- men immersed for 30 min, MS 1 is the Marshall stability of the specimen immersed for 48 h, and MS 0 is the resid- ual stability of immersion. C. HE et al.: EPOXY-RESIN ADHESIVE FOR SEAM FILLING AND POTHOLE REPAIR IN PAVEMENT MAINTENANCE Materiali in tehnologije / Materials and technology 56 (2022) 6, 661–667 665 It can be seen from Table 6 that Marshall-stability values before and after the immersion are large, and the residual stability of the specimen immersed is more than 95 %, meeting the requirements of the Technical Specifi- cation for Highway Asphalt Pavement Construction (JTG F40-2004), stipulating that the residual stability of an ordinary asphalt mixture in a wet area should not be less than 80 %. The above results indicate that the cold patching mixture prepared with the adhesive has excel- lent water stability. Table 7: Freeze-thaw splitting test results R T1 (MPa) R T2 (MPa) TSR (%) Specification re- quirement (%) 3.617 3.359 92.87 75 In Table 7, R T1 is the splitting strength of the first group of specimens, R T2 is the splitting strength of the second group of specimens, and TSR is the freeze-thaw splitting strength ratio. Table 7 shows that the splitting strength ratio of the cold patch is above 90 %, and according to the Technical Specification for Highway Asphalt Pavement Construc- tion (JTG F40-2004), the splitting strength ratio of an or- dinary asphalt mixture in semi-arid areas should not be less than 75 %. It can be seen that the water stability of the pavement cold patching mixture used in this study is significantly higher than that of the ordinary asphalt mix- ture. In summary, the epoxy pavement cold patching mixture has high water stability. 4 CONCLUSIONS In this paper, an epoxy-resin adhesive that can be used for pavement crack filling and pothole repair was prepared. The properties of the adhesive and cold patch- ing mixture, and their road performance were studied us- ing physical-property, construction-performance and road-performance tests. The main results are as follows: 1) With regard to viscosity, the epoxy-resin adhesive exhibits good perfusion, allowing fast early strength for- mation and high strength, small curing volume shrink- age, good low-temperature properties and tensile proper- ties, and excellent toughness. 2) As a filling sealant, the epoxy-resin adhesive has excellent low-temperature flexural-tensile strength, and the flexural-tensile bond strength of the beam repaired with this adhesive is restored to 83.3 % of the strength of the undamaged specimen. 3) The epoxy-resin cold patching mixture shows good cohesiveness in the test temperature range, and it still has good porosity and compactness after 4-h storage at each temperature. The high temperature performance of the cold patching mixture is significantly higher than that of the asphalt mixture, and its dynamic stability reaches 83200 times/mm. The bending strain at –10 °C meets the requirements for the asphalt mixture in a se- vere cold region. 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