A kind of high permeability emulsified asphalt and preparation method thereof
By using melt mixing of modified epoxy resin and matrix asphalt in emulsified bitumen and crosslinking polyether sulfonate structure emulsification additives with modified epoxy resin, combined with penetration aids and curing additives, the problems of poor permeability and poor compatibility of emulsified bitumen are solved, and higher permeability and stability are achieved.
Patent Information
- Application Number
- CN202410490394.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-04-23
- Publication Date
- 2025-05-09
- Estimated Expiration
- 2044-04-23
AI Technical Summary
The existing emulsified asphalt has poor permeability and poor compatibility and dispersion of epoxy resin with matrix asphalt, resulting in insufficient adhesion and mechanical properties.
Modified epoxy resin and matrix asphalt are melted and mixed in a high-speed shearing machine to form modified asphalt, and the permeability and stability of emulsified asphalt are improved by preparing an emulsification additive with a polyether sulfonate structure crosslinked by modified epoxy resin, combining a penetration additive composed of a fatty alcohol polyoxyethylene ether and a low foam penetration agent SF, and a curing additive with amino-modified long silicone segments.
The permeability and adhesion of emulsified asphalt are improved, the demulsification speed and elongation of evaporated residues are reduced, and the stability and fluidity of emulsified asphalt are enhanced.
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Abstract
Description
Technical Field
[0001] The invention relates to the technical field of emulsified asphalt processing, and in particular to a high-permeability emulsified asphalt and a preparation method thereof. Background Art
[0002] With the rapid development of transportation infrastructure construction, the requirements for asphalt materials in road construction are increasing. At present, most of my country's highways use stable graded aggregates such as cement, lime, sand and gravel as the base layer, and asphalt concrete as the pavement surface layer. However, the strength modulus between the base layer and the surface layer is quite different, and the deformation coordination is poor. If no treatment is performed between the layers, when the horizontal shear force is greater than or equal to the ultimate strength of the layers, the interlayer joint will become a weak link in the pavement structure. Under the action of strong horizontal shear force, the asphalt surface layer will displace at the joint surface, and in severe cases, it will cause slippage, pushing and congestion and other diseases.
[0003] As an important road construction material, emulsified asphalt has the advantages of convenient construction, environmental protection and energy saving. It is widely used in the fields of road paving, repair and maintenance. In the existing technology, emulsified asphalt is often used as a penetration oil for spreading treatment to enhance the bonding performance between the base layer and the surface layer, and reduce the interlayer slippage, congestion and other road diseases of asphalt pavement caused by poor bonding between the road base and surface layers.
[0004] However, the emulsified asphalt in the prior art is mainly composed of base asphalt, emulsifier, additive and water. The asphalt is dispersed in an aqueous solution containing an emulsifier in the form of tiny particles to form an oil-in-water, relatively stable emulsion. There is interfacial tension at the contact interface between the emulsified asphalt and the base aggregate. If the interfacial tension is too large and exceeds the dead weight of the emulsified asphalt particles, the emulsified asphalt may not be able to penetrate effectively. Under the conditions of charge adsorption and water loss, the asphalt matrix in the common emulsified asphalt flows out and forms a connection. Once the emulsified asphalt breaks, it will increase the difficulty of its further penetration. The permeability of the emulsified asphalt needs to be further improved. The water-based epoxy resin can better improve the adhesion of the evaporation residue of the emulsified asphalt. However, due to the large difference in properties between the epoxy resin and the base asphalt, the compatibility of the epoxy resin and the base asphalt is poor, and the amount of epoxy resin used is small, it is difficult to achieve a uniform dispersion effect in the base asphalt. The amount of epoxy resin used and the adhesion and mechanical properties of the emulsified asphalt need to be further improved.
[0005] In view of the technical defects in this aspect, a solution is now proposed. Summary of the invention
[0006] The object of the present invention is to provide a high-permeability emulsified asphalt and a preparation method thereof, so as to solve the technical problems in the prior art that the emulsified asphalt has poor permeability, the property difference between the epoxy resin and the matrix asphalt is large, the compatibility of the epoxy resin and the matrix asphalt is poor, the epoxy resin is difficult to achieve uniform dispersion in the matrix asphalt, and the amount of epoxy resin used and the adhesion and mechanical properties of the emulsified asphalt need to be further improved.
[0007] The object of the present invention can be achieved by the following technical scheme: a high permeability emulsified asphalt, comprising the following components in parts by weight: 40-50 parts of modified asphalt, 50-60 parts of composite emulsion, 5-7 parts of permeation aid and 4-6 parts of curing aid;
[0008] The modified asphalt is processed by the following steps:
[0009] A1, adding epoxy resin and ethyl acetate to a reactor and stirring, raising the temperature of the reactor to 65-75°C, stirring and keeping warm until the system is completely dissolved, adding hexachlorodecane, an acid binding agent and a catalyst to the reactor, keeping warm for 6-8h, and post-treating to obtain a modified epoxy resin;
[0010] The synthetic reaction principle of modified epoxy resin is:
[0011] Under the condition of catalyst, the chlorine atom of hexadecane chloride and the hydroxyl group of epoxy resin undergo nucleophilic substitution reaction under the action of catalyst to generate modified epoxy resin with hexadecane modified epoxy resin. The acid binding agent can capture and neutralize the hydrogen chloride generated during the reaction, thereby maintaining the alkaline environment of the reaction system, which is conducive to the reaction.
