Epoxy modified colored asphalt material and preparation method thereof

By adding specific components to the epoxidized petroleum resin solution for chemical grafting and esterification, a long, durable, high-flexible, crack-resistant epoxy modified color asphalt material was prepared, which solved the problems of poor low temperature and insufficient weather resistance of existing cementitious materials, and achieved efficient improvement in the performance of color asphalt materials.

CN119735913APending Publication Date: 2025-04-01江苏创为交通科技发展有限公司
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Patent Information

Application Number
CN202411981863.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-12-31
Publication Date
2025-04-01

AI Technical Summary

Technical Problem

The existing cements for colored pavement have problems such as poor low temperature flexibility, easy cracking, and poor weather resistance, which limits its application range and life.

Method used

By adding end-hydroxy long-chain silicone oil, PH regulator, end-polyol colorant, isocyanate, catalyst, epoxy resin and epoxy curing agent to the epoxidized petroleum resin solution, chemical grafting and esterification reactions, a long-durable, high-flexible, crack-resistant epoxy modified color asphalt material was prepared.

Benefits of technology

The material has high and low temperature properties, high flexibility, crack resistance, long durability and strong bonding properties, which significantly improves the weather resistance and service life of colored asphalt.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses an epoxy modified colored asphalt material and a preparation method thereof. The epoxy modified colored asphalt material comprises the following raw materials in parts by weight: 100 parts of petroleum resin, 30-33 parts of hydroxyl-terminated long-chain silicone oil, 4-8 parts of an oxidizing agent, 6-9 parts of diol amine, 1-3 parts of a pH regulator, 5 parts of a solvent, 100 parts of normal hexane, 6-9 parts of a coloring agent, 6-9 parts of isocyanate, 1-3 parts of a catalyst, 26-28 parts of epoxy resin and 10-12 parts of an epoxy curing agent. The epoxy modified colored asphalt material prepared by the method disclosed by the invention has high and low temperature performance, high flexibility, cracking resistance, long durability and strong adhesion.
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Description

Technical Field

[0001] The invention relates to the field of road paving, in particular to an epoxy modified colored asphalt material and a preparation method thereof. Background Art

[0002] Colored pavement has the advantages of diverting traffic, providing visual warnings, and reducing the risk of fatigue driving. It is often paved in special areas such as service areas, toll stations, and bus ports. Common binders for colored pavements include decolorized asphalt, light-colored binding binders, epoxy resins, polyurethanes, acrylic resins, etc.

[0003] Decolorized asphalt is generally washed with acid to remove the colored components in the asphalt, leaving behind lighter components with high adhesion to asphalt pavements. However, the preparation process is complex, the price is expensive, and it pollutes the environment, so it is gradually being eliminated. Light-colored bonding binders are made of lightweight resins represented by petroleum resins, aromatic oils, polymers and additives. They have the advantages of wide sources, diverse types, low prices, and high adhesion to asphalt pavements, and are widely used. However, they also have problems such as poor low-temperature flexibility, easy cracking, poor weather resistance, and easy aging. Epoxy resins, polyurethanes, and acrylic resins are mostly modified resin materials with the advantages of high cohesive strength, good toughness, and strong adhesion to the base surface. However, the high price of resins limits the promotion of such materials. Some industry insiders also reduce costs by adding inorganic fillers, but this is often accompanied by problems such as brittleness and easy cracking.

[0004] In view of the above-mentioned problems existing in the existing colored pavement binders, the inventors, based on their rich experience and professional knowledge in such structures and materials for many years, combined with theoretical analysis, conducted research and innovation, and developed a long-lasting, highly flexible and crack-resistant epoxy-modified colored asphalt material and a preparation method thereof. Summary of the invention

[0005] In view of the problems existing in the above-mentioned background technology, the present invention provides a long-lasting, highly flexible and crack-resistant epoxy-modified colored asphalt material and a preparation method thereof. The epoxy-modified colored asphalt has both high and low temperature performance, high flexibility, crack resistance, long durability and strong adhesion.

