High-heat-resistance high-viscosity asphalt as well as preparation method and application thereof
By combining high heat-resistant epoxy monomers, crosslinking agents, and modifiers, a crosslinked three-dimensional comb polymer was prepared, which solved the problems of low-temperature flexibility and high-temperature stability of high-viscosity asphalt in areas with large diurnal temperature differences, improved the viscosity, toughness, and storage stability of asphalt, and is suitable for road construction.
Patent Information
- Application Number
- CN202511633789.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-11-10
- Publication Date
- 2026-02-06
AI Technical Summary
Existing high-viscosity asphalt is difficult to maintain both low-temperature flexibility and high-temperature stability in areas with large diurnal temperature differences, and its adhesion and waterproofing properties are insufficient, affecting road performance and lifespan.
A cross-linked three-dimensional comb polymer is formed by combining high heat-resistant epoxy monomers, cross-linking agents, reactive modifiers, and high viscosity modifiers through a specific preparation method, which enhances the viscosity, toughness, and storage stability of asphalt.
It improves the low-temperature flexibility, shear strength, impact resistance, and adhesion of asphalt, ensuring good performance and stability in areas with large diurnal temperature variations.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of asphalt modification technology, specifically to a high heat-resistant, high-viscosity asphalt, its preparation method, and its application. Background Technology
[0002] my country experiences significant climatic variations, with the Northwest region characterized by large diurnal temperature ranges. Due to these large temperature differences, asphalt needs to maintain a certain level of flexibility at low temperatures to prevent embrittlement or cracking, while simultaneously maintaining stability at high temperatures to avoid softening and deformation. However, research on high-viscosity asphalt suitable for regions with large diurnal temperature variations is limited, and multiple factors need to be considered, including temperature resistance, viscosity stability, adhesion, and waterproofing. Only by comprehensively considering these factors can a high-viscosity asphalt suitable for local climatic and road conditions be selected to ensure good pavement performance and extended service life. This invention provides a high-heat-resistant, high-viscosity asphalt for regions with large diurnal temperature variations to ensure optimal performance under specific climatic and environmental conditions. Summary of the Invention
[0003] To address the technical problems in existing technologies, the present invention aims to provide a high-heat-resistant, high-viscosity asphalt, its preparation method, and its applications. This invention modifies the asphalt, effectively improving its high and low temperature stability, resulting in excellent viscosity and toughness, and good storage stability.
[0004] To achieve the above objectives, the technical solution provided by the present invention is as follows: A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 87-95 parts of base asphalt, 15-30 parts of high-heat-resistant epoxy monomer, 1-10 parts of crosslinking agent, 5-20 parts of reactive modifier, and 35-65 parts of high-viscosity modifier. It should be noted that other additives may be appropriately added depending on the specific application environment. Preferably, the base asphalt is No. 90 base asphalt.
[0005] Preferably, a high heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of base asphalt, 19-29 parts of high heat-resistant epoxy monomer, 3-5 parts of crosslinking agent, 15-19 parts of reactive modifier, and 50-59 parts of high-viscosity modifier.
[0006] As described above, the high-heat-resistant, high-viscosity asphalt comprises a high-heat-resistant epoxy monomer that is one or a mixture of α-naphthyl glycidyl ether, triphenylmethyl glycidyl ether, 2-biphenyl glycidyl ether, and poly[(phenyl glycidyl ether)-co-formaldehyde]. Preferably, the high-heat-resistant epoxy monomer is poly[(phenyl glycidyl ether)-co-formaldehyde]. The high-heat-resistant epoxy monomer has a structure of biphenyl, naphthalene, triphenylmethane, and polyphenylformaldehyde dehydrated glycerol ether, which have high thermal stability and high glass transition temperature and melting point. The epoxy groups react with a crosslinking agent to form side chain end groups of a comb-shaped polymer.
[0007] The high heat-resistant, high-viscosity asphalt described above uses citrulline-malic acid as the crosslinking agent.