[0012] A2. Heat the base asphalt and modified epoxy resin to a molten flow state respectively, then add the asphalt and modified epoxy resin into a high-speed shearing machine with a box temperature of 180-200°C, mix them at a shear rate of 800-1200r / min for 10-20min, add a diluent into the high-speed shearing machine, mix them at a shear rate of 600-900r / min for 30-50min under heat preservation, and obtain modified asphalt.
[0013] Furthermore, in step A1, the epoxy resin, ethyl acetate, hexadecane chloride, acid binding agent and catalyst are used in a ratio of 10g:70mL:4g:1g:0.2g, the catalyst is dibutyltin dilaurate, and the acid binding agent is triethylamine. The post-treatment operation includes: after the reaction is completed, the temperature of the reactor is lowered to room temperature, 0.1mol / L hydrochloric acid solution is added to the reactor, stirred for 10-20min, allowed to stand for separation, the organic phase is washed twice with purified water, and then the organic phase is transferred to a rotary evaporator, the water bath temperature is set to 65-75°C, and low-boiling impurities are removed under reduced pressure to obtain a modified epoxy resin; in step A2, the base asphalt, modified epoxy resin and diluent are used in a ratio of 100g:80g:30mL, and the diluent is 1,4-butanediol diglycidyl ether.
[0014] Furthermore, the preparation method of the composite emulsion is: add an emulsifying aid, purified water, and a stabilizer into a reaction kettle and stir, increase the temperature of the reaction kettle to 65-75° C., and stir for 40-60 minutes to obtain a composite emulsion.
[0015] Furthermore, the preparation method of the composite emulsion is as follows: the usage ratio of the emulsifying aid, purified water and stabilizer is 3g:180mL:1g, and the stabilizer is composed of sodium dodecyl sulfate and sodium alginate in a weight ratio of 1:2.
[0016] Furthermore, the emulsifying aid is obtained by processing the following steps:
[0017] B1, adding polyetheramine and 1,4-butane sultone into a reactor and stirring, raising the temperature of the reactor to 55-65°C, keeping the temperature for 4-5h, adding 0.5mol / L sodium hydroxide solution into the reactor, adjusting the pH of the system to 7-8, adding purified water into the reactor to obtain a polyether sulfonate solution;
[0018] The synthetic reaction principle of polyether sulfonate is:
[0019] The amino group in the polyetheramine is used as a nucleophilic reagent, and the carbonyl carbon in 1,4-butanesulfone is used as an electrophilic center, and a ring-opening reaction of the amine and the lactone occurs. After the reaction is completed, the sulfonic acid group reacts with sodium hydroxide to form polyether sulfonate. By controlling the amount of purified water, polyether sulfonate with different mass concentrations can be obtained.
[0020] B2. Add the modified epoxy resin and the mixed liquid into a reactor and stir. The temperature of the reactor is raised to 70-80°C. Stirring is continued until the system is dissolved. The polyether sulfonate solution is added dropwise into the reactor. The reaction is continued for 3-4 hours. The emulsifying agent is obtained by post-processing.
[0021] The synthetic reaction principle of emulsifying additives is:
[0022] The -NH- group on the polyether sulfonate is nucleophilic and can act as a nucleophilic agent to attack the carbon atom in the epoxy group. When the -NH- group on the polyether sulfonate is close to the epoxy group on the modified epoxy resin, the nitrogen atom in the amino group will attack the carbon atom in the epoxy group, resulting in the ring opening of the epoxy group. At the same time, the nitrogen atom forms a new chemical bond with the carbon atom after the ring opening to achieve chemical crosslinking, thereby forming an emulsifying aid having a polyether sulfonate structure crosslinked with the modified epoxy resin.
[0023] Furthermore, in step B1, the amount ratio of the polyetheramine and 1,4-butanesulfonic acid lactone is 1 mol:2 mol, and the polyetheramine is polyetheramine D220 with a molecular weight of 300; in step B2, the amount ratio of the modified epoxy resin, the mixed solution and the polyether sulfonate solution is 1 g:5 mL:4 g, the mass content of the polyether sulfonate solution is 50-55%, and the mixed solution is composed of ethylene glycol and toluene in a volume ratio of 2:1. The post-treatment operation includes: after the reaction is completed, the temperature of the reactor is lowered to room temperature, petroleum ether is added to the reactor, solids are precipitated, and filtered, the filter cake is washed with petroleum ether 3 times and then dried, and the filter cake is transferred to a drying oven at a temperature of 60-70°C, and dried to constant weight to obtain an emulsifier.
[0024] Furthermore, the penetration aid is composed of fatty alcohol polyoxyethylene ether and low-foaming penetrant SF in a weight ratio of 3:2.
[0025] Furthermore, the preparation method of the curing aid is: 1,7-dimethoxyoctamethyltetrasiloxane, aminopropylmethyldiethoxysilane, and anhydrous ethanol are added to a nitrogen-protected reactor, the temperature of the reactor is increased to 70-80°C, a catalyst solution is added to the reactor, the reaction is kept warm for 6-8 hours, and the curing aid is obtained by post-processing.