[0006] In order to achieve the above object, the present invention specifically adopts the following technical solutions:

[0007] An epoxy modified colored asphalt material is obtained by sequentially adding hydroxyl-terminated long-chain silicone oil, a pH regulator, a terminal polyol colorant, an isocyanate, a catalyst, an epoxy resin, and an epoxy curing agent to an epoxidized petroleum resin solution; the terminal polyol colorant is obtained by dissolving a colorant in a solvent, adding a diol amine and a pH regulator, and then reacting; the epoxidized petroleum resin solution is obtained by dissolving a petroleum resin in n-hexane, and then adding an oxidant to react;

[0008] The weight parts of the above raw material components are as follows:

[0009]

[0010] Furthermore, the petroleum resin of the present invention is any one of common C5 petroleum resin and C9 petroleum resin or a mixture of more than one of them.

[0011] Furthermore, the terminal hydroxyl long-chain silicone oil described in the present invention is a linear long-chain silicone oil with a functionality of 2 and a weight-average molecular weight ≥2000, specifically selected from any one of double-terminal alcohol hydroxyl long-chain alkyl silicone oil, double-terminal alcohol hydroxyl silicone oil, and hydroxyl-terminated methyl vinyl silicone oil or a mixture of more than one thereof; the grafted long-chain linear silicone oil can greatly improve the low-temperature flexibility of petroleum resin and effectively prevent low-temperature cracking.

[0012] Furthermore, the oxidant of the present invention is an acidic peroxide selected from any one of meta-chloroperbenzoic acid, peracetic acid, and hydrogen peroxide; the acidic peroxide introduces epoxy groups into the petroleum resin structure, which facilitates the subsequent grafting of linear silicone oil through esterification reaction to modify the flexibility of the petroleum resin.

[0013] Furthermore, the diolamine described in the present invention is one of hydroxyalkyl substituents such as diethanolamine and dipropanolamine; it reacts with silicone oil and colorant to generate polyurethane groups, thereby improving the toughness and weather resistance of asphalt, changing the color of asphalt, and subsequently grafting epoxy resin.

[0014] Furthermore, the pH regulator of the present invention is aqueous ammonia.

[0015] Furthermore, the solvent of the present invention is selected from any one of dichloromethane, N,N-dimethylacetamide and dichloroethane.

[0016] Furthermore, the present invention adopts n-hexane solvent to reduce the viscosity of petroleum resin and the difficulty of operation, and it will be removed in the subsequent synthesis steps.

[0017] Furthermore, the colorant described in the present invention is one of the acidic colorants, such as red and yellow pigments are azo-type acidic colorants, and blue pigments are ricinol-type acidic colorants; the acidic colorant can react chemically with diolamines, and the produced terminal polyol colorant can be grafted onto the molecular structure of petroleum resin, making the coloring more uniform, stable and durable.

[0018] Furthermore, the isocyanate of the present invention is selected from any one of MDI, TDI, IPDI or a mixture of more than one thereof, and the NCO group reacts with the hydroxyl groups on the long-chain polyol and the epoxy resin to form a long-chain polyurethane group, which effectively improves the flexibility and weather resistance of the petroleum resin.

[0019] Furthermore, the catalyst of the present invention is any one of T9 and T12.

[0020] Furthermore, the epoxy resin described in the present invention is a bisphenol A epoxy resin, selected from any one of E44, E51, and E20; the grafted epoxy resin can enhance the high temperature, weather resistance, and adhesion properties of the petroleum resin, reduce the risk of road cracking, and resist seepage and water.

[0021] Furthermore, the epoxy curing agent described in the present invention is a long-chain fatty amine curing agent, which is selected from any one of oleylamine, dodecylamine, and hexadecylamine; the long-chain fatty amine reacts with the epoxy group to transform the petroleum resin from thermoplastic to thermosetting, greatly improving the mechanical properties and weather resistance of the colored asphalt.