[0008] The high heat-resistant, high-viscosity asphalt described above uses a reactive modifier called LOTADER. ® AX8750 or LOTADER ® AX8750T. LOTADER® AX8750 and LOTADER® AX8750T are reactive random ethylene-butyl acrylate-glycidyl methacrylate terpolymers. Butyl acrylate contributes to the flexibility and polarity. Unlike grafted polymers, the reactive monomer glycidyl acrylate is polymerized on the ethylene backbone, which facilitates the formation of a more regular comb-like polymer structure.
[0009] The high-heat-resistant, high-viscosity asphalt described above uses a styrene-ethylene / propylene-styrene block copolymer as the high-viscosity modifier, which is obtained by selective hydrogenation of a styrene-isoprene-styrene compound. Preferably, the high-viscosity modifier is SEPS thermoplastic elastomer purchased from Kraton Polymers, Inc., with a styrene content of 15-20% (%wt). Its full English name is Styrene-ethylene / propylene-styrene block copolymer, hereinafter referred to as "SEPS".
[0010] This invention is achieved as follows: SEPS is obtained by selective hydrogenation of a styrene-isoprene-styrene compound. After the double bonds in the isoprene blocks or segments are saturated, an ethylene-propylene alternating structure is formed, abbreviated as EP structure. Preferably, the type with a high EP structure content is selected, with the styrene content controlled at 15-20%. The hydrogenated polyisoprene has branched methyl side chains, a glass transition temperature below -60°C, and no crystallinity; therefore, SEPS exhibits good elasticity and hysteresis behavior. When swollen and dispersed in asphalt, the modified asphalt, similar to a thermoplastic elastomer, has its flexibility further enhanced. Its superior flexibility and high elasticity allow the SEPS-modified asphalt to maintain enhanced shear and impact resistance even at low temperatures. The transformation of unsaturated double bonds in the isoprene blocks or segments into saturated bonds after hydrogenation also improves the polymer's oxidation resistance and weather resistance. The styrene segments enhance the impact resistance and strength of SEPS.
[0011] Both the crosslinking agents citrulline and malic acid are bifunctional, capable of ring-opening reactions with reactive modifiers and epoxy groups of high-heat-resistant epoxy monomers to form crosslinked stereocomb polymers. The styrene blocks of SEPS and the aromatic ring structures of the high-heat-resistant monomers exhibit similar compatibility, aggregating to form hard regions that maintain high impact resistance at high temperatures. Meanwhile, the EP blocks and the ethylene-acrylic acid backbone form soft regions, possessing high toughness and viscoelasticity, serving as energy-absorbing regions for the modified asphalt. They also exhibit a low glass transition temperature, ensuring low-temperature flexibility and good weather resistance of the modified material. The hydroxyl groups and butyl acrylate generated by the crosslinking agents and epoxy ring-opening have polar structures, ensuring good adhesion and water stability between the modified asphalt and aggregates.
[0012] Based on the same inventive concept, this invention provides a method for preparing the high heat-resistant, high-viscosity asphalt as described above, comprising the following steps: Step 1: Take No. 90 base asphalt according to the set ratio and heat it to 180-185℃. Add high viscosity modifier and reactive modifier according to the set ratio. Shear and disperse for 1-3 hours at a speed of 3000-4000 rpm and maintain the temperature at 180-190℃ until the high viscosity modifier is evenly dispersed. Preferably, take No. 90 base asphalt according to the set ratio and heat it to 180℃. Add high viscosity modifier and reactive modifier according to the set ratio. Shear and disperse for 2 hours at a speed of 3000 rpm and maintain the temperature at 180℃ until the high viscosity modifier is evenly dispersed. Step 2: Switch to stirring mode, add the high heat-resistant epoxy monomer according to the set ratio, and continue to disperse for 15-50 minutes until the high heat-resistant epoxy monomer is completely dissolved. Maintain the temperature at 180-190℃ and the rotation speed at 3000-4000 rpm. Preferably, add the high heat-resistant epoxy monomer according to the set ratio, continue to disperse for 30 minutes until the high heat-resistant epoxy monomer is completely dissolved, maintain the temperature at 180℃ and the rotation speed at 3000 rpm. Step 3: Lower the temperature to 160-170℃, add the crosslinking agent in batches according to the set ratio, control the temperature below 170℃, and rotate the speed at 300-350 rpm until the material is added; preferably, lower the temperature to 160-170℃, add the crosslinking agent in batches according to the set ratio, control the temperature at 160℃, and rotate the speed at 300 rpm until the material is added. Step 4: Heat to 180-185℃ and continue to mature for 1.5-2 hours to obtain high heat-resistant high viscosity asphalt; preferably, heat to 180℃ and continue to mature for 2 hours to obtain high heat-resistant high viscosity asphalt.