[0026] The synthetic reaction principle of curing additive is:
[0027] Under the action of the catalyst solution, the siloxane bonds on 1,7-dimethoxyoctamethyltetrasiloxane and aminopropylmethyldiethoxysilane are broken to form active silanol groups. At the same time, a self-assembly reaction occurs to generate a curing aid of polysiloxane with amino-modified long siloxane chains.
[0028] Furthermore, the amount ratio of the 1,7-dimethoxyoctamethyltetrasiloxane and aminopropylmethyldiethoxysilane is 1 mol:1 mol, the amount ratio of the 1,7-dimethoxyoctamethyltetrasiloxane, anhydrous ethanol and catalyst solution is 2 g:7 mL:3 mL, the catalyst solution is a 10-25 wt% potassium hydroxide solution, and the post-treatment operation includes: after the reaction is completed, adding 0.5 mol / L hydrochloric acid to the reactor, adjusting the system pH to 7-8, distilling off the solvent under reduced pressure, adding anhydrous ethanol to the reactor, filtering, transferring the filtrate to a rotary evaporator, setting the water bath temperature to 55-65°C, and distilling off ethanol under reduced pressure to obtain a curing aid.
[0029] A method for preparing high-permeability emulsified asphalt comprises the following steps:
[0030] S1. Heat the modified asphalt to 150-180°C and keep it in a fluid state to obtain a molten asphalt liquid;
[0031] S2, adding the composite emulsion, the penetration aid and the curing aid into a high-speed shearing machine with a box temperature of 70-80°C, and stirring for 10-15 minutes to obtain an emulsified dilution;
[0032] S3. Set the speed of the high-speed shearing machine to 800-1000r / min, slowly add the molten asphalt liquid into the emulsified diluent, and after the addition is completed, keep warm and stir for 8-12 minutes to obtain emulsified asphalt.
[0033] The present invention has the following beneficial effects:
[0034] The high-permeability emulsified asphalt of the present application is prepared by melt-mixing a modified epoxy resin modified with hexadecane and a base asphalt in a high-speed shearing machine. As a non-polar substance, the introduction of hexadecane can reduce the polarity of the epoxy resin and make its dielectric constant closer to that of petroleum asphalt. The base asphalt is mainly composed of hydrocarbon substances and is hydrophobic. The introduction of hexadecane can increase the hydrophobicity of the epoxy resin and improve the compatibility of the epoxy resin and the base asphalt, so that the modified epoxy resin can be evenly mixed with the base asphalt, reducing the stratification and segregation phenomenon after mixing, making the modified asphalt have more stable performance, and improving the dispersion stability of the amphoteric modified asphalt composed of the epoxy resin and the base asphalt in the composite emulsion, reducing the demulsification rate of the emulsified asphalt, and improving the adhesion between the emulsified asphalt and the aggregate.
[0035] The high-permeability emulsified asphalt of the present application is a composite emulsion composed of an emulsifying aid having a polyether sulfonate structure cross-linked with a modified epoxy resin and a stabilizer composed of sodium dodecyl sulfate and sodium alginate; the hydrophilic groups such as hydroxyl groups and sulfonic acid groups in the structure of the emulsifying aid give it good water solubility, and the hydrophilic groups can form hydrogen bonds with water molecules, so that the entire molecule can be evenly dispersed in water to form a stable water phase. During the emulsification process, the hydrophilic groups tend to gather at the interface between asphalt particles and water to form an interfacial film, which reduces the interfacial tension between the asphalt particles and water, so that the modified asphalt can Better dispersed in water to prevent its aggregation and sedimentation; the modified epoxy resin part in the emulsifier structure has good compatibility with asphalt and good hydrophobicity, so that the emulsifier can be tightly adsorbed on the surface of asphalt particles, forming a protective layer on the surface of modified asphalt to prevent direct contact and aggregation between modified asphalt, thereby forming asphalt dispersed particles with smaller particle size during high-speed shear mixing. At the same time, the modified epoxy resin can also interact with the hydrophilic groups in the water phase to form a three-dimensional network structure to cooperate with the stabilizer, thereby improving the emulsification stability of the emulsified asphalt and reducing the demulsification rate.
