CN112625454A - Phase-change thermoregulation asphalt and preparation method thereof - Google Patents

Phase-change thermoregulation asphalt and preparation method thereof Download PDF

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Publication number
CN112625454A
CN112625454A CN202011436128.4A CN202011436128A CN112625454A CN 112625454 A CN112625454 A CN 112625454A CN 202011436128 A CN202011436128 A CN 202011436128A CN 112625454 A CN112625454 A CN 112625454A
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asphalt
parts
tetradecane
phase change
octanoic acid
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马峰
刘健
董文豪
傅珍
金彦鑫
温雅噜
李思琪
袁康博
郭兴隆
刘松然
史柯
王钰洁
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Changan University
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Changan University
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K9/00Use of pretreated ingredients
    • C08K9/10Encapsulated ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/01Hydrocarbons
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00Use of organic ingredients
    • C08K5/04Oxygen-containing compounds
    • C08K5/09Carboxylic acids; Metal salts thereof; Anhydrides thereof

Abstract

The invention provides phase-change thermoregulation asphalt and a preparation method thereof, wherein the phase-change thermoregulation asphalt comprises the following components in parts by mass: tetradecane (50-51), n-octanoic acid (49-51), melamine (15-22.5), formaldehyde (45-67.5), polyvinyl alcohol (0.2-0.5) and TiO (0.5-1)2Nanoparticles, (0.2-0.5) parts SDS and 93 parts asphalt; the phase change microcapsule is prepared by tetradecane and n-caprylic acid, and the phase change material is changed from a liquid state to a solid state in a low-temperature environment to release heat, so that the cooling rate of asphalt can be delayed to a certain extent, the purposes of delaying or shortening the occurrence and duration of extreme low temperature are achieved, and the low-temperature performance of the asphalt binder is improved.

