Epoxy resin binder for elastic road surfaces and process for the production thereof
By preparing epoxy resin binder, the problems of stress concentration and poor durability of rubber elastic pavement at low temperatures were solved, achieving good flexibility and rubber particle adhesion, and improving the overall performance of rubber elastic pavement.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- CHANGAN UNIV
- Filing Date
- 2025-04-22
- Publication Date
- 2026-04-10
AI Technical Summary
In existing technologies, rubber elastic pavement is prone to stress concentration at the rubber-binder interface at low temperatures, leading to local cracking and poor durability. Furthermore, the existing polyurethane binder has insufficient adhesion to rubber, increasing production costs and construction difficulty.
An epoxy resin binder preparation method is adopted, in which diluent, epoxy resin, curing agent and accelerator are stirred and reacted, combined with modified rubber powder and limestone powder to form epoxy resin binder, and then stirred with filler to obtain epoxy resin binder, ensuring good flexibility and modulus similar to rubber particles at low temperature.
It improves the overall quality and durability of rubber elastic pavement, reduces interfacial stress, enhances the adhesion of rubber particles, and improves the low-temperature elastic recovery and durability of the pavement.
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Figure CN120442003B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The present application belongs to the technical field of road engineering materials, and particularly relates to an epoxy resin binder for elastic pavement and a preparation method thereof. BACKGROUND
[0002] The elastic pavement is a new type of pavement mainly composed of rubber particles, stones and polymer binders, and the rubber content is usually not less than 20% of the mass of the mixture, which has excellent noise reduction performance and environmental protection characteristics. Although the rubber elastic pavement performs well in noise reduction, the existing technology has a large difference between the high-elastic service temperature range of the binder and the mechanical properties of the rubber, which easily causes stress concentration at the rubber-binder interface at low temperature, resulting in local cracking of the mixture and poor durability, thereby reducing the service life of the rubber elastic pavement.
[0003] The existing technology uses elastic polyurethane binder to improve the durability of the rubber aggregate pavement by increasing the amount of polyurethane binder, and enhances the adhesion of rubber and polyurethane binder through surface modification technology of rubber particles.
[0004] However, the adhesion of polyurethane binder and rubber is insufficient, and there is still a large mechanical property between the existing polyurethane binder and rubber particles at certain temperatures, which leads to insufficient durability of the polyurethane-based rubber elastic pavement, and the surface modification process of the rubber particles is complex, which increases the production cost and construction difficulty. SUMMARY
[0005] In order to solve the above problems existing in the prior art, the present application provides an epoxy resin binder for elastic pavement and a preparation method thereof. The technical problem to be solved by the present application is solved by the following technical scheme:
[0006] The present application provides a preparation method of an epoxy resin binder for elastic pavement, comprising the following steps:
[0007] S1, the diluent, the epoxy resin and the curing agent are mutually soluble and stirred and reacted at a molar ratio of (1-2.5):1:(0.23-0.4), and after the reaction is cooled to room temperature, a promoter is added and stirred to obtain an epoxy resin binder; wherein the weight of the promoter accounts for 0.8-1.4% of the sum of the weights of the diluent, the epoxy resin and the curing agent;
[0008] S2, the fillers and the epoxy resin binder are stirred to obtain an epoxy resin binder at a mass ratio of (0.7-1.4):1.
[0009] In an embodiment of the present application, the epoxy resin comprises bisphenol A type epoxy resin, and the epoxy equivalent weight of the bisphenol A type epoxy resin is 185-230 g / mol, and the density is 1.15-1.2 g / cm3 .
[0010] In one embodiment of the present application, the diluent is obtained by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether in a mass ratio of (4.5-9):1:(0.5-1) at 30-50°C.
[0011] In one embodiment of the present application, the curing agent is obtained by stirring trimethylolpropane tris(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyetheramine in a mass ratio of (6-8):1:(0.5-1.5) at 30-50°C.
[0012] In one embodiment of the present application, the accelerator comprises 1-cyanoethyl-2-ethyl-4-methylimidazole and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:(0.5-0.8).