[0036] The high-permeability emulsified asphalt of the present application is enhanced by using fatty alcohol polyoxyethylene ether and low-foam penetrant SF as a penetration aid, and using polysiloxane with amino-modified long siloxane chain segments as a curing aid to enhance the asphalt emulsion; fatty alcohol polyoxyethylene ether has good wettability and permeability, and low-foam penetrant SF helps to reduce the generation of foam, while reducing the tension between the liquid and the solid surface of the base aggregate, reducing the generation of foam, making the asphalt emulsion more evenly distributed on the base, and making it easier for the asphalt emulsion to penetrate into the tiny cracks and pores of the base, so that it can better combine with the base and improve the penetration efficiency; the chain segment of the curing aid is a long straight line, and the curing aid itself has a certain lubricating effect. This structure enables the polysiloxane to penetrate more effectively into the This penetration not only fills the gaps in the asphalt, but also makes the overall structure of the emulsified asphalt tighter and more uniform, improves the stability and fluidity of the emulsified asphalt, and thus enhances the penetration ability of the emulsified asphalt. The amino group on the curing aid is a polar group that can form hydrogen bonds or other interactions with polar functional groups such as carboxylic acids and hydroxyls in the asphalt, thereby enhancing the bonding force between the asphalt and the polysiloxane and the adhesion between the asphalt and the base layer. The increased adhesion makes it easier for the emulsified asphalt to adhere to the surface of the base layer and effectively penetrate into the base layer. In addition, the amino group on the curing aid can also undergo an addition reaction with the epoxy group of the epoxy resin to generate new chemical bonds, thereby achieving the curing of the epoxy resin and promoting the curing of the emulsified asphalt. DETAILED DESCRIPTION
[0037] The technical solution of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all of the embodiments. 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.
[0038] The low-foam penetrant SF in this application is purchased from Hai'an Petrochemical Plant in Jiangsu Province, with an active matter content higher than 99wt% and a pH of 6-7; the fatty alcohol polyoxyethylene ether model in this application is AEO-9; the epoxy resin in this application is bisphenol A type epoxy resin, model E51; the base asphalt in this application is SK90# road petroleum asphalt; the polyetheramine in this application is polyetheramine D220, with a molecular weight of 300. Example 1
[0039] This embodiment provides a method for preparing high-permeability emulsified asphalt, comprising the following steps:
[0040] S1. Preparation of modified epoxy resin
[0041] Weigh: 500g of E51 bisphenol A epoxy resin and 3500mL of ethyl acetate are added to a reactor and stirred. The temperature of the reactor is raised to 65°C, and the mixture is stirred and kept warm until the system is completely dissolved. 200g of hexachlorodecane, 50g of triethylamine and 10g of dibutyltin dilaurate are added to the reactor, and the mixture is kept warm for 6h. After the reaction is completed, the temperature of the reactor is lowered to room temperature, 1000mL of 0.1mol / L hydrochloric acid solution is added to the reactor, and the mixture is stirred for 10min. The mixture is allowed to stand for separation, and the organic phase is washed twice with purified water. The organic phase is transferred to a rotary evaporator, and the water bath temperature is set to 65°C. Low-boiling impurities are removed under reduced pressure to obtain a modified epoxy resin.
[0042] S2. Preparation of modified asphalt
[0043] Weigh: 1000 g of base asphalt, 800 g of modified epoxy resin, and 300 mL of 1,4-butanediol diglycidyl ether, and set aside;
[0044] The base asphalt and modified epoxy resin were heated to a molten flow state respectively, and then the asphalt and the modified epoxy resin were added to a high-speed shearing machine with a box temperature of 180°C, and mixed for 10 minutes at a shear rate of 800 r / min. 300 mL of 1,4-butanediol diglycidyl ether was added to the high-speed shearing machine, and the mixture was kept warm and mixed for 30 minutes at a shear rate of 600 r / min to obtain modified asphalt.
[0045] S3. Preparation of composite emulsion
[0046] Weigh: 600 g of polyetheramine and 544.6 g of 1,4-butane sultone, add them into a reactor and stir, raise the temperature of the reactor to 55°C, keep the temperature for 4 hours, add 0.5 mol / L sodium hydroxide solution into the reactor, adjust the pH of the system to 7, add purified water into the reactor to obtain a polyether sulfonate solution;
[0047] Ethylene glycol and toluene are mixed evenly in a volume ratio of 2:1 to obtain a mixed solution for later use;
[0048] Weigh: 100 g of modified epoxy resin and 500 mL of the mixed solution are added to a reactor and stirred. The temperature of the reactor is raised to 70°C. The mixture is stirred at this temperature until the system is dissolved. 400 g of a 50% polyether sulfonate solution is added dropwise to the reactor. The mixture is reacted at this temperature for 3 h. The temperature of the reactor is lowered to room temperature. Petroleum ether is added to the reactor. Solids are precipitated. The solids are filtered. The filter cake is washed with petroleum ether for 3 times and then dried. The filter cake is transferred to a drying oven at 60°C and dried to constant weight to obtain an emulsifying agent.
[0049] Mix sodium lauryl sulfate and sodium alginate in a weight ratio of 1:2 to obtain a stabilizer for later use;
[0050] Weigh: 30 g of emulsifying aid, 1800 mL of purified water, and 10 g of stabilizer, add into a reactor and stir, raise the temperature of the reactor to 65° C., keep warm and stir for 40 min, and obtain a composite emulsion.
[0051] S4. Preparation of penetration enhancer
[0052] The fatty alcohol polyoxyethylene ether and the low-foaming penetrant SF are uniformly mixed in a weight ratio of 3:2 to obtain a penetration enhancer.