Description

Phase-change thermoregulation asphalt and preparation method thereof
Technical Field
The invention relates to the field of asphalt preparation, in particular to phase-change temperature-regulating asphalt and a preparation method thereof.
Background
In winter, low-temperature weather frequently occurs, and under the weather condition all the year round, the asphalt mixture needs to have better pavement performance to ensure daily use. Due to the fact that the temperature of the area is low, when the area meets rainy and snowy weather, the road surface is easy to freeze. The data show that the coefficient of adhesion between soft snow road and tire is between 0.20 and 0.40, the coefficient of adhesion between compacted snow road and vehicle tire is between 0.15 and 0.50, and the coefficient of adhesion between frozen road is only 1/8 to 1/4 of dry road. The low temperature can also reduce the anti-skid and anti-cracking performance of the asphalt mixture, and the use of roads and the life and property safety of people are seriously influenced. How to alleviate the traffic problem caused by the low road temperature in winter is a focus of attention of vast highway researchers.
Disclosure of Invention
The invention aims to provide phase-change thermoregulation asphalt and a preparation method thereof, which solve the defects of poor anti-sliding and anti-cracking performance of asphalt mixtures in the prior art in a low-temperature environment.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides phase-change thermoregulation asphalt which comprises the following components in parts by mass: (50-51) tetradecane, (49-)51) N-octanoic acid (15-22.5 portions), melamine (45-67.5 portions), formaldehyde (0.2-0.5 portions), polyvinyl alcohol (0.5-1 portions), and TiO (0.5-1 portions)2Nanoparticles, (0.2-0.5) parts SDS, and 93 parts bitumen.
Preferably, the coating comprises the following components in parts by mass: 50.5 parts of tetradecane, 49.5 parts of n-octanoic acid, 15 parts of melamine, 45 parts of formaldehyde, 0.4 part of polyvinyl alcohol, 0.7 part of TiO2Nanoparticles, 0.3 parts SDS, and 93 parts asphalt.
A phase-change thermoregulation asphalt comprises the following steps:
step 1, weighing the following components in parts by mass: tetradecane (50-51), n-octanoic acid (49-51), melamine (15-22.5), formaldehyde (45-67.5), polyvinyl alcohol (0.2-0.5) and TiO (0.5-1)2Nanoparticles, (0.2-0.5) parts SDS and 93 parts asphalt;
step 2, mixing the weighed tetradecane and n-octanoic acid to obtain a uniformly mixed tetradecane-n-octanoic acid binary phase change system A;
step 3, mixing the weighed melamine, formaldehyde, polyvinyl alcohol and deionized water to obtain a mixed solution; adjusting the pH value of the obtained mixed solution to 8, and then carrying out constant-temperature water bath reaction to obtain PVA modified melamine formaldehyde resin;
adding TiO into the obtained PVA modified melamine formaldehyde resin2Nanoparticles to obtain doped TiO2PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles;
step 4, mixing the tetradecane-n-octanoic acid binary phase change system A obtained in the step 1 with water to obtain a mixed solution;
adjusting the pH value of the obtained mixed solution to 3-4, adding SDS (sodium dodecyl sulfate) into a constant-temperature water bath for intensive stirring, emulsifying and dispersing, and dripping the doped TiO into the mixed solution during the intensive stirring process2Slowly stirring the PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles after finishing dripping, and obtaining a phase change microcapsule dispersion liquid after finishing the reaction;
step 5, filtering, cleaning and drying the obtained phase change microcapsule dispersion liquid to obtain tetradecane-n-octanoic acid phase change microcapsules;
and 6, slowly adding the tetradecane-n-octanoic acid phase change microcapsule with the mixing amount of 1-10% into the asphalt in the molten state, and slowly stirring until the phase change temperature regulation asphalt is uniformly mixed to prepare the phase change temperature regulation asphalt.
Preferably, the method comprises the following steps:
step 1, weighing the following components in parts by mass: 50.5 parts of tetradecane, 49.5 parts of n-octanoic acid, 15 parts of melamine, 45 parts of formaldehyde, 0.4 part of polyvinyl alcohol, 0.7 part of TiO2 nanoparticles, 0.3 part of SDS and 93 parts of asphalt;
step 2, mixing the weighed tetradecane and n-octanoic acid to obtain a uniformly mixed tetradecane-n-octanoic acid binary phase change system A;
step 3, mixing the weighed melamine, formaldehyde, polyvinyl alcohol and deionized water to obtain a mixed solution; adjusting the pH value of the obtained mixed solution to 8, and then carrying out constant-temperature water bath reaction to obtain PVA modified melamine formaldehyde resin;
adding TiO into the obtained PVA modified melamine formaldehyde resin2Nanoparticles to obtain doped TiO2PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles;
step 4, mixing the tetradecane-n-octanoic acid binary phase change system A obtained in the step 1 with water to obtain a mixed solution;
adjusting the pH value of the obtained mixed solution to 3-4, adding SDS (sodium dodecyl sulfate) into a constant-temperature water bath for intensive stirring, emulsifying and dispersing, and dripping the doped TiO into the mixed solution during the intensive stirring process2Slowly stirring the PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles after finishing dripping, and obtaining a phase change microcapsule dispersion liquid after finishing the reaction;
step 5, filtering, cleaning and drying the obtained phase change microcapsule dispersion liquid to obtain tetradecane-n-octanoic acid phase change microcapsules;
and 6, slowly adding the tetradecane-n-octanoic acid phase change microcapsule with the mixing amount of 1-10% into the asphalt in the molten state, and slowly stirring until the phase change temperature regulation asphalt is uniformly mixed to prepare the phase change temperature regulation asphalt.
Preferably, the process conditions of the constant temperature water bath reaction in step 3 and step 4 are as follows: and carrying out constant-temperature water bath reaction at the temperature of 70 ℃ for 30 min.
Preferably, in the step 4, the volume ratio of the tetradecane-n-octanoic acid binary phase change system A to water is 1: 2.
Compared with the prior art, the invention has the beneficial effects that:
according to the phase-change temperature-regulating asphalt and the preparation method thereof, the phase-change microcapsules are prepared from tetradecane and n-caprylic acid, and the phase-change material is changed from a liquid state to a solid state in a low-temperature environment to release heat, so that the cooling rate of the asphalt can be delayed to a certain extent, the purpose of delaying or shortening the occurrence and duration of extreme low temperature is achieved, and the low-temperature performance of the asphalt binder is improved.
Drawings
FIG. 1 is a diagram of the temperature regulating effect of phase change temperature regulating asphalt tested by a comparative test.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The invention provides phase-change thermoregulation asphalt which comprises the following components in parts by mass: tetradecane (50-51), n-octanoic acid (49-51), melamine (15-22.5), formaldehyde (45-67.5), polyvinyl alcohol (0.2-0.5) and TiO (0.5-1)2Nanoparticles, (0.2-0.5) parts SDS, and 93 parts bitumen.
Further, the phase-change thermoregulation asphalt provided by the invention comprises the following components in parts by mass: 50.5 parts of tetradecane, 49.5 parts of n-octanoic acid, 15 parts of melamine, 45 parts of formaldehyde, 0.4 part of polyvinyl alcohol