[0013] In one embodiment of the present application, the filler comprises modified rubber powder and limestone powder, wherein,
[0014] The modified rubber powder is obtained by surface treatment of rubber powder using a silane coupling agent;
[0015] The mass of the modified rubber powder is less than or equal to 20% of the mass of the limestone powder.
[0016] In one embodiment of the present application, step S1 comprises:
[0017] The diluent, epoxy resin and curing agent are miscible in a molar ratio of (1-2.5):1:(0.23-0.4) and stirred to react at 50-70°C for 10-20 min, and after the reactants are cooled to room temperature, the accelerator is added and stirred for 5-10 min to obtain an epoxy resin binder.
[0018] In one embodiment of the present application, step S2 comprises:
[0019] At room temperature, the filler and the epoxy resin binder in a mass ratio of (0.7-1.4):1 are first stirred at 300-500 rpm for 300-420 s, and then stirred at 500-1000 rpm for 300-420 s to obtain an epoxy resin cement.
[0020] Another embodiment of the present application provides an epoxy resin cement for elastic pavement, comprising: a filler and an epoxy resin binder in a mass ratio of (0.7-1.4):1, wherein,
[0021] The raw materials of the epoxy resin binder comprise a diluent, an epoxy resin, a curing agent and an accelerator;
[0022] The molar ratio of the diluent, the epoxy resin, the curing agent is (1-2.5):1:(0.23-0.4);
[0023] The weight of the accelerator accounts for 0.8-1.4% of the sum of the weights of the diluent, the epoxy resin and the curing agent.
[0024] In an embodiment of the present application, the high-elasticity service temperature of the epoxy resin binder is greater than or equal to -25℃, the viscosity is 2-30 Pa·s, and the gel time is greater than or equal to 1 h.
[0025] Compared with the prior art, the present application has the following beneficial effects:
[0026] The preparation method of the epoxy resin binder of the present application first stirs the diluent, the epoxy resin, the curing agent and the accelerator to obtain an epoxy resin binder, and then stirs the epoxy resin binder and the filler to obtain the epoxy resin binder. The epoxy resin binder has good flexibility, is in a stable high-elasticity state in a wide temperature range at low temperature, has good low-temperature elastic recovery capacity, and has a modulus similar to that of rubber particles, which can significantly reduce the interfacial stress and improve the overall quality and durability of the rubber elastic pavement. In addition, the adhesion between the epoxy resin binder and the rubber particles is good, which can effectively enhance the durability of the rubber elastic pavement. BRIEF DESCRIPTION OF DRAWINGS
[0027] Figure 1 A flowchart of a preparation method of an epoxy resin binder for an elastic pavement is provided for the embodiments of the present application. DETAILED DESCRIPTION
[0028] The present application will be further described in detail below in conjunction with specific embodiments, but the embodiments of the present application are not limited thereto.
[0029] Example 1
[0030] Please refer to Figure 1 , Figure 1 A flowchart of a preparation method of an epoxy resin binder for an elastic pavement is provided for the embodiments of the present application. The preparation method of the epoxy resin binder comprises the following steps:
[0031] S1, the diluent, the epoxy resin and the curing agent with a molar ratio of (1-2.5):1:(0.23-0.4) are mutually soluble and stirred to react, and after the reaction product is cooled to room temperature, the accelerator is added and stirred to obtain an epoxy resin binder.
[0032] Specifically, the diluent, the epoxy resin and the curing agent are mixed in a molar ratio of (1-2.5):1:(0.23-0.4), and stirred and reacted at 50-70°C for 10-20 min, and then the accelerator is added after the reaction product is cooled to room temperature, and stirred for 5-10 min to obtain the epoxy resin binder. The weight of the accelerator accounts for 0.8-1.4% of the total weight of the diluent, the epoxy resin and the curing agent.
[0033] Further, the epoxy resin comprises bisphenol A type epoxy resin, and the epoxy equivalent weight of the bisphenol A type epoxy resin is 185-230 g / mol, and the density is 1.15-1.2 g / cm 3 .