[0053] S5. Preparation of curing aid
[0054] Weigh: 342.7 g of 1,7-dimethoxyoctamethyltetrasiloxane, 191.3 g of aminopropylmethyldiethoxysilane, and 1200 mL of anhydrous ethanol, add them to a nitrogen-protected reactor, raise the temperature of the reactor to 70°C, add 514.1 mL of 10 wt% potassium hydroxide solution to the reactor, and keep the reaction warm for 6 hours. After the reaction is completed, add 0.5 mol / L hydrochloric acid to the reactor, adjust the pH of the system to 7, evaporate the solvent under reduced pressure, add anhydrous ethanol to the reactor, filter, transfer the filtrate to a rotary evaporator, set the water bath temperature to 55°C, and evaporate the ethanol under reduced pressure to obtain a curing aid.
[0055] S6. Preparation of emulsified asphalt
[0056] Weigh: 400 g of modified asphalt, heat to 150°C, keep it in a fluid state, and obtain molten asphalt liquid;
[0057] Weigh: 500 g of composite emulsion, 50 g of penetration aid and 40 g of curing aid, add into a high-speed shearing machine with a box temperature of 70°C, keep warm and stir for 10 minutes to obtain an emulsified dilution;
[0058] The speed of the high-speed shearing machine was set to 800 r / min, and 400 g of molten asphalt liquid was slowly added to the emulsified diluent. After the addition was completed, the mixture was stirred at a temperature of 8 minutes to obtain emulsified asphalt. Example 2
[0059] This embodiment provides a method for preparing high-permeability emulsified asphalt, comprising the following steps:
[0060] S1. Preparation of modified epoxy resin
[0061] Weigh: 500g of E51 bisphenol A epoxy resin and 3500mL of ethyl acetate are added to a reactor and stirred. The temperature of the reactor is raised to 70°C, and the mixture is stirred and kept warm until the system is completely dissolved. 200g of hexachlorodecane, 50g of triethylamine and 10g of dibutyltin dilaurate are added to the reactor, and the mixture is kept warm for 7h. After the reaction is completed, the temperature of the reactor is lowered to room temperature, 1000mL of 0.1mol / L hydrochloric acid solution is added to the reactor, and the mixture is stirred for 15min. The mixture is allowed to stand for separation, and the organic phase is washed twice with purified water. The organic phase is transferred to a rotary evaporator, and the water bath temperature is set to 70°C. Low-boiling impurities are removed under reduced pressure to obtain a modified epoxy resin.
[0062] S2. Preparation of modified asphalt
[0063] Weigh: 1000 g of base asphalt, 800 g of modified epoxy resin, and 300 mL of 1,4-butanediol diglycidyl ether, and set aside;
[0064] The base asphalt and modified epoxy resin were heated to a molten flow state respectively, and then the asphalt and the modified epoxy resin were added to a high-speed shearing machine with a box temperature of 190°C, and mixed for 15 minutes at a shear rate of 1000 r / min. 300 mL of 1,4-butanediol diglycidyl ether was added to the high-speed shearing machine, and the mixture was kept warm and mixed for 40 minutes at a shear rate of 750 r / min to obtain modified asphalt.
[0065] S3. Preparation of composite emulsion
[0066] Weigh: 600 g of polyetheramine and 544.6 g of 1,4-butane sultone, add them into a reactor and stir, raise the temperature of the reactor to 60°C, keep the temperature for 4.5 hours, add 0.5 mol / L sodium hydroxide solution into the reactor, adjust the pH of the system to 7.5, add purified water into the reactor to obtain a polyether sulfonate solution;
[0067] Ethylene glycol and toluene are mixed evenly in a volume ratio of 2:1 to obtain a mixed solution for later use;
[0068] Weigh: 100 g of modified epoxy resin and 500 mL of mixed solution are added to a reactor and stirred. The temperature of the reactor is raised to 75°C. The mixture is stirred at this temperature until the system is dissolved. 400 g of a polyether sulfonate solution with a mass content of 53% is added dropwise to the reactor. The mixture is reacted at this temperature for 3.5 h. The temperature of the reactor is lowered to room temperature. Petroleum ether is added to the reactor. Solids are precipitated. The solids are filtered. The filter cake is washed with petroleum ether for 3 times and then dried. The filter cake is transferred to a drying oven at a temperature of 65°C and dried to constant weight to obtain an emulsifying agent.
[0069] Mix sodium lauryl sulfate and sodium alginate in a weight ratio of 1:2 to obtain a stabilizer for later use;
[0070] Weigh: 30 g of emulsifying aid, 1800 mL of purified water, and 10 g of stabilizer, add into a reactor and stir, raise the temperature of the reactor to 70° C., keep warm and stir for 50 min, and obtain a composite emulsion.
[0071] S4. Preparation of penetration enhancer
[0072] The fatty alcohol polyoxyethylene ether and the low-foaming penetrant SF are uniformly mixed in a weight ratio of 3:2 to obtain a penetration enhancer.
[0073] S5. Preparation of curing aid
[0074] Weigh: 342.7 g of 1,7-dimethoxyoctamethyltetrasiloxane, 191.3 g of aminopropylmethyldiethoxysilane, and 1200 mL of anhydrous ethanol, add them to a nitrogen-protected reactor, raise the temperature of the reactor to 75°C, add 514.1 mL of 20 wt% potassium hydroxide solution to the reactor, and keep the reaction warm for 7 hours. After the reaction is completed, add 0.5 mol / L hydrochloric acid to the reactor, adjust the pH of the system to 7.5, evaporate the solvent under reduced pressure, add anhydrous ethanol to the reactor, filter, transfer the filtrate to a rotary evaporator, set the water bath temperature to 60°C, and evaporate the ethanol under reduced pressure to obtain a curing aid.