[0013] Based on the same inventive concept, this invention provides a high-viscosity asphalt mixture, comprising a high-heat-resistant high-viscosity asphalt as described above or a high-heat-resistant high-viscosity asphalt prepared by the preparation method described above. Preferably, the high-viscosity asphalt accounts for 5.2% by weight in the high-viscosity asphalt mixture.
[0014] Based on the same inventive concept, the present invention also provides the application of the high heat-resistant high viscosity asphalt as described above, or the high heat-resistant high viscosity asphalt prepared by the preparation method described above, or the high viscosity asphalt mixture described above, as a road construction material in road maintenance or road construction.
[0015] The beneficial effects of the technical solution provided by this invention are as follows: 1. The present invention provides a high heat-resistant, high-viscosity asphalt, preferably of a type with a high EP content, with the styrene content controlled at 15-20%. The hydrogenated polyisoprene has branched methyl side chains, a glass transition temperature below -60°C, and no crystallinity, thus SEPS has good elasticity and hysteresis behavior. When swollen and dispersed in asphalt, the modified asphalt, which forms a thermoplastic elastomer, has its flexibility further enhanced. Its superior flexibility and high elasticity enable the SEPS-modified asphalt to still have enhanced shear and impact resistance even at low temperatures. After hydrogenation, the unsaturated double bonds of the EP chain are transformed into saturated bonds, which also improves the polymer's oxidation resistance and weather resistance.
[0016] 2. This invention provides a high-heat-resistant, high-viscosity asphalt. The crosslinking agents citrulline and malic acid are both bifunctional, capable of ring-opening reactions with reactive modifiers and epoxy groups of high-heat-resistant epoxy monomers to form crosslinked, three-dimensional comb-shaped polymers. The styrene blocks of SEPS aggregate to form hard regions, maintaining high impact resistance even at high temperatures, while the EP blocks and ethylene-acrylic acid backbone form soft regions with high toughness and viscoelasticity, ensuring the modified material's low-temperature flexibility and good weather resistance. The hydroxyl groups and butyl acrylate generated by the crosslinking of the crosslinking agent and the ring-opening of the epoxy resin have polar structures, ensuring good adhesion and water stability between the modified asphalt and aggregates.
[0017] 3. The high viscosity asphalt provided by this invention has high viscosity and its viscosity toughness (25℃) is 27.4~31.2Nm, which is relatively high; its TFOT (or RTFOT) residue ductility (10℃, 5cm / min) is 20.7~22.8 cm, which is good aging resistance; in addition, its storage stability segregation (48h softening point difference) is 0.5~0.9℃, which is good storage stability.
[0018] 4. The high-viscosity asphalt mixture provided by this invention has a dynamic stability of 6749-7736 cycles / mm in high-temperature rutting tests and a stiffness modulus of 3.95-4.36 MPa in low-temperature bending tests. This indicates that the high-viscosity asphalt mixture prepared using the high-heat-resistant high-viscosity asphalt provided by this invention has significant high-temperature rutting resistance and low-temperature resistance, and can be well adapted to the climatic conditions of areas with large diurnal temperature differences. Detailed Implementation
[0019] The technical solutions of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0020] Unless otherwise defined, all technical and scientific terms used in this specification have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used in this specification is for the purpose of describing particular embodiments only and is not intended to limit the invention. The term "and / or" as used in this specification includes any and all combinations of one or more of the associated listed items. It should be understood that, unless otherwise specified, all materials of this invention are commercially available.