[0022] Furthermore, the present invention also provides a method for preparing the above-mentioned long-lasting, highly flexible and crack-resistant epoxy-modified colored asphalt material, comprising:

[0023] First, a colorant is dissolved in a solvent, and a diol amine and a pH regulator are added to react to obtain a terminal polyol colorant; petroleum resin is dissolved in n-hexane, and an oxidant is added to react to obtain an epoxidized petroleum resin solution; then, terminal hydroxyl long-chain silicone oil and a pH regulator are added to the epoxidized petroleum resin solution to react to obtain a petroleum resin solution of partially hydroxyl-terminated grafted long-chain silicone oil, and the above-mentioned terminal polyol colorant and pH regulator are added to the petroleum resin solution to react to obtain a terminal hydroxyl colored petroleum resin solution; finally, isocyanate, a catalyst, an epoxy resin, and an epoxy curing agent are added in sequence to react to obtain the epoxy-modified colored asphalt material of the present invention.

[0024] Furthermore, the present invention also provides a specific preparation method of the above-mentioned long-lasting, highly flexible and crack-resistant epoxy-modified colored asphalt material, comprising the following steps:

[0025] (1) Preparation of terminal polyol colorant: In a four-necked flask equipped with a condenser reflux tube and a stirrer, add a colorant and a solvent, stir for 30-40 minutes, add diol amine, adjust the pH to 10 with a pH regulator, heat to 40-50° C., react at constant temperature for 10 hours, extract and remove the water generated by the reaction, and filter to obtain the terminal polyol colorant;

[0026] (2) Preparation of epoxidized petroleum resin solution: Add petroleum resin and n-hexane into a four-necked flask equipped with a condenser reflux tube and a stirrer, stir at 70-80°C for 30-40 minutes to fully dissolve the petroleum resin, then cool to 40-50°C, add an oxidant, and react at a constant temperature for 3-4 hours to obtain an epoxidized petroleum resin solution;

[0027] (3) Preparation of a petroleum resin solution grafted with long-chain silicone oil: heating the epoxidized petroleum resin solution obtained in step (2) to 80-90° C., adding the hydroxyl-terminated long-chain silicone oil, and then adding a pH regulator to adjust the pH to 10, and reacting at a constant temperature for 4-5 hours to obtain a petroleum resin solution grafted with a partially hydroxyl-terminated long-chain silicone oil;

[0028] (4) Preparation of a hydroxyl-terminated colored petroleum resin solution: The product obtained in step (3) is heated to 80-90° C., and the polyol-terminated colorant obtained in step (1) is added thereto, and the pH is adjusted to 10 using a pH regulator, and the reaction is carried out at a constant temperature for 4-5 hours to obtain a hydroxyl-terminated colored petroleum resin solution;

[0029] (5) Preparation of terminal NCO-modified petroleum resin solution: heating the terminal hydroxyl colored petroleum resin solution obtained in step (4) to 60-70° C., adding isocyanate and catalyst in sequence, and reacting at a constant temperature for 2-3 hours to obtain a terminal NCO-modified petroleum resin solution;

[0030] (6) Preparation of colored petroleum resin: heating the NCO-modified petroleum resin solution obtained in step (5) to 60-80° C., adding epoxy resin and reacting at constant temperature for 4-5 hours, removing the solvent, and obtaining a colored petroleum resin end-capped with epoxy resin;

[0031] (7) Preparation of epoxy-modified colored asphalt material: The colored petroleum resin obtained in step (6) is heated to 160° C. and then mixed with an epoxy curing agent in a certain proportion to obtain the epoxy-modified colored asphalt material of the present invention.

[0032] Compared with the prior art, the present invention has the following beneficial effects:

[0033] (1) The preparation of colored asphalt is achieved by introducing colorants onto petroleum resin through the method of chemical grafting. Compared with the mechanical mixing of colorants, the chemical grafting of colorants has more stable colors and better weather resistance to ultraviolet rays, water, solvents, etc. At the same time, the prepared colored asphalt has more uniform color and is less prone to color difference.