[0075] S6. Preparation of emulsified asphalt
[0076] Weigh: 450 g of modified asphalt, heat to 165°C, keep it in a fluid state, and obtain molten asphalt liquid;
[0077] Weigh: 550g of composite emulsion, 60g of penetration aid and 50g of curing aid, add into a high-speed shearing machine with a box temperature of 75°C, keep warm and stir for 13 minutes to obtain an emulsified dilution;
[0078] The speed of the high-speed shearing machine was set to 900 r / min, and 450 g of molten asphalt liquid was slowly added to the emulsified diluent. After the addition was completed, the mixture was kept warm and stirred for 10 minutes to obtain emulsified asphalt. Example 3
[0079] This embodiment provides a method for preparing high-permeability emulsified asphalt, comprising the following steps:
[0080] S1. Preparation of modified epoxy resin
[0081] Weigh: 500g of E51 bisphenol A epoxy resin and 3500mL of ethyl acetate are added to a reactor and stirred. The temperature of the reactor is raised to 75°C, and the mixture is stirred and kept warm until the system is completely dissolved. 200g of hexachlorodecane, 50g of triethylamine and 10g of dibutyltin dilaurate are added to the reactor, and the mixture is kept warm for 8h. After the reaction is completed, the temperature of the reactor is lowered to room temperature, 1000mL of 0.1mol / L hydrochloric acid solution is added to the reactor, and the mixture is stirred for 20min. The mixture is allowed to stand for separation, and the organic phase is washed twice with purified water. The organic phase is transferred to a rotary evaporator, and the water bath temperature is set to 75°C. Low-boiling impurities are removed under reduced pressure to obtain a modified epoxy resin.
[0082] S2. Preparation of modified asphalt
[0083] Weigh: 1000 g of base asphalt, 800 g of modified epoxy resin, and 300 mL of 1,4-butanediol diglycidyl ether, and set aside;
[0084] The base asphalt and modified epoxy resin were heated to a molten flow state respectively, and then the asphalt and the modified epoxy resin were added to a high-speed shearing machine with a box temperature of 200°C, and mixed for 20 minutes at a shear rate of 1200 r / min. 300 mL of 1,4-butanediol diglycidyl ether was added to the high-speed shearing machine, and the mixture was kept warm and mixed for 50 minutes at a shear rate of 900 r / min to obtain modified asphalt.
[0085] S3. Preparation of composite emulsion
[0086] Weigh: 600 g of polyetheramine and 544.6 g of 1,4-butane sultone, add them into a reactor and stir, raise the temperature of the reactor to 65°C, keep the temperature for 5 hours, add 0.5 mol / L sodium hydroxide solution into the reactor, adjust the pH of the system to 8, add purified water into the reactor to obtain a polyether sulfonate solution;
[0087] Ethylene glycol and toluene are mixed evenly in a volume ratio of 2:1 to obtain a mixed solution for later use;
[0088] Weigh: 100 g of modified epoxy resin and 500 mL of mixed solution are added to a reactor and stirred. The temperature of the reactor is raised to 80°C. The mixture is stirred at this temperature until the system is dissolved. 400 g of a polyether sulfonate solution with a mass content of 55% is added dropwise to the reactor. The mixture is reacted at this temperature for 4 hours. The temperature of the reactor is lowered to room temperature. Petroleum ether is added to the reactor. Solids are precipitated. The solids are filtered. The filter cake is washed with petroleum ether for 3 times and then dried. The filter cake is transferred to a drying oven at a temperature of 70°C and dried to constant weight to obtain an emulsifying agent.
[0089] Mix sodium lauryl sulfate and sodium alginate in a weight ratio of 1:2 to obtain a stabilizer for later use;
[0090] Weigh: 30 g of emulsifying aid, 1800 mL of purified water, and 10 g of stabilizer, add into a reactor and stir, raise the temperature of the reactor to 75° C., keep warm and stir for 60 min, and obtain a composite emulsion.
[0091] S4. Preparation of penetration enhancer
[0092] The fatty alcohol polyoxyethylene ether and the low-foaming penetrant SF are uniformly mixed in a weight ratio of 3:2 to obtain a penetration enhancer.
[0093] S5. Preparation of curing aid
[0094] Weigh: 342.7 g of 1,7-dimethoxyoctamethyltetrasiloxane, 191.3 g of aminopropylmethyldiethoxysilane, and 1200 mL of anhydrous ethanol, add them to a nitrogen-protected reactor, raise the temperature of the reactor to 80°C, add 514.1 mL of 25 wt% potassium hydroxide solution to the reactor, and keep the reaction warm for 8 hours. After the reaction is completed, add 0.5 mol / L hydrochloric acid to the reactor, adjust the pH of the system to 8, evaporate the solvent under reduced pressure, add anhydrous ethanol to the reactor, filter, transfer the filtrate to a rotary evaporator, set the water bath temperature to 65°C, and evaporate the ethanol under reduced pressure to obtain a curing aid.