[0021] The α-naphthyl glycidyl ether, CAS No.: 61249-00-1, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; triphenylmethyl glycidyl ether, CAS No.: 65291-30-7, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; 2-biphenyl glycidyl ether, CAS No.: 7144-65-2, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; poly[(phenyl glycidyl ether)-co-formaldehyde], CAS No.: 28064-14-4, was purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; citrulline Malic acid, CAS number: 54940-97-5, was purchased from Wuhan Beileye Biomedical Technology Co., Ltd.; LOTADER® AX8750 and LOTADER® AX8750T were both purchased from SK Group, South Korea; SEPS thermoplastic elastomer was purchased from Kraton Polymers, Inc., USA, G1702SQR1111; No. 90 bitumen was purchased from Shandong Jingbo Petrochemical Co., Ltd., with a penetration (25℃, 5s, 100g) of 80-100 at 0.1mm, a softening point (R&B) of 46℃, and a ductility (cm) of 47 at 10℃.
[0022] Example 1 A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 28 parts of poly[(phenyl glycidyl ether)-co-formaldehyde], 3 parts of citrulline-malic acid, and LOTADER. ® AX8750 15 copies, SEPS 54 copies.
[0023] This high-heat-resistant, high-viscosity asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 2 hours, rotation speed 3000 rpm, temperature maintained at 180℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add poly[(phenyl glycidyl ether)-co-formaldehyde] according to the set ratio, continue to disperse for 30 minutes until poly[(phenyl glycidyl ether)-co-formaldehyde] is completely dissolved, keep the temperature at 180℃ and the speed at 3000 rpm; Step 3: Lower the temperature to 160℃, add citrulline-malic acid in batches according to the set ratio, control the temperature at 160℃ and the rotation speed at 300 rpm, and the feeding is complete. Step 4: Raise the temperature to 180℃ and continue to mature for 2 hours to obtain high heat-resistant, high-viscosity asphalt.
[0024] Example 2 A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 21 parts of α-naphthyl glycidyl ether, 4 parts of citrulline-malic acid, and LOTADER. ® AX8750 17 copies, SEPS 58 copies.
[0025] This high-heat-resistant, high-viscosity asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 1.5 hours, rotation speed 3500 rpm, temperature maintained at 180℃, until SEPS is uniformly dispersed; Step 2: Switch to stirring mode, add α-naphthyl glycidyl ether according to the set ratio, and continue to disperse for 40 minutes until the high heat-resistant epoxy monomer α-naphthyl glycidyl ether is completely dissolved. Maintain the temperature at 180℃ and the rotation speed at 3000 rpm. Step 3: Lower the temperature to 170℃, add citrulline-malic acid in batches according to the set ratio, control the temperature at 170℃ and the rotation speed at 350 rpm, and the feeding is complete. Step 4: Raise the temperature to 180℃ and continue to mature for 2 hours to obtain high heat-resistant, high-viscosity asphalt.
[0026] Example 3 A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 19 parts of triphenylmethyl-glycidyl ether, 4 parts of citrulline-malic acid, and LOTADER. ® AX8750 18 copies, SEPS 59 copies.
[0027] This high-heat-resistant, high-viscosity asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 185℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 3 hours, rotation speed 3000 rpm, temperature maintained at 185℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add triphenylmethyl glycidyl ether according to the set ratio, continue to disperse for 20 minutes until the triphenylmethyl glycidyl ether is completely dissolved, keep the temperature at 185℃ and the speed at 3000 rpm; Step 3: Lower the temperature to 160℃, add citrulline-malic acid in batches according to the set ratio, control the temperature at 160℃ and the rotation speed at 350rpm, and the feeding is complete. Step 4: Raise the temperature to 185℃ and continue to mature for 1.5 hours to obtain high heat-resistant, high-viscosity asphalt.
