Regenerant for efficiently reactivating SBS modified asphalt and preparation method thereof

Abstract

The invention discloses a regenerant for efficiently reactivating SBS modified asphalt and a preparation method of the regenerant. The regenerant for efficiently reactivating the SBS modified asphalt comprises the following components in parts by mass: 50-75 parts of tung oil, 5-15 parts of a plasticizer, 15-25 parts of an SBS efficient activator and 5-10 parts of an initiator. According to the present invention, the component deficiency of the aged asphalt can be completely supplemented and balanced, the network structure of the SBS modified asphalt can be activated and enhanced, the high and low temperature, anti-aging and fatigue performance of the aged SBS modified asphalt can be significantly improved, the important significance is provided for further improving the pavement performance of the recycled asphalt pavement, and the method is suitable for large-scale promotion.

Description

Technical Field

[0001] The invention relates to the technical field of road construction materials, in particular to a regeneration agent for efficiently reactivating SBS modified asphalt and a preparation method thereof. Background Art

[0002] SBS is a thermoplastic copolymer with a triblock structure formed by the polymerization reaction of butadiene and styrene. As a thermoplastic material, SBS can flow and deform when heated, and has good compatibility with asphalt. When cooled to room temperature, it can form a rubber network structure in the asphalt and restore its elastic properties, thereby improving the mechanical properties of asphalt. Although SBS can significantly improve the high and low temperature performance of the matrix asphalt, as the service time increases, the modifier SBS will also be affected by the external environment and naturally age like the asphalt matrix, resulting in the deterioration of the road performance of the road paved with its modified asphalt. The damaged road surface needs to be repaired or rebuilt to restore the service performance of the road surface, which will generate a large amount of Waste SBS modified asphalt mixture. In recent years, with the extensive use of SBS modified asphalt in highway construction, the high-performance regeneration and recycling of waste SBS modified asphalt has become a hot topic in the field of road materials research in the world. Unlike the aging of base asphalt, the aging of SBS modified asphalt is not only the aging of the asphalt, but also the aging of the SBS modifier. After aging, the molecular chain of SBS will break and change from a triblock structure to a diblock structure (SB), resulting in the loss of the properties of the SBS elastomer and the destruction of the cross-linked network structure formed in the asphalt. Therefore, in addition to supplementing the asphalt components, the regeneration of aged SBS modified asphalt also needs to restore its triblock structure.

[0003] Patent CN201310380129.5 discloses an SBS modified asphalt regeneration agent composed of 20% to 45% heavy oil, 40% to 75% catalytic cracking oil slurry, 1% to 5% penetrant, and 3% to 10% SBS molecular structure restorer. Patent CN112143244B discloses an SBS modified asphalt regeneration agent composed of 65wt% to 75wt% catalytic cracking oil slurry, 5wt% to 15wt% penetrant, and 15wt% to 25wt% amino-terminated SBS molecular structure restorer. Patents CN201310380129.5 and CN112143244B respectively use esterification reaction and amidation reaction to restore the SBS molecular structure. Both reactive repair agents simply restore the SBS molecular structure and use the self-crosslinking effect of the SBS modifier to restore the network structure. The restored network structure has low strength and poor resistance to secondary aging, which affects the durability of the regenerated asphalt pavement. Summary of the invention

[0004] The object of the present invention is to provide a regeneration agent for efficiently reactivating SBS modified asphalt and a preparation method thereof, so as to solve the problems raised in the above background technology.

[0005] To achieve the above object, the present invention provides the following technical scheme: a regeneration agent for efficient reactivation of SBS modified asphalt and a preparation method thereof, wherein the regeneration agent for efficient reactivation of SBS modified asphalt comprises the following components by weight: 50 to 75 parts of tung oil, 5 to 15 parts of plasticizer, 15 to 25 parts of SBS efficient activator, and 5 to 10 parts of initiator; the preparation method of the regeneration agent for efficient reactivation of SBS modified asphalt comprises the following steps:

[0006] Step 1: Heat 50-75 parts of tung oil to 90-100°C;

[0007] Step 2: Add 5 to 15 parts of plasticizer and 15 to 25 parts of SBS high-efficiency activator to the heated tung oil by weight, and under the premise of keeping the temperature constant, stir the mixed materials with an automatic stirring device for 10 to 30 minutes, and set the stirring rate of the automatic stirring device to 300 r / min;

[0008] Step 3: Add 5 to 10 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 to 10 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after stirring and mixing, you can get a regeneration agent that efficiently reactivates SBS modified asphalt.

[0009] Preferably, the plasticizer is dioctyl phthalate.

[0010] Preferably, the initiator is benzil dimethyl ether.

[0011] Preferably, the automatic stirring equipment used in step 2 and step 3 is a constant temperature stirrer.