[0095] S6. Preparation of emulsified asphalt
[0096] Weigh: 500 g of modified asphalt is heated to 180°C and kept in a fluid state to obtain molten asphalt liquid;
[0097] Weigh: 600 g of composite emulsion, 70 g of penetration aid and 60 g of curing aid, add into a high-speed shearing machine with a box temperature of 80°C, keep warm and stir for 15 minutes to obtain an emulsified dilution;
[0098] The speed of the high-speed shearing machine was set to 1000 r / min, and 500 g of molten asphalt liquid was slowly added to the emulsified diluent. After the addition was completed, the mixture was stirred at a temperature of 12 minutes to obtain emulsified asphalt.
[0099] Comparative Example 1
[0100] The difference between this comparative example and Example 3 is that step S1 is eliminated, and the bisphenol A epoxy resin in step S1 replaces the modified epoxy resin in step S1 to participate in subsequent processing.
[0101] Comparative Example 2
[0102] The difference between this comparative example and Example 3 is that step S2 is eliminated, and the modified asphalt in step S2 is replaced by the asphalt matrix in step S2 and the subsequent processing
[0103] Comparative Example 3
[0104] The difference between this comparative example and Example 3 is that in step S3, the emulsifying aid is replaced by the polyether sulfonate solid powder obtained by evaporating the polyether sulfonate solution to dryness.
[0105] Comparative Example 4
[0106] The difference between this comparative example and Example 3 is that step S5 is omitted and ethylenediamine is used as a curing aid.
[0107] Performance Test:
[0108] The permeability coefficients of the emulsified asphalts prepared in Examples 1-3 and Comparative Examples 1-4 were determined with reference to the standard GB / T 38050-2019 "Determination of permeability of emulsified asphalt", and the demulsification rate of the samples, the elongation at break and the breaking strength of the evaporation residue, the amount of adhered sand and the change rate of the wheel track width were determined with reference to the standard GB / T 38990-2020 "Water-based epoxy resin emulsified asphalt mixture for roads". The specific test results are shown in the table below:
[0109]
[0110] Data Analysis:
[0111] Comparative analysis of the data in the above table shows that the permeability coefficient of the emulsified asphalt prepared by the present invention reaches 1.40 cm, the demulsification speed reaches slow cracking, the elongation at break of the evaporation residue (25°C) reaches 67.9%, the fracture strength of the evaporation residue (25°C) reaches 0.85 MPa, and the amount of adhesive sand in the sample reaches 458.4 g / m 2 , the profile change rate of the sample reached 1.3%, and all performance tests were better than the control example;
[0112] It is explained that the present invention prepares a composite emulsion by preparing an emulsifying aid and a stabilizer in combination with each other, and then mixes the composite emulsion with a penetration aid and a curing aid to form an emulsified diluent, and the modified asphalt is evenly dispersed in the emulsified diluent. After high-speed dispersion, the prepared emulsified asphalt not only has excellent emulsification stability and penetration performance, but also has good sand adhesion performance and mechanical strength.
[0113] The above contents are merely examples and explanations of the structure of the present invention. The technicians in this technical field may make various modifications or additions to the specific embodiments described or replace them in a similar manner. As long as they do not deviate from the structure of the invention or exceed the scope defined by the claims, they should all fall within the protection scope of the present invention.
[0114] In the description of this specification, the description with reference to the terms "one embodiment", "example", "specific example", etc. means that the specific features, structures, materials or characteristics described in conjunction with the embodiment or example are included in at least one embodiment or example of the present invention. In this specification, the schematic representation of the above terms does not necessarily refer to the same embodiment or example. Moreover, the specific features, structures, materials or characteristics described can be combined in any one or more embodiments or examples in a suitable manner.
[0115] The preferred embodiments of the present invention disclosed above are only used to help explain the present invention. The preferred embodiments do not describe all the details in detail, nor do they limit the invention to only specific implementation methods. Obviously, many modifications and changes can be made according to the content of this specification. This specification selects and specifically describes these embodiments in order to better explain the principles and practical applications of the present invention, so that those skilled in the art can understand and use the present invention well. The present invention is limited only by the claims and their full scope and equivalents.