[0034] (2) By introducing high molecular weight, long chain linear silicone oil into the petroleum resin structure, on the one hand, it can chemically bond with the silicon-oxygen bonds on the surface of the stone used in the paving process of the colored pavement, greatly improving the adhesion of the colored asphalt to the stone, effectively resisting peeling and cracking, and improving the flame retardant properties of the colored asphalt; on the other hand, the long chain linear high molecular weight silicone oil can effectively improve the low temperature flexibility of the petroleum resin, effectively inhibit the occurrence of cracking problems during the use of the colored pavement in winter, and provide active groups for the grafted epoxy resin structure.

[0035] (3) The epoxy resin is grafted onto the end of the petroleum resin and reacts with fatty amines to solidify, transforming the colored asphalt from a thermoplastic material into a thermosetting material, effectively improving the colored asphalt's resistance to high temperatures, UV rays, acids, alkalis, and discoloration. At the same time, the epoxy resin effectively improves the wear resistance and bonding properties of the colored asphalt, resists driving wear, and prevents discoloration. In addition, both epoxy resin and petroleum resin contain structures such as benzene rings and long carbon chains, have similar structures, good compatibility, and are easy to process. DETAILED DESCRIPTION

[0036] The above contents are combined with the following embodiments to further illustrate the present invention.

[0037] The sources of the components in the embodiments and comparative examples of the present invention are shown in Table 1.

[0038] Table 1 Component sources

[0039]

[0040] Example 1

[0041] The invention discloses an epoxy modified colored asphalt material, wherein the raw materials include the following components: acid blue black 10B, N,N-dimethylacetamide, diethanolamine, C5 resin, meta-chloroperbenzoic acid, double-end alcohol hydroxyl long-chain alkyl silicone oil, MDI, T9 catalyst, epoxy resin E51, and long-chain amine curing agent oleylamine.

[0042] A method for preparing an epoxy-modified colored asphalt material comprises the following steps:

[0043] (1) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 7 parts of acid blue black 10B and 5 parts of N,N-dimethylacetamide, stir for 35 minutes, gradually add 8 parts of diethanolamine, adjust the pH to 10 with ammonia water, heat to 45°C, react at constant temperature for 10 hours, remove the water generated by the reaction, filter and wash to obtain a terminal polyol colorant;

[0044] (2) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 100 parts of C5 petroleum resin and 100 parts of n-hexane, stir at 75°C for 35 minutes to fully dissolve the petroleum resin, cool to 45°C, add 8 parts of m-chloroperbenzoic acid, and react at a constant temperature for 3.5 hours to obtain an epoxidized petroleum resin solution;

[0045] (3) 100 parts of the modified petroleum resin solution were heated to 85° C., 31 parts of double-terminated hydroxyl long-chain alkyl silicone oil were added, ammonia water was added to adjust the pH to 10, and the reaction was carried out at a constant temperature for 4.5 hours to obtain a petroleum resin solution with a partial hydroxyl-terminated grafted long-chain silicone oil;

[0046] (4) heating 131 parts of the product of step (3) to 85° C., adding 15 parts of a terminal polyol colorant, adjusting the pH to 10, and reacting at a constant temperature for 4.5 hours to obtain a terminal hydroxyl colored petroleum resin solution;

[0047] (5) heating 146 parts of the petroleum resin solution prepared in step (4) to 65° C., adding 7 parts of MDI and 2 parts of T9 catalyst, and reacting at a constant temperature for 2.5 hours to obtain a terminal NCO-modified petroleum resin solution;

[0048] (6) 153 parts of the petroleum resin solution of step (5) were heated to 70° C., 27 parts of E51 epoxy resin were added, and the mixture was reacted at a constant temperature for 4.5 hours, and the solvent was removed to obtain a colored petroleum resin with epoxy-terminated grafted epoxy resin;

[0049] (7) The colored asphalt is heated to 160° C., and the mixture is cured and cured at a ratio of colored asphalt to oleylamine of 100:11 to obtain a modified colored asphalt sample for road surface.

[0050] Example 2

[0051] The invention discloses an epoxy modified colored asphalt material, wherein the raw materials include the following components: 1,2-hydroxyanthraquinone, ethylene dichloride, diethanolamine, C5 resin, meta-chloroperbenzoic acid, double-end alcohol hydroxyl long-chain alkyl silicone oil, MDI, T9 catalyst, epoxy resin E51, and long-chain amine curing agent oleylamine.