[0028] Example 4 A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 29 parts of 2-biphenyl glycidyl ether, 4 parts of citrulline-malic acid, and LOTADER. ® AX8750 17 copies, SEPS 50 copies.
[0029] This high-heat-resistant, high-viscosity asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 1 hour, rotation speed 4000 rpm, temperature maintained at 180℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add 2-biphenyl glycidyl ether according to the set ratio, continue to disperse for 40 minutes until 2-biphenyl glycidyl ether is completely dissolved, keep the temperature at 180℃ and the speed at 4000 rpm; Step 3: Lower the temperature to 170℃, add the crosslinking agent citrulline-malic acid in batches according to the set ratio, control the temperature at 170℃ and the rotation speed at 350 rpm, and the feeding is complete. Step 4: Raise the temperature to 185℃ and continue to mature for 2 hours to obtain high heat-resistant, high-viscosity asphalt.
[0030] Example 5 A high-heat-resistant, high-viscosity asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 25 parts of poly[(phenyl glycidyl ether)-co-formaldehyde], 5 parts of citrulline-malic acid, and LOTADER. ® AX8750T 19 copies, SEPS 51 copies.
[0031] This high-heat-resistant, high-viscosity asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750T, shear dispersion for 2 hours, rotation speed 3500 rpm, temperature maintained at 180℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add poly[(phenyl glycidyl ether)-co-formaldehyde] according to the set ratio, continue to disperse for 40 minutes until poly[(phenyl glycidyl ether)-co-formaldehyde] is completely dissolved, keep the temperature at 180℃ and the speed at 3500 rpm; Step 3: Lower the temperature to 170℃, add the crosslinking agent citrulline-malic acid in batches according to the set ratio, control the temperature at 170℃ and the rotation speed at 300 rpm, and the feeding is complete. Step 4: Raise the temperature to 185℃ and continue to mature for 1.5 hours to obtain high heat-resistant, high-viscosity asphalt.
[0032] Comparative Example 1 A modified asphalt, mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 28 parts of BPA epoxy resin, 3 parts of citrulline-malic acid, and LOTADER. ® AX8750 15 copies, SEPS 54 copies.
[0033] The BPA epoxy resin was purchased from Jinan Xinwo Chemical Co., Ltd., CAS No.: 80-05-7. The same base asphalt, citrulline-malic acid, and LOTADER were used as in Example 1. ® AX8750, SEPS.
[0034] The modified asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 2 hours, rotation speed 3000 rpm, temperature maintained at 180℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add BPA epoxy resin according to the set ratio, continue to disperse for 30 minutes until the BPA epoxy resin is completely dissolved, keep the temperature at 180℃ and the speed at 3000 rpm. Step 3: Lower the temperature to 160℃, add the crosslinking agent citrulline-malic acid in batches according to the set ratio, control the temperature at 160℃ and the rotation speed at 300 rpm, and the feeding is complete. Step 4: Heat to 180℃ and continue maturation for 2 hours to obtain modified asphalt.
[0035] Comparative Example 2 A modified asphalt, mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 28 parts of poly[(phenyl glycidyl ether)-co-formaldehyde], 3 parts of adipic acid, and LOTADER. ® AX8750 15 parts, SEPS 54 parts. Adipic acid, CAS number: 124-04-9, was purchased from Sigma-Aldrich (Shanghai) Trading Co., Ltd. The same base bitumen, poly[(phenyl glycidyl ether)-co-formaldehyde], and loter were used as in Example 1. ® AX8750, SEPS.