Claims
1. A high permeability emulsified asphalt, characterized in that: The invention comprises the following components in parts by weight: 40-50 parts of modified asphalt, 50-60 parts of composite emulsion, 5-7 parts of penetration aid and 4-6 parts of curing aid; The modified asphalt is processed by the following steps: A1, adding epoxy resin and ethyl acetate to a reactor and stirring, raising the temperature of the reactor to 65-75°C, stirring and keeping warm until the system is completely dissolved, adding hexachlorodecane, an acid binding agent and a catalyst to the reactor, keeping warm for 6-8h, and post-treating to obtain a modified epoxy resin; A2. Heat the base asphalt and the modified epoxy resin to a molten flow state respectively, add the asphalt and the modified epoxy resin to a high-speed shearing machine with a box temperature of 180-200°C, mix them at a shear rate of 800-1200r / min for 10-20min, add a diluent to the high-speed shearing machine, and mix them at a shear rate of 600-900r / min for 30-50min to obtain modified asphalt; The penetration enhancer is composed of fatty alcohol polyoxyethylene ether and low-foaming penetrant SF; The preparation method of the curing aid is as follows: 1,7-dimethoxyoctamethyltetrasiloxane, aminopropylmethyldiethoxysilane and anhydrous ethanol are added to a nitrogen-protected reactor, the temperature of the reactor is increased to 70-80° C., a catalyst solution is added to the reactor, the reaction is carried out by heat preservation for 6-8 hours, and the curing aid is obtained by post-processing; The preparation method of the composite emulsion is as follows: an emulsifying agent, purified water and a stabilizer are added into a reaction kettle and stirred, the temperature of the reaction kettle is increased to 65-75° C., and the mixture is stirred for 40-60 minutes to obtain a composite emulsion, wherein the stabilizer is composed of sodium dodecyl sulfate and sodium alginate; The emulsifying aid is obtained by processing the following steps: B1, adding polyetheramine and 1,4-butane sultone into a reactor and stirring, raising the temperature of the reactor to 55-65°C, keeping the temperature for 4-5h, adding 0.5mol / L sodium hydroxide solution into the reactor, adjusting the pH of the system to 7-8, adding purified water into the reactor to obtain a polyether sulfonate solution; B2. Add the modified epoxy resin and the mixed liquid into a reactor and stir. The temperature of the reactor is raised to 70-80°C. Stirring is continued until the system is dissolved. The polyether sulfonate solution is added dropwise into the reactor. The reaction is continued for 3-4 hours. The emulsifying agent is obtained by post-processing.
2. A high permeability emulsified asphalt according to claim 1, characterized in that: In step A1, the epoxy resin, ethyl acetate, hexadecane chloride, acid binding agent and catalyst are used in a ratio of 10g:70mL:4g:1g:0.2g, the catalyst is dibutyltin dilaurate, and the acid binding agent is triethylamine. The post-treatment operation includes: after the reaction is completed, the temperature of the reactor is lowered to room temperature, 0.1mol / L hydrochloric acid solution is added to the reactor, stirred for 10-20min, and allowed to stand for liquid separation. After the organic phase is washed twice with purified water, the organic phase is transferred to a rotary evaporator, the water bath temperature is set to 65-75°C, and low-boiling impurities are removed under reduced pressure to obtain a modified epoxy resin; in step A2, the base asphalt, modified epoxy resin and diluent are used in a ratio of 100g:80g:30mL, and the diluent is 1,4-butanediol diglycidyl ether.
3. A high permeability emulsified asphalt according to claim 1, characterized in that: The usage ratio of the emulsifying aid, purified water and stabilizer is 3g:180mL:1g, and the stabilizer is composed of sodium dodecyl sulfate and sodium alginate in a weight ratio of 1:
2.
4. A high permeability emulsified asphalt according to claim 1, characterized in that: In step B1, the amount ratio of the polyetheramine and 1,4-butanesulfonic acid lactone is 1 mol:2 mol, and the polyetheramine is polyetheramine D220 with a molecular weight of 300; in step B2, the amount ratio of the modified epoxy resin, the mixed solution and the polyether sulfonate solution is 1 g:5 mL:4 g, the mass content of the polyether sulfonate solution is 50-55%, and the mixed solution is composed of ethylene glycol and toluene in a volume ratio of 2:
1. The post-treatment operation includes: after the reaction is completed, the temperature of the reactor is lowered to room temperature, petroleum ether is added to the reactor, solids are precipitated, and filtered, the filter cake is washed with petroleum ether 3 times and then dried, and the filter cake is transferred to a drying oven at a temperature of 60-70°C, and dried to constant weight to obtain an emulsifier.
5. A high permeability emulsified asphalt according to claim 1, characterized in that: The dosage ratio of the 1,7-dimethoxyoctamethyltetrasiloxane and aminopropylmethyldiethoxysilane is 1 mol:1 mol, the dosage ratio of the 1,7-dimethoxyoctamethyltetrasiloxane, anhydrous ethanol and catalyst solution is 2 g:7 mL:3 mL, the catalyst solution is a 10-25 wt% potassium hydroxide solution, and the post-treatment operation comprises: after the reaction is completed, adding 0.5 mol / L hydrochloric acid to the reactor, adjusting the system pH to 7-8, distilling off the solvent under reduced pressure, adding anhydrous ethanol to the reactor, filtering, transferring the filtrate to a rotary evaporator, setting the water bath temperature to 55-65° C., distilling off the ethanol under reduced pressure, and obtaining a curing aid.
6. A method for preparing a high permeability emulsified asphalt according to any one of claims 1 to 5, characterized in that: The following steps are involved: S1. Heat the modified asphalt to 150-180°C and keep it in a fluid state to obtain a molten asphalt liquid; S2, adding the composite emulsion, the penetration aid and the curing aid into a high-speed shearing machine with a box temperature of 70-80°C, and stirring for 10-15 minutes to obtain an emulsified dilution; S3. Set the speed of the high-speed shearing machine to 800-1000r / min, slowly add the molten asphalt liquid into the emulsified diluent, and after the addition is completed, keep warm and stir for 8-12 minutes to obtain emulsified asphalt.
Citation Information
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