[0052] A method for preparing an epoxy-modified colored asphalt material comprises the following steps:

[0053] (1) In a four-necked flask equipped with a condenser reflux tube and a stirrer, 9 parts of 1,2-hydroxyanthraquinone and 5 parts of dichloroethane were added, stirred for 35 minutes, 6 parts of diethanolamine were gradually added, the pH was adjusted to 10 with ammonia water, the temperature was raised to 45° C., the reaction was carried out at a constant temperature for 10 hours, the water generated by the reaction was removed, and the terminal polyol colorant was obtained by filtering and washing;

[0054] (2) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 100 parts of C5 petroleum resin and 100 parts of n-hexane, stir at 80°C for 30 minutes to fully dissolve the petroleum resin, cool to 40°C, add 5 parts of m-chloroperbenzoic acid, and react at constant temperature for 4 hours to obtain an epoxidized petroleum resin solution;

[0055] (3) 100 parts of the modified petroleum resin solution were heated to 90° C., 33 parts of double-terminated alcohol hydroxyl long-chain alkyl silicone oil were added, ammonia water was added to adjust the pH to 10, and the reaction was carried out at a constant temperature for 4 hours to obtain a petroleum resin solution with a partial hydroxyl-terminated grafted long-chain silicone oil;

[0056] (4) heating 133 parts of the product of step (3) to 80° C., adding 15 parts of a terminal polyol colorant, adjusting the pH to 10, and reacting at a constant temperature for 5 hours to obtain a terminal hydroxyl colored petroleum resin solution;

[0057] (5) heating 148 parts of the petroleum resin solution prepared in step (4) to 60° C., adding 9 parts of MDI and 3 parts of T9 catalyst, and reacting at a constant temperature for 3 hours to obtain a terminal NCO-modified petroleum resin solution;

[0058] (6) 157 parts of the petroleum resin solution of step (5) were heated to 70° C., 26 parts of E51 epoxy resin were added, and the mixture was reacted at a constant temperature for 4.5 hours, and the solvent was removed to obtain a colored petroleum resin with epoxy-terminated grafted epoxy resin;

[0059] (7) The colored asphalt is heated to 160° C., and the mixture is cured and cured at a ratio of colored asphalt to oleylamine of 100:10 to obtain a modified colored asphalt sample for road surface.

[0060] Example 3

[0061] Disclosed is an epoxy modified colored asphalt material, wherein the raw materials include the following components: pigment yellow 38, N,N-dimethylacetamide, dipropanolamine, C9 resin, peracetic acid, double-terminal alcohol hydroxy silicone oil, TDI, T9 catalyst, epoxy resin E51, and long-chain amine curing agent dodecylamine.

[0062] A method for preparing an epoxy-modified colored asphalt material comprises the following steps:

[0063] (1) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 8 parts of Pigment Yellow 38 and 5 parts of N,N-dimethylacetamide, stir for 40 minutes, gradually add 7 parts of diethanolamine, adjust the pH to 10 with ammonia water, heat to 40°C, react at constant temperature for 10 hours, remove the water generated by the reaction, filter and wash to obtain a terminal polyol colorant;

[0064] (2) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 100 parts of C9 petroleum resin and 100 parts of n-hexane, stir at 70°C for 40 minutes to fully dissolve the petroleum resin, cool to 50°C, add 5 parts of peracetic acid, and react at constant temperature for 3 hours to obtain an epoxidized petroleum resin solution;

[0065] (3) 100 parts of the modified petroleum resin solution were heated to 80° C., 32 parts of double-terminated alcohol hydroxy silicone oil were added, ammonia water was added to adjust the pH to 10, and the reaction was carried out at a constant temperature for 5 hours to obtain a petroleum resin solution with a partial hydroxyl-terminated grafted long-chain silicone oil;

[0066] (4) heating 132 parts of the product of step (3) to 90° C., adding 15 parts of a terminal polyol colorant, adjusting the pH to 10, and reacting at a constant temperature for 4 hours to obtain a terminal hydroxyl colored petroleum resin solution;