[0034] Specifically, the diluent is obtained by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether in a mass ratio of (4.5-9):1:(0.5-1) at 30-50°C. For example, the stirring time is 15 min.
[0035] Further, the curing agent is obtained by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine in a mass ratio of (6-8):1:(0.5-1.5) at 30-50°C. For example, the stirring time is 20 min.
[0036] Further, the accelerator comprises 1-cyanoethyl-2-ethyl-4-methylimidazole and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:(0.5-0.8).
[0037] Further, the filler comprises modified rubber powder and limestone powder. The rubber powder meets the technical requirements of “Road Waste Tire Vulcanized Rubber Powder (JT / T 797-2011)”, and the limestone powder meets the technical requirements of “Technical Specification for Construction of Highway Asphalt Pavement” (JTG F40-2004). The modified rubber powder is obtained by surface treatment of the rubber powder with a silane coupling agent. The fineness of the rubber powder is 150 mesh, and the addition amount of the silane coupling agent is 0.8% of the mass of the rubber powder. The mass of the modified rubber powder is less than or equal to 20% of the mass of the limestone powder.
[0038] In this embodiment, the curing agent comprises trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine. The mercapto groups in trimethylolpropane tri(3-mercaptopropionate) and pentaerythritol tetra-3-mercaptopropionate provide high crosslinking density, and the flexible ether bond of polyether amine forms an elastic network in the early stage. The two are chemically complementary through sulfide bonds and ether bonds, which not only ensures high temperature strength, but also provides low temperature elasticity.
[0039] In this embodiment, 1-cyanoethyl-2-ethyl-4-methylimidazole is used as an accelerator to synergize with 2, 4, 6-tris(dimethylaminomethyl)phenol to realize staged curing, extend the operable time, and ensure the mechanical stability of the cured material.
[0040] In this embodiment, the delayed curing property of the accelerator 1-cyanoethyl-2-ethyl-4-methylimidazole and the flexibility of the curing agent polyetheramine are matched in time gradient at the initial stage of crosslinking to avoid stress concentration caused by premature crosslinking, and the acceleration of 2, 4, 6-tris(dimethylaminomethyl)phenol is synchronized with the reaction process of the high-activity mercapto curing agent at the later stage of curing to promote the crosslinking reaction together and ensure gradual increase in crosslinking density.
[0041] In this embodiment, 1-cyanoethyl-2-ethyl-4-methylimidazole forms hydrogen bonds with polyetheramine to enhance the interfacial adhesion between the epoxy resin binder and the silanized rubber filler, thereby improving the integrity of the epoxy resin cement.
[0042] S2, the filler and the epoxy resin binder in a mass ratio of (0.7-1.4):1 are stirred to obtain the epoxy resin cement.
[0043] Specifically, at room temperature, the filler and the epoxy resin binder in a mass ratio of (0.7-1.4):1 are first stirred at 300-500 rpm for 300-420 s, and then stirred at 500-1000 rpm for 300-420 s to obtain the epoxy resin cement.
[0044] Further, the epoxy resin cement prepared has a high-elasticity service temperature of greater than or equal to -25℃, a viscosity of 2-30 Pa·s, and a gel time of greater than or equal to 1 h.
[0045] The epoxy resin cement prepared by the preparation method of the epoxy resin cement of this embodiment is prepared by stirring the diluent, the epoxy resin, the curing agent, and the accelerator to obtain the epoxy resin binder, and then stirring the epoxy resin binder and the filler to obtain the epoxy resin cement, which can react at a relatively low temperature and has mild reaction conditions and is easy to shape.
[0046] The epoxy resin cement prepared by the preparation method of this embodiment has good flexibility, is in a stable high-elastic state in a low-temperature and wide-temperature range, has good low-temperature elastic recovery capacity, and has a modulus similar to that of the rubber particles, which can significantly reduce the interfacial stress and improve the overall quality and durability of the rubber elastic pavement; in addition, the adhesion between the epoxy resin cement and the rubber particles is good, which can effectively enhance the durability of the rubber elastic pavement.