[0036] The modified asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base asphalt to 180℃ according to the set ratio, and add SEPS and LOTADER according to the set ratio. ® AX8750, shear dispersion for 2 hours, rotation speed 3000 rpm, temperature maintained at 180℃, until SEPS is evenly dispersed; Step 2: Switch to stirring mode, add poly[(phenyl glycidyl ether)-co-formaldehyde] according to the set ratio, continue to disperse for 30 minutes until poly[(phenyl glycidyl ether)-co-formaldehyde] is completely dissolved, keep the temperature at 180℃ and the speed at 3000 rpm; Step 3: Lower the temperature to 160℃, add adipic acid in batches according to the set ratio, control the temperature at 160℃ and the rotation speed at 300 rpm, and the feeding is complete; Step 4: Heat to 180℃ and continue maturation for 2 hours to obtain modified asphalt.
[0037] Comparative Example 3 A modified asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 28 parts of poly[(phenyl glycidyl ether)-co-formaldehyde], 3 parts of citrulline-malic acid, 15 parts of EBA 1400HN, and 54 parts of SEPS. EBA 1400HN is a copolymer of ethylene and butyl acrylate, purchased from Lucobi GmbH, Germany, CAS number: 10056-2-1. The same base asphalt, poly[(phenyl glycidyl ether)-co-formaldehyde], citrulline-malic acid, and SEPS are used as in Example 1.
[0038] The modified asphalt is prepared by the following method, including the following steps: Step 1: Take No. 90 base asphalt according to the set ratio and heat it to 180℃. Add SEPS and EBA according to the set ratio, shear and disperse for 2 hours, rotate at 3000 rpm, and keep the temperature at 180℃ until the SEPS is evenly dispersed. Step 2: Switch to stirring mode, add the high heat-resistant epoxy monomer poly[(phenyl glycidyl ether)-co-formaldehyde], and continue to disperse for 30 minutes until the high heat-resistant epoxy monomer poly[(phenyl glycidyl ether)-co-formaldehyde] is completely dissolved. Maintain the temperature at 180℃ and the rotation speed at 3000 rpm.
[0039] Step 3: Lower the temperature to 160℃, add the crosslinking agent citrulline-malic acid in batches, control the temperature at 160℃ and the rotation speed at 300 rpm, and the feeding is complete.
[0040] Step 4: Heat to 180℃ and continue maturation for 2 hours to obtain modified asphalt.
[0041] Comparative Example 4 A modified asphalt is mainly prepared from the following components in parts by weight: 90 parts of No. 90 base asphalt, 28 parts of poly[(phenyl glycidyl ether)-co-formaldehyde], 3 parts of citrulline-malic acid, 15 parts of LOTADER® AX8750, and 54 parts of SBS resin. The SBS resin is a block copolymer of styrene and butadiene, purchased from Sinopec brand 1301. The same base asphalt, poly[(phenyl glycidyl ether)-co-formaldehyde], citrulline-malic acid, and LOTADER® were used as in Example 1. ® AX8750.
[0042] The modified asphalt is prepared by the following method, including the following steps: Step 1: Heat No. 90 base bitumen to 180°C according to the set ratio, and add SBS resin and LOTADER according to the set ratio. ® AX8750, shear dispersion for 2 hours, rotation speed 3000 rpm, temperature maintained at 180℃, until SBS is uniformly dispersed; Step 2: Switch to stirring mode, add poly[(phenyl glycidyl ether)-co-formaldehyde] according to the set ratio, continue to disperse for 30 minutes until poly[(phenyl glycidyl ether)-co-formaldehyde] is completely dissolved, keep the temperature at 180℃ and the speed at 3000 rpm; Step 3: Lower the temperature to 160℃, add the crosslinking agent citrulline-malic acid in batches according to the set ratio, control the temperature at 160℃ and the rotation speed at 300 rpm, and the feeding is complete. Step 4: Heat to 180℃ and continue maturation for 2 hours to obtain modified asphalt.