[0067] (5) heating 147 parts of the petroleum resin solution prepared in step (4) to 65° C., adding 8 parts of TDI and 2 parts of T9 catalyst, and reacting at a constant temperature for 2.5 hours to obtain a terminal NCO-modified petroleum resin solution;

[0068] (6) 155 parts of the petroleum resin solution of step (5) were heated to 60° C., 26 parts of E51 epoxy resin were added, and the mixture was reacted at a constant temperature for 5 hours, and the solvent was removed to obtain a colored petroleum resin with epoxy-terminated grafted epoxy resin;

[0069] (7) The colored asphalt is heated to 160° C., and the mixture is cured and cured at a ratio of colored asphalt to dodecylamine of 100:11 to obtain a modified colored asphalt sample for road surface.

[0070] Example 4

[0071] The invention discloses an epoxy modified colored asphalt material, wherein the raw materials include the following components: 1,2-hydroxyanthraquinone, dichloromethane, dipropanolamine, C9 resin, hydrogen peroxide, hydroxyl-terminated methyl vinyl silicone oil, IPDI, T12 catalyst, epoxy resin E44, and long-chain amine curing agent hexadecylamine.

[0072] A method for preparing an epoxy-modified colored asphalt material comprises the following steps:

[0073] (1) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 6 parts of 1,2-hydroxyanthraquinone and 5 parts of dichloromethane, stir for 30 minutes, gradually add 9 parts of dipropanolamine, adjust the pH to 10 with ammonia water, heat to 50° C., react at constant temperature for 10 hours, remove the water generated by the reaction, filter and wash to obtain a terminal polyol colorant;

[0074] (2) In a four-necked flask equipped with a condenser reflux tube and a stirrer, add 100 parts of C9 petroleum resin and 100 parts of n-hexane, stir at 75°C for 35 minutes to fully dissolve the petroleum resin, cool to 45°C, add 7 parts of hydrogen peroxide, and react at constant temperature for 3.5 hours to obtain an epoxidized petroleum resin solution;

[0075] (3) 100 parts of the modified petroleum resin solution were heated to 85° C., 30 parts of hydroxyl-terminated methyl vinyl silicone oil were added, ammonia water was added to adjust the pH to 10, and the reaction was carried out at a constant temperature for 4.5 hours to obtain a petroleum resin solution partially end-capped with hydroxyl-grafted long-chain silicone oil;

[0076] (4) heating 130 parts of the product of step (3) to 85° C., adding 15 parts of a terminal polyol colorant, adjusting the pH to 10, and reacting at a constant temperature for 4.5 hours to obtain a terminal hydroxyl colored petroleum resin solution;

[0077] (5) heating 145 parts of the petroleum resin solution prepared in step (4) to 70° C., adding 6 parts of IPDI and 1 part of T12 catalyst, and reacting at a constant temperature for 2 hours to obtain a terminal NCO-modified petroleum resin solution;

[0078] (6) 151 parts of the petroleum resin solution of step (5) were heated to 80° C., 28 parts of E44 epoxy resin were added, and the mixture was reacted at a constant temperature for 4 hours, and the solvent was removed to obtain a colored petroleum resin with epoxy-terminated grafted epoxy resin;

[0079] (7) The colored asphalt is heated to 160° C., and the mixture is cured and cured at a ratio of colored asphalt to hexadecylamine of 100:12 to obtain a modified colored asphalt sample for road surface.

[0080] Comparative Example 1

[0081] The difference between Comparative Example 1 and Example 1 is that the raw material of the epoxy modified asphalt in Comparative Example 1 is not grafted with a colorant, and the colorant is directly physically mixed with the modified asphalt.

[0082] Comparative Example 2

[0083] The difference between Comparative Example 2 and Example 1 is that the raw material of the epoxy modified asphalt in Comparative Example 1 does not contain terminal hydroxyl long-chain silicone oil.

[0084] Comparative Example 3

[0085] The difference between Comparative Example 3 and Example 1 is that the raw material of the epoxy-modified asphalt in Comparative Example 1 does not contain bisphenol A epoxy resin.