[0047] Example Two
[0048] On the basis of the first embodiment, the present embodiment provides an epoxy resin binder for elastic pavement. The epoxy resin binder comprises: fillers and epoxy resin binders in a mass ratio of (0.7-1.4):1; wherein the raw materials of the epoxy resin binder comprise a diluent, an epoxy resin, a curing agent and an accelerator; the molar ratio of the diluent, the epoxy resin and the curing agent is (1-2.5):1:(0.23-0.4); and the weight of the accelerator accounts for 0.8-1.4% of the total weight of the diluent, the epoxy resin and the curing agent.
[0049] Specifically, the epoxy resin comprises bisphenol A type epoxy resin, the epoxy equivalent weight of the bisphenol A type epoxy resin is 185-230 g / mol, and the density is 1.15-1.2 g / cm 3 .
[0050] Specifically, the diluent comprises polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether in a mass ratio of (4.5-9):1:(0.5-1).
[0051] Specifically, the curing agent comprises trimethylolpropane tris(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine in a mass ratio of (6-8):1:(0.5-1.5).
[0052] Specifically, the accelerator comprises 1-cyanoethyl-2-ethyl-4-methylimidazole and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:(0.5-0.8).
[0053] Specifically, the fillers comprise modified rubber powder and limestone powder; wherein the modified rubber powder is obtained by surface treatment of rubber powder with a silane coupling agent; and the mass of the modified rubber powder is less than or equal to 20% of the mass of the limestone powder.
[0054] Specifically, the high-elasticity service temperature of the epoxy resin binder of the present embodiment is greater than or equal to -25℃, the viscosity is 2-30 Pa·s, and the gel time is greater than or equal to 1 h.
[0055] The epoxy resin binder of the present embodiment has good flexibility, is in a stable high-elasticity state in a wide temperature range at low temperature, has good low-temperature elastic recovery capacity, and has a modulus similar to that of rubber particles, which can significantly reduce the interfacial stress and improve the overall quality and durability of the rubber elastic pavement; in addition, the adhesion between the epoxy resin binder and the rubber particles is good, which can effectively enhance the durability of the rubber elastic pavement.
[0056] The epoxy resin binder of the present embodiment has a wide temperature range, suitable viscosity and gel time, and good workability and ease of use.
[0057] Embodiment three
[0058] On the basis of embodiment one and embodiment two, the present embodiment illustrates the epoxy resin binder for elastic pavement and the preparation method by the following examples and comparative examples.
[0059] Example 1
[0060] The diluent is obtained by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40°C for 15 min, the curing agent is obtained by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40°C for 20 min, the accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl) phenol with a mass ratio of 1:0.6, and the filler is composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0061] The diluent, epoxy resin and curing agent are intermiscible with a molar ratio of 1.62:1:0.32, stirred and reacted at 60°C for 10 min, after cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent is added, stirred for 10 min to obtain the epoxy resin binder, and then the filler with a mass ratio of 1.1:1 is stirred with the epoxy resin binder at room temperature at 300 rpm for 300 s, and then at 500 rpm for 300 s to prepare the wide temperature range epoxy resin binder.
[0062] Example 2
[0063] The diluent is obtained by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 4.5:1:1 at 40°C for 15 min, the curing agent is obtained by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 6:1:0.5 at 40°C for 20 min, the accelerator is 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl) phenol with a mass ratio of 1:0.8, and the filler is composed of limestone powder.
[0064] The diluent, epoxy resin and curing agent are intermiscible with a molar ratio of 1:1:0.4, stirred and reacted at 60°C for 10 min, after cooling to room temperature, 1.4% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent is added, stirred for 10 min to obtain the epoxy resin binder, and then the filler with a mass ratio of 1.4:1 is stirred with the epoxy resin binder at room temperature at 300 rpm for 300 s, and then at 500 rpm for 300 s to prepare the wide temperature range epoxy resin binder.
[0065] Example 3
[0066] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 9:1:0.5 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyetheramine with a mass ratio of 9:1:1.5 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.5, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 5:1.