[0012] Preferably, the constant temperature of the stirring equipment in step 2 and step 3 is 90-100°C.

[0013] Compared with the prior art, the beneficial effects of the present invention are as follows: the regeneration agent for efficient reactivation of SBS modified asphalt and the preparation method thereof introduce nanocellulose crystals with active thiol groups, and the nanocellulose crystals are catalyzed by an initiator to undergo a thiol-ene click reaction with aged SBS molecules, so as to firmly connect the nanocellulose crystals with SBS to form a nano-modified SBS network structure with SBS as the matrix and nanocellulose crystals as the filler; as the hydroxyl groups on the surface of the nanocellulose crystals are retained, they overlap with each other to form a stable percolation network; in this process, the chemical self-crosslinking effect of SBS further strengthens the construction of the network structure; benefiting from these three strong interactions, the activated SBS molecules are nanocellulose crystal-modified SBS molecules, which evolve from a single SBS network structure to a multiple network structure in which the nanocellulose crystals and SBS fully interact with each other, and while maintaining the characteristics of the SBS network structure, its strength and modulus are greatly improved, so that the regenerated SBS modified asphalt exhibits better high and low temperature performance, fatigue resistance and secondary aging resistance. DETAILED DESCRIPTION

[0014] The technical solutions in the embodiments of the present invention are described clearly and completely below. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0015] The invention provides a technical solution: a regeneration agent for efficient reactivation of SBS modified asphalt and a preparation method thereof, wherein the regeneration agent for efficient reactivation of SBS modified asphalt comprises the following components by weight: 50-75 parts of tung oil, 5-15 parts of plasticizer, 15-25 parts of SBS efficient activator, and 5-10 parts of initiator; the plasticizer is dioctyl phthalate, the initiator is benzil dimethyl ether, the tung oil selected in the invention is natural tung oil, which is a commercially available product provided by Jinan Yingshun Chemical Co., Ltd.; the selected nanocellulose crystals are sulfonated nanocellulose crystals obtained by hydrolyzing natural plant fibers with sulfuric acid, and the surface of the cellulose crystals is sulfonated nanocellulose crystals. It has a sulfonic acid group and is a commercially available product provided by Nanjing Tianlu Nanotechnology Co., Ltd.; the remaining reagents are analytically pure reagents provided by Shanghai MacLean Biochemical Technology Co., Ltd. The preparation method of the SBS high-efficiency activator is as follows: prepare a nanocellulose crystal aqueous solution with a concentration of 10 g / L, heat the temperature to 70°C; add sodium carbonate buffer to adjust the pH to 9.2; then add 0.3 mmol of cysteamine hydrochloride and 135 mmol of sodium triacetoxyborohydride, maintain the temperature at 70°C, rotate at 300 r / min and fully react for 24 hours; then vacuum dry at 70°C to obtain the SBS high-efficiency activator;

[0016] The method for preparing the regeneration agent for efficiently reactivating SBS modified asphalt comprises the following steps:

[0017] Step 1: Heat 50-75 parts of tung oil to 90-100°C;

[0018] Step 2: Add 5 to 15 parts of plasticizer and 15 to 25 parts of SBS high-efficiency activator to the heated tung oil by weight, and under the premise of keeping the temperature constant, stir the mixed materials for 10 to 30 minutes using an automatic stirring device, set the stirring rate of the automatic stirring device to 300 r / min, and the automatic stirring device is a constant temperature stirrer, and the constant temperature of the device is 90 to 100° C.;

[0019] Step 3: Add 5 to 10 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 to 10 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after stirring and mixing, you can get a regeneration agent that efficiently reactivates SBS modified asphalt.

[0020] The aged SBS modified asphalt used in the following examples is prepared by short-term aging and long-term aging of SBS modified asphalt according to the T0610 and T0630 test methods in the national standard specification "Test Procedures for Asphalt and Asphalt Mixtures for Highway Engineering" JTG E20-2011.

[0021] Embodiment 1:

[0022] A regeneration agent for efficient reactivation of SBS modified asphalt, comprising the following components by mass: 50 parts of tung oil, 15 parts of dioctyl phthalate, 25 parts of SBS efficient activator, and 10 parts of benzil dimethyl ether. ;

[0023] A method for preparing a regeneration agent for efficiently reactivating SBS modified asphalt, the method comprising the following steps:

[0024] Step 1: Heat 50 parts of tung oil to 90-100°C;

[0025] Step 2: Add 15 parts of plasticizer and 25 parts of SBS high-efficiency activator to the heated tung oil, and under the premise of keeping the temperature constant, stir the mixed materials thoroughly for 30 minutes using an automatic stirring device, and set the stirring rate of the automatic stirring device to 300r / min;