[0086] Comparative Example 4

[0087] The difference between Comparative Example 4 and Example 1 is that the final product of the epoxy modified asphalt in Comparative Example 1 is not cured with fatty amine.

[0088] Test standard:

[0089] The specific test items and test standards are as follows: acid and alkali resistance refer to GB / T 9756-2018; wear resistance refer to GB / T9756-2018; elongation at break and tensile strength refer to GB / T_1040.1-2018; asphalt aging refer to JTG / E20-2011; adhesion test method refer to GB / T16777-2008; low temperature performance refer to GB 18242-2008. Table 2 shows the performance tests of various embodiments and comparative examples.

[0090] Table 2 Performance test of modified asphalt materials in various embodiments and comparative examples

[0091]

[0092] From the data in Table 2, we can find that:

[0093] The epoxy modified colored asphalt prepared in Examples 1-4 of the present invention has a tensile strength and elongation of 2.1-2.7 MPa and 215-289% before aging, respectively. After aging, the tensile strength and elongation both decrease, but not significantly, and the tensile strength and elongation are between 1.8-2.2 MPa and 200-258%, respectively.

[0094] Compared with Example 1, the colorant in Example 1 is not grafted, but is added by physical mixing. The color asphalt is not resistant to acid and alkali, abrasion, and weather resistance.

[0095] Compared with Example 1, Comparative Example 2 was not grafted with long-chain silicone oil, and cracking occurred during the low-temperature test.

[0096] Compared with Example 1, Comparative Example 3 is not grafted with epoxy resin, has too high reaction activity, is directly cured, cannot be formed, and is not feasible.

[0097] Compared with Example 1, no curing agent was added in Comparative Example 4, and the colored asphalt finally still existed in the form of a thermoplastic, and its performance was much worse than that of a thermoplastic.

[0098] The amount of the long-chain silicone oil, epoxy resin, colorant, fatty amine curing agent and each component of the present invention is controlled within the above range, which helps to color the colored asphalt, improve the anti-discoloration ability of the colored asphalt, improve the weather resistance of the colored asphalt, and extend the service life of the asphalt, thereby increasing the service life of the colored asphalt in special areas such as service areas, toll stations, and bus ports.

[0099] 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. An epoxy modified colored asphalt material, characterized in that: The method is obtained by sequentially adding hydroxyl-terminated long-chain silicone oil, pH regulator, terminal polyol colorant, isocyanate, catalyst, epoxy resin and epoxy curing agent to an epoxidized petroleum resin solution for reaction; the terminal polyol colorant is obtained by dissolving the colorant in a solvent, adding diolamine and pH regulator, and then reacting; the epoxidized petroleum resin solution is obtained by dissolving the petroleum resin in n-hexane, adding an oxidant and reacting; The weight parts of the above raw material components are as follows: The terminal hydroxyl long-chain silicone oil is a linear long-chain silicone oil with a functionality of 2 and a weight average molecular weight ≥ 2000; The oxidant is an acidic peroxide; The epoxy resin is bisphenol A epoxy resin; The epoxy curing agent is a long-chain fatty amine curing agent.

2. The epoxy modified colored asphalt material according to claim 1, characterized in that: The petroleum resin is selected from any one of C5 petroleum resin and C9 petroleum resin or a mixture of more than one of them.

3. The epoxy modified colored asphalt material according to claim 1, characterized in that: The terminal hydroxyl long-chain silicone oil is selected from any one of double-terminal alcohol hydroxyl long-chain alkyl silicone oil, double-terminal alcohol hydroxyl silicone oil, and hydroxyl-terminated methyl vinyl silicone oil, or a mixture of more than one of them.

4. The epoxy modified colored asphalt material according to claim 1, characterized in that: The oxidant is selected from any one of meta-chloroperbenzoic acid, peracetic acid and hydrogen peroxide.

5. The epoxy modified colored asphalt material according to claim 1, characterized in that: The diolamine is any one of diethanolamine and dipropanolamine.

6. The epoxy modified colored asphalt material according to claim 1, characterized in that: The colorant is one of the acidic colorants, wherein the red and yellow pigments are azo-type acidic colorants, and the blue pigment is aricinol-type acidic colorant.

7. The epoxy modified colored asphalt material according to claim 1, characterized in that: The isocyanate is selected from any one of MDI, TDI, and IPDI or a mixture of more than one; The epoxy resin is selected from any one of E44, E51, and E20; The epoxy curing agent is selected from any one of oleylamine, dodecylamine and hexadecylamine.

8. The epoxy modified colored asphalt material according to claim 1, characterized in that: The catalyst is any one of T9 and T12; The solvent is selected from any one of dichloromethane, N,N-dimethylacetamide and dichloroethane; The pH regulator is aqueous ammonia.

9. A method for preparing the epoxy-modified colored asphalt material according to any one of claims 1 to 8, characterized in that: include: First, a colorant is dissolved in a solvent, and a diol amine and a pH regulator are added to react to obtain a terminal polyol colorant; petroleum resin is dissolved in n-hexane, and an oxidant is added to react to obtain an epoxidized petroleum resin solution; then, terminal hydroxyl long-chain silicone oil and a pH regulator are added to the epoxidized petroleum resin solution to react to obtain a petroleum resin solution of partially hydroxyl-terminated grafted long-chain silicone oil, and the above-mentioned terminal polyol colorant and pH regulator are added to the petroleum resin solution to react to obtain a terminal hydroxyl colored petroleum resin solution; finally, isocyanate, a catalyst, an epoxy resin, and an epoxy curing agent are added in sequence to react to obtain the epoxy-modified colored asphalt material.

10. The method for preparing the epoxy modified colored asphalt material according to claim 9, characterized in that: The specific steps include: (1) Preparation of terminal polyol colorant: In a four-necked flask equipped with a condenser reflux tube and a stirrer, add a colorant and a solvent, stir for 30-40 minutes, add diol amine, adjust the pH to 10 with a pH regulator, heat to 40-50° C., react at constant temperature for 10 hours, extract and remove the water generated by the reaction, and filter to obtain the terminal polyol colorant; (2) Preparation of epoxidized petroleum resin solution: Add petroleum resin and n-hexane into a four-necked flask equipped with a condenser reflux tube and a stirrer, stir at 70-80°C for 30-40 minutes to fully dissolve the petroleum resin, then cool to 40-50°C, add an oxidant, and react at a constant temperature for 3-4 hours to obtain an epoxidized petroleum resin solution; (3) Preparation of a petroleum resin solution grafted with long-chain silicone oil: heating the epoxidized petroleum resin solution obtained in step (2) to 80-90° C., adding the hydroxyl-terminated long-chain silicone oil, and then adding a pH regulator to adjust the pH to 10, and reacting at a constant temperature for 4-5 hours to obtain a petroleum resin solution grafted with a partially hydroxyl-terminated long-chain silicone oil; (4) Preparation of a hydroxyl-terminated colored petroleum resin solution: The product obtained in step (3) is heated to 80-90° C., and the polyol-terminated colorant obtained in step (1) is added thereto, and the pH is adjusted to 10 using a pH regulator, and the reaction is carried out at a constant temperature for 4-5 hours to obtain a hydroxyl-terminated colored petroleum resin solution; (5) Preparation of terminal NCO-modified petroleum resin solution: heating the terminal hydroxyl colored petroleum resin solution obtained in step (4) to 60-70° C., adding isocyanate and catalyst in sequence, and reacting at a constant temperature for 2-3 hours to obtain a terminal NCO-modified petroleum resin solution; (6) Preparation of colored petroleum resin: heating the NCO-modified petroleum resin solution obtained in step (5) to 60-80° C., adding epoxy resin and reacting at constant temperature for 4-5 hours, removing the solvent, and obtaining a colored petroleum resin end-capped with epoxy resin; (7) Preparation of epoxy-modified colored asphalt material: The colored petroleum resin obtained in step (6) is heated to 160° C. and then mixed with an epoxy curing agent in a certain proportion to obtain the epoxy-modified colored asphalt material.