[0043] Experimental Results and Performance Analysis 1. Preparation and performance testing of high-viscosity asphalt The high heat-resistant, high-viscosity asphalt prepared in Examples 1-5 and the asphalt prepared in Comparative Examples 1-4 of this application are evaluated by testing the performance indicators of the prepared high-viscosity asphalt. Specifically, to characterize the performance of the high heat-resistant, high-viscosity asphalt prepared in Examples 1-5 and compared with the asphalt in Comparative Examples 1-4, the asphalt prepared in Examples 1-5 and Comparative Examples 1-4 were used respectively, and performance tests were performed on the different high-viscosity asphalts.
[0044] According to the standard "JTGE20-2011 Test Procedures for Asphalt and Asphalt Mixtures in Highway Engineering", various relevant indicators of high viscosity asphalt were tested. The specific test evaluation results are shown in Table 1.
[0045] Table 1 Evaluation results of high viscosity asphalt
[0046] As can be seen from Table 1, the high viscosity asphalt prepared by this invention has a high viscosity and a viscosity toughness (25℃) of 27.4~31.2Nm, which is relatively high. Its TFOT (or RTFOT) residue ductility (10℃, 5cm / min) is 20.7~22.8 cm, which is good aging resistance. In addition, its storage stability segregation (48h softening point difference) is 0.5~0.9℃, which is good storage stability.
[0047] Compared with Example 1, the asphalt prepared by replacing poly[(phenyl glycidyl ether)-co-formaldehyde] with BPA epoxy resin in Comparative Example 1 has a higher penetration and lower viscosity toughness. This indicates that the addition of poly[(phenyl glycidyl ether)-co-formaldehyde] in this application increases the viscosity of the high-viscosity asphalt and also increases the intermolecular forces, resulting in better resistance to shear deformation.
[0048] Compared with Example 1, the asphalt prepared by replacing citrulline-malic acid with adipic acid in Comparative Example 2 had a lower dynamic viscosity at 60°C, indicating that the addition of citrulline-malic acid in this application effectively improved the crosslinking degree of the high-viscosity asphalt system.
[0049] Compared to Example 1, Comparative Example 3, where asphalt was prepared by replacing Lotader® AX8750 with EBA 1400HN, showed a significant decrease in ductility and poor storage stability, indicating that the Lotader® used in this application... ® AX8750 has a good effect on improving the ductility and dispersion stability of high viscosity asphalt.
[0050] Compared with Example 1, the asphalt prepared by replacing SEPS with SBS resin in Comparative Example 4 showed varying degrees of performance degradation after aging, indicating that the addition of SEPS in this application has significant anti-aging properties. It is also evident that the asphalt prepared in Examples 1-5, compared with the asphalt prepared in Comparative Examples 1-4, has higher viscosity, viscoelasticity, and better aging resistance. Furthermore, the high-viscosity asphalt in this application also exhibits better storage stability.
[0051] 2. Preparation and performance testing of high-viscosity asphalt mixtures Standard samples of high-viscosity asphalt mixtures were prepared and tested according to GB / T 36143-2018 High-modulus Fatigue-Resistant Asphalt Mixtures for Roads. The test results are shown in Table 2. The content of high-viscosity asphalt was 5.2%.
[0052] Table 2 Evaluation Results of Asphalt Mixtures
[0053] As shown in Table 2, the high-viscosity asphalt mixtures prepared using the high-heat-resistant high-viscosity asphalt in Examples 1 to 5 exhibit significantly improved high-temperature dynamic stability and low-temperature stiffness modulus compared to the asphalt mixtures prepared using asphalt in Comparative Examples 1 to 4. The high-viscosity asphalt mixture prepared by this invention shows a dynamic stability of 6749–7736 cycles / mm in high-temperature rutting tests and a stiffness modulus of 3.95–4.36 MPa in low-temperature bending tests. This indicates that the asphalt mixture prepared using the high-heat-resistant high-viscosity asphalt provided in this application has significant high-temperature rutting resistance and low-temperature resistance, making it well-suited for climatic conditions with large diurnal temperature variations.
[0054] Analysis of the test results in Tables 1 to 2 of Examples 1 to 5 and Comparative Examples 1 to 4 shows that the high-viscosity asphalt mixture prepared by the high heat-resistant high-viscosity asphalt in this application has high viscosity, good dispersion stability and shear resistance, significant high-temperature rutting resistance and low-temperature resistance, and is well-suited for the climate conditions of areas with large diurnal temperature differences.
[0055] In other words, the high heat-resistant epoxy monomer, crosslinking agent, reactive modifier, and high viscosity modifier of this invention work together to achieve the overall comprehensive performance of asphalt and asphalt mixture. Replacing similar components cannot achieve the excellent effect of this invention.
[0056] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from its spirit or basic characteristics. Therefore, the embodiments should be considered exemplary and non-limiting in all respects, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention. Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.
Claims
1. A high-heat-resistant, high-viscosity asphalt, characterized in that, It is mainly prepared from the following components in parts by weight: 87-95 parts of base asphalt, 15-30 parts of high heat-resistant epoxy monomer, 1-10 parts of crosslinking agent, 5-20 parts of reactive modifier, and 35-65 parts of high viscosity modifier.
2. The high heat-resistant, high-viscosity asphalt according to claim 1, characterized in that, The base asphalt is No. 90 base asphalt.
3. The high heat-resistant, high-viscosity asphalt according to claim 2, characterized in that, The high heat-resistant epoxy monomer is one or a mixture of α-naphthyl glycidyl ether, triphenylmethyl glycidyl ether, 2-biphenyl glycidyl ether, and poly[(phenyl glycidyl ether)-co-formaldehyde].
4. The high heat-resistant, high-viscosity asphalt according to claim 2, characterized in that, The crosslinking agent is citrulline-malic acid.
5. The high heat-resistant, high-viscosity asphalt according to claim 2, characterized in that, The reactive modifier is LOTADER. ® AX8750 or LOTADER ® AX8750T.
6. The high heat-resistant, high-viscosity asphalt according to claim 2, characterized in that, The high-viscosity modifier is a styrene-ethylene / propylene-styrene block copolymer, which is a product obtained by selective hydrogenation of styrene-isoprene-styrene compound.
7. The high heat-resistant, high-viscosity asphalt according to claim 2, characterized in that, It is mainly prepared from the following components in parts by weight: 90 parts of base asphalt, 19-29 parts of high heat-resistant epoxy monomer, 3-5 parts of crosslinking agent, 15-19 parts of reactive modifier, and 50-59 parts of high viscosity modifier.
8. A method for preparing high-heat-resistant, high-viscosity asphalt according to claims 2-7, characterized in that, Includes the following steps: Step 1: Take No. 90 base asphalt according to the set ratio and heat it to 180-185℃. Add high viscosity modifier and reactive modifier according to the set ratio. Shear and disperse for 1-3 hours, with a rotation speed of 3000-4000 rpm and the temperature maintained at 180-190℃ until the high viscosity modifier is evenly dispersed. Step 2: Switch to stirring mode, add the high heat-resistant epoxy monomer according to the set ratio, and continue to disperse for 15-50 minutes until the high heat-resistant epoxy monomer is completely dissolved. Maintain the temperature at 180-190℃ and the rotation speed at 3000-4000 rpm. Step 3: Lower the temperature to 160-170℃, add the crosslinking agent in batches according to the set ratio, control the temperature below 170℃, and rotate the speed at 300-350 rpm until the material is added. Step 4: Raise the temperature to 180-185℃ and continue to mature for 1.5-2 hours to obtain high heat-resistant, high-viscosity asphalt.
9. A high-viscosity asphalt mixture, characterized in that, This includes a high heat-resistant, high-viscosity asphalt as described in claims 1 to 7, or a high heat-resistant, high-viscosity asphalt prepared by the preparation method described in claim 8.
10. The application of a high heat-resistant high-viscosity asphalt as described in claims 1 to 7, or a high heat-resistant high-viscosity asphalt prepared by the preparation method described in claim 8, or a high-viscosity asphalt mixture as described in claim 9, as a road construction material in road maintenance or road construction.