[0026] Step 3: Add 10 parts of initiator by mass, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after the stirring and mixing is completed, the regeneration agent that efficiently reactivates the SBS modified asphalt can be obtained;

[0027] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0028] Embodiment 2:

[0029] A regeneration agent for efficiently reactivating SBS modified asphalt, comprising the following components by weight: 62 parts of tung oil, 10 parts of dioctyl phthalate, 20 parts of SBS high-efficiency activator, and 8 parts of benzil dimethyl ether;

[0030] A method for preparing a regeneration agent for efficiently reactivating SBS modified asphalt, the method comprising the following steps:

[0031] Step 1: Heat 62 parts of tung oil to 90-100°C;

[0032] Step 2: Add 10 parts of plasticizer and 20 parts of SBS high-efficiency activator to the heated tung oil, and under the premise of keeping the temperature constant, stir the mixed materials thoroughly for 20 minutes using an automatic stirring device, and set the stirring rate of the automatic stirring device to 300r / min;

[0033] Step 3: Add 8 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 8 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after the stirring and mixing is completed, the regeneration agent that efficiently reactivates the SBS modified asphalt can be obtained;

[0034] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0035] Embodiment 3:

[0036] A regeneration agent for efficiently reactivating SBS modified asphalt, comprising the following components by weight: 75 parts of tung oil, 5 parts of dioctyl phthalate, 15 parts of SBS high-efficiency activator, and 5 parts of benzil dimethyl ether;

[0037] A method for preparing a regeneration agent for efficiently reactivating SBS modified asphalt, the method comprising the following steps:

[0038] Step 1: Heat 75 parts of tung oil to 90-100°C;

[0039] Step 2: Add 5 parts of plasticizer and 15 parts of SBS high-efficiency activator to the heated tung oil by weight, and under the premise of keeping the temperature constant, stir the mixed materials with an automatic stirring device for 10 minutes, and set the stirring rate of the automatic stirring device to 300r / min;

[0040] Step 3: Add 5 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after the stirring and mixing is completed, the regeneration agent that efficiently reactivates the SBS modified asphalt can be obtained;

[0041] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0042] Embodiment 4:

[0043] A regeneration agent for efficiently reactivating SBS modified asphalt, comprising the following components by weight: 60 parts of tung oil, 5 parts of dioctyl phthalate, 25 parts of SBS high-efficiency activator, and 10 parts of benzil dimethyl ether;

[0044] A method for preparing a regeneration agent for efficiently reactivating SBS modified asphalt, the method comprising the following steps:

[0045] Step 1: Heat 60 parts of tung oil to 90-100°C;

[0046] Step 2: Add 5 parts of plasticizer and 25 parts of SBS high-efficiency activator to the heated tung oil, and under the premise of keeping the temperature constant, stir the mixed materials thoroughly for 20 minutes using an automatic stirring device, and set the stirring rate of the automatic stirring device to 300r / min;

[0047] Step 3: Add 10 parts of initiator by mass, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 10 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after the stirring and mixing is completed, a regeneration agent that efficiently reactivates the SBS modified asphalt can be obtained;

[0048] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0049] Embodiment 5:

[0050] A regeneration agent for efficiently reactivating SBS modified asphalt, comprising the following components by weight: 65 parts of tung oil, 15 parts of dioctyl phthalate, 15 parts of SBS high-efficiency activator, and 5 parts of benzil dimethyl ether;

[0051] A method for preparing a regeneration agent for efficiently reactivating SBS modified asphalt, the method comprising the following steps:

[0052] Step 1: Heat 65 parts of tung oil to 90-100°C;

[0053] Step 2: Add 15 parts of plasticizer and 15 parts of SBS high-efficiency activator to the heated tung oil by weight, and under the premise of keeping the temperature constant, stir the mixed materials with an automatic stirring device for 20 minutes, and set the stirring rate of the automatic stirring device to 300r / min;

[0054] Step 3: Add 5 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after the stirring and mixing is completed, the regeneration agent that efficiently reactivates the SBS modified asphalt can be obtained;

[0055] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0056] Comparative Example 1:

[0057] Patent CN201310380129.5 discloses an SBS modified asphalt regeneration agent composed of 20% to 45% heavy oil, 40% to 75% catalytic cracking oil slurry, 1% to 5% penetrant, and 3% to 10% SBS molecular structure restorer (1,4-butanediol diglycidyl ether). The preparation process of the regeneration agent is: weigh 29 parts by mass of heavy oil (softening point of 40°C, needle penetration of 220dmm) heated to 130°C and 63 parts by mass of catalytic cracking oil slurry (aromatic component mass content of 65%) heated to 130°C, add the catalytic cracking oil slurry to the heavy oil, stir at 130°C and 150rpm for 25min, then add 4 parts by mass of furfural and 4 parts by mass of 1,4-butanediol diglycidyl ether, maintain the temperature at 130°C and the speed at 150rpm, and continue stirring for 10min to obtain the SBS modified asphalt regeneration agent.