[0067] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 2.5:1:0.23, and stirred at 60 °C for 10 min. After cooling to room temperature, 0.8% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler and the epoxy resin binder with a mass ratio of 0.7:1 were stirred at room temperature at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the wide temperature range epoxy resin adhesive.
[0068] Comparative Example 1
[0069] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 9:1:0.5 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyetheramine with a mass ratio of 9:1:1.5 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0070] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler and the epoxy resin binder with a mass ratio of 1.1:1 were stirred at room temperature at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the wide temperature range epoxy resin adhesive.
[0071] Comparative Example 2
[0072] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was prepared by mixing 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was prepared by mixing limestone powder and 150 mesh silanized rubber powder with a mass ratio of 3:1.
[0073] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was mixed with the epoxy resin binder at room temperature, stirred at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the wide temperature range epoxy resin adhesive.
[0074] Comparative Example 3
[0075] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was prepared by mixing 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was prepared by mixing limestone powder and 150 mesh silanized rubber powder with a mass ratio of 3:1.
[0076] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was mixed with the epoxy resin binder at room temperature, stirred at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the wide temperature range epoxy resin adhesive.
[0077] Comparative Example 4
[0078] The diluent was prepared by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0079] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 4:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler and the epoxy resin binder with a mass ratio of 1.1:1 were stirred at room temperature at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the epoxy resin adhesive with a wide temperature range.
[0080] Comparative Example 5
[0081] The diluent was prepared by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0082] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.15, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler and the epoxy resin binder with a mass ratio of 1.1:1 were stirred at room temperature at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the epoxy resin adhesive with a wide temperature range.
[0083] Comparative Example 6
[0084] The diluent was prepared by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyetheramine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0085] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 3% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was mixed with the epoxy resin binder at room temperature, stirred at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the epoxy resin adhesive with a wide temperature range.
[0086] Comparative Example 7
[0087] The diluent was prepared by stirring the polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring the trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyetheramine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl)phenol with a mass ratio of 1:0.6, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0088] The diluent, epoxy resin and curing agent were mixed with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 3% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain the epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was mixed with the epoxy resin binder at room temperature, stirred at 300 rpm for 300 s, and then stirred at 500 rpm for 300 s to prepare the epoxy resin adhesive with a wide temperature range.
[0089] Comparative Example 8
[0090] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 2,4, 6-tris(dimethylaminomethyl) phenol, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0091] The diluent, epoxy resin and curing agent were intermiscible with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain an epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was stirred with the epoxy resin binder at room temperature at 300 rpm for 300 s, and then at 500 rpm for 300 s to prepare a wide temperature range epoxy resin adhesive.
[0092] Comparative Example 9
[0093] The diluent was prepared by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether with a mass ratio of 8:1:0.8 at 40 °C for 15 min, the curing agent was prepared by stirring trimethylolpropane tri(3-mercaptopropionate), pentaerythritol tetra-3-mercaptopropionate and polyether amine with a mass ratio of 7:1:1 at 40 °C for 20 min, the accelerator was 2,4, 6-tris(dimethylaminomethyl) phenol, and the filler was composed of limestone powder and 150 mesh silanized rubber powder with a mass ratio of 10:1.
[0094] The diluent, epoxy resin and curing agent were intermiscible with a molar ratio of 1.62:1:0.32, and stirred at 60 °C for 10 min. After cooling to room temperature, 1% of the accelerator based on the total weight of the diluent, epoxy resin and curing agent was added, and stirred for 10 min to obtain an epoxy resin binder. Then, the filler with a mass ratio of 1.1:1 was stirred with the epoxy resin binder at room temperature at 300 rpm for 300 s, and then at 500 rpm for 300 s to prepare a wide temperature range epoxy resin adhesive.
[0095] Comparative Example 10
[0096] A commercially available road polyether single-component polyurethane was used as the adhesive.
[0097] According to the preparation methods of Examples 1-3 and Comparative Examples 1-10, 13 groups of epoxy resin adhesive samples were prepared respectively, each group of samples having the same size and shape. The following tests were conducted:
[0098] (1) Using dynamic mechanical analyzer, the dynamic mechanical parameters of the sample were measured to obtain the high-elasticity service temperature range of the sample and the dynamic modulus at 25°C.
[0099] (2) According to GB / T 5210-2006 "Paints and Varnishes Adhesion by Tearing", the adhesive and rubber 25°C adhesion test was performed on the sample, and the tensile strength of the sample was recorded.
[0100] (3) According to GB / T 1681-2009 "Determination of Resilience of Vulcanized Rubber", the sample was tested for resilience at 25°C, and the resilience value of the test was recorded.
[0101] (4) The test rotational viscosity at 25°C was tested by a rotational viscometer, and the corresponding viscosity value was recorded.
[0102] (5) The isothermal curing test of the sample at 25°C was performed by a differential scanning calorimeter, and the corresponding gel time was recorded.
[0103] The results are shown in Table 1:
[0104] Table 1 Performance test results of wide temperature range epoxy resin adhesive
[0105]
[0106] From the results of Table 1, it can be seen that Comparative Example 1, which only uses polypropylene glycol diglycidyl ether as a diluent, has a significantly reduced tensile strength and dynamic modulus, because the long-chain ether bond of polypropylene glycol diglycidyl ether has a high molecular chain flexibility, which reduces the crosslinking density of the cement. Comparative Example 2, which only uses pentaerythritol tetra-3-mercaptopropionate curing agent, has a significantly reduced high-elasticity service temperature range, reduced resilience and gel time, and increased strength, because the four-mercapto structure of pentaerythritol tetra-3-mercaptopropionate provides a high crosslinking density, indicating that the flexible amine group is indispensable. Comparative Example 3 uses rubber powder filler that exceeds the proportion limit, resulting in a cement with too high viscosity, which is difficult to mix. Comparative Example 4 uses an excessive amount of diluent, resulting in a cement with reduced viscosity and a significantly increased gel time, which is prone to segregation. Comparative Example 5 uses an insufficient amount of curing agent, resulting in an incomplete reaction and an inability to form a uniform cement. Comparative Example 6 uses an excessive amount of accelerator, resulting in a reaction that proceeds too quickly and does not have sufficient construction time. Comparative Example 7 only uses phenyl glycidyl ether diluent, resulting in a cement with significantly reduced viscosity and a tendency to segregate. Comparative Example 8 only uses 2, 4, 6-tris(dimethylaminomethyl) phenol as an accelerator, resulting in a significant decrease in gel time, indicating that 1-cyanoethyl-2-ethyl-4-methylimidazole and 2, 4, 6-tris(dimethylaminomethyl) phenol have a synergistic effect on construction time. Comparative Example 9 uses rubber powder that has not been treated with a silane coupling agent as a filler, resulting in a significant decrease in overall mechanical properties. Comparative Example 10 is a road polyurethane binder, and in comparison, Examples 1-3 have a wider high-elasticity service temperature range and better adhesion between rubber particles, while ensuring dynamic modulus and resilience properties that match those of rubber, and have good construction and workability.
[0107] In summary, the wide-temperature-range epoxy resin cement of the present embodiment has good adhesion to both rubber and stone, and has a road service temperature range that is highly matched to the mechanical properties of rubber aggregate, thereby improving the durability of the rubber elastic road surface.
[0108] The above is a further detailed description of the present application in conjunction with specific preferred embodiments, and the specific implementation of the present application should not be limited to these descriptions. For ordinary skilled persons in the technical field to which the present application belongs, without departing from the concept of the present application, a number of simple deductions or substitutions can be made, which should be considered within the scope of protection of the present application.
Claims
1. A method for preparing an epoxy resin binder for elastic pavements, characterized in that, Including the following steps: S1. A diluent, epoxy resin, and curing agent in a molar ratio of (1~2.5):1:(0.23~0.4) are miscible and stirred to react. After the reactants are cooled to room temperature, an accelerator is added and stirred to obtain an epoxy resin binder. The epoxy resin includes bisphenol A type epoxy resin. The weight of the accelerator accounts for 0.8~1.4% of the sum of the weights of the diluent, epoxy resin, and curing agent. The diluent includes polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether, and phenyl glycidyl ether in a mass ratio of (4.5~9):1:(0.5~1). The curing agent includes trimethylolpropane tris(3-mercaptopropionic acid), pentaerythritol tetra-3-mercaptopropionate, and polyetheramine in a mass ratio of (6~8):1:(0.5~1.5). The accelerator includes a mixture in a mass ratio of 1: (0.5~0.8) of 1-cyanoethyl-2-ethyl-4-methylimidazol and 2,4,6-tris(dimethylaminomethyl)phenol; S2. Stir the filler and the epoxy resin binder at a mass ratio of (0.7~1.4):1 to obtain an epoxy resin binder; the filler includes modified rubber powder and limestone powder, the modified rubber powder is obtained by surface treatment of the rubber powder with a silane coupling agent, and the mass of the modified rubber powder is less than or equal to 20% of the mass of the limestone powder.
2. The method for preparing epoxy resin binder for elastic pavement according to claim 1, characterized in that, The bisphenol A type epoxy resin has an epoxy equivalent of 185~230 g / mol and a density of 1.15~1.2 g / cm³. 3 .
3. The method for preparing epoxy resin binder for elastic pavement according to claim 1, characterized in that, The diluent is obtained by stirring polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether at 30-50°C.
4. The method for preparing the epoxy resin binder for elastic pavement according to claim 1, characterized in that, The curing agent is obtained by stirring trimethylolpropane tris(3-mercaptopropionic acid), pentaerythritol tetra-3-mercaptopropionic acid ester and polyetheramine at 30~50°C.
5. The method for preparing epoxy resin binder for elastic pavement according to claim 1, characterized in that, Step S1 includes: The diluent, epoxy resin and curing agent are mixed in a molar ratio of (1~2.5):1:(0.23~0.4) and stirred at 50~70°C for 10~20 min. After the reactants are cooled to room temperature, the accelerator is added and stirred for 5~10 min to obtain epoxy resin binder.
6. The method for preparing epoxy resin binder for elastic pavement according to claim 1, characterized in that, Step S2 includes: At room temperature, the filler and the epoxy resin binder with a mass ratio of (0.7~1.4):1 are first stirred at 300~500 rpm for 300~420 s, and then stirred at 500~1000 rpm for 300~420 s to obtain the epoxy resin binder.
7. An epoxy resin binder for elastic pavements, characterized in that, include: A filler and epoxy resin binder with a mass ratio of (0.7~1.4):1, wherein, The raw materials of the epoxy resin binder include diluent, epoxy resin, curing agent and accelerator; The diluent comprises polypropylene glycol diglycidyl ether, 1,4-butanediol diglycidyl ether and phenyl glycidyl ether in a mass ratio of (4.5~9):1:(0.5~1); The epoxy resin includes bisphenol A type epoxy resin; The curing agent comprises trimethylolpropane tris(3-mercaptopropionic acid), pentaerythritol tetra-3-mercaptopropionic acid ester, and polyetheramine in a mass ratio of (6~8):1:(0.5~1.5); The accelerator comprises 1-cyanoethyl-2-ethyl-4-methylimidazol and 2,4,6-tris(dimethylaminomethyl)phenol in a mass ratio of 1:(0.5~0.8). The molar ratio of the diluent, the epoxy resin, and the curing agent is (1~2.5):1:(0.23~0.4). The accelerator accounts for 0.8 to 1.4% of the total weight of the diluent, the epoxy resin, and the curing agent. The filler includes modified rubber powder and limestone powder. The modified rubber powder is obtained by surface treatment of the rubber powder with a silane coupling agent. The mass of the modified rubber powder is less than or equal to 20% of the mass of the limestone powder.
8. The epoxy resin binder for elastic pavement according to claim 7, characterized in that, The epoxy resin binder has a high elasticity service temperature greater than or equal to -25℃, a viscosity of 2~30 Pa·s, and a gel time greater than or equal to 1h.
Citation Information
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