[0058] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0059] Comparative Example 2:

[0060] Patent CN112143244B discloses an SBS modified asphalt regeneration agent composed of 65wt% to 75wt% of catalytic cracking oil slurry, 5wt% to 15wt% of penetrant, and 15wt% to 25wt% of amino-terminated SBS molecular structure restorer. The preparation method of the amino-terminated SBS molecular structure restorer in the regeneration agent is as follows: heating laurylamine dipropylene diamine to 50 to 65°C, then slowly dripping carboxyl-terminated nitrile liquid rubber to keep the temperature constant, stirring at 200 to 400rpm for 30 to 45min after the dripping is completed, and then obtaining the amino-terminated SBS molecular structure restorer. The molar ratio of the carboxyl-terminated nitrile liquid rubber to the laurylamine dipropylene diamine is 1:2 to 1:2.5; and the average molecular weight of the carboxyl-terminated nitrile liquid rubber is 1500 to 2000. The preparation process of the regeneration agent is as follows: weigh 75 parts by weight of catalytic cracking oil slurry (with an aromatic component mass content of 65 wt%), heat it to 75° C., add 15 parts by weight of an amino-terminated SBS molecular structure restoration agent, stir it at a speed of 400 rpm and 75° C. for 5 minutes, then add 10 parts by weight of furfural, stir it at a speed of 400 rpm and 75° C. for 15 minutes, and thus obtain an amino-terminated reactive SBS modified asphalt regeneration agent.

[0061] 100 parts by mass of aged SBS modified asphalt was heated to 160-170° C., 7 parts by mass of the above regeneration agent was added, and stirred at a rotation speed of 300-500 r / min for 15 minutes to obtain regenerated SBS modified asphalt.

[0062] The regenerated SBS modified asphalt prepared in Examples 1-5 of the present invention and Comparative Examples 1-2 was subjected to performance tests. The experimental results are shown in Table 1 below.

[0063] Table 1 Test results of recycled SBS modified asphalt performance

[0064]

[0065] It can be seen from the test results of the examples in Table 1 that the comprehensive performance of the SBS modified asphalt regeneration agent prepared in Examples 1 to 5 far exceeds that of Comparative Examples 1 to 2, indicating that the SBS modified asphalt regeneration agent prepared by the present invention has superior performance. Compared with the comparative examples, the regeneration agent in Examples 1 to 5 not only repairs and activates the SBS molecular structure, but also performs nano-modification on it, and utilizes the interaction between nanocellulose crystals and SBS molecules to enhance the network structure in the modified asphalt, thereby greatly improving the high and low temperature performance and secondary aging resistance of the regenerated SBS modified asphalt.

[0066] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A regeneration agent for efficient reactivation of SBS modified asphalt and a preparation method thereof, characterized in that: The regeneration agent for efficient reactivation of SBS modified asphalt comprises the following components by weight: 50-75 parts of tung oil, 5-15 parts of plasticizer, 15-25 parts of SBS efficient activator, and 5-10 parts of initiator; the preparation method of the regeneration agent for efficient reactivation of SBS modified asphalt comprises the following steps: Step 1: Heat 50-75 parts of tung oil to 90-100°C; Step 2: Add 5 to 15 parts of plasticizer and 15 to 25 parts of SBS high-efficiency activator to the heated tung oil by weight, and under the premise of keeping the temperature constant, stir the mixed materials with an automatic stirring device for 10 to 30 minutes, and set the stirring rate of the automatic stirring device to 300 r / min; Step 3: Add 5 to 10 parts of initiator by weight, and under the premise of keeping the temperature constant, start the automatic stirring equipment again to stir the mixed materials for 5 to 10 minutes, set the stirring rate of the automatic stirring equipment to 300r / min, and after stirring and mixing, you can get a regeneration agent that efficiently reactivates SBS modified asphalt.

2. A regeneration agent for efficient reactivation of SBS modified asphalt and a preparation method thereof according to claim 1, characterized in that: The plasticizer is dioctyl phthalate.

3. The regeneration agent for efficient reactivation of SBS modified asphalt and its preparation method according to claim 1, characterized in that: The initiator is benzil dimethyl ether.

4. The regeneration agent for efficient reactivation of SBS modified asphalt and its preparation method according to claim 1, characterized in that: The automatic stirring equipment used in step 2 and step 3 is a constant temperature stirrer.

5. The regeneration agent for efficient reactivation of SBS modified asphalt and its preparation method according to claim 1, characterized in that: The constant temperature of the stirring equipment in step 2 and step 3 is 90-100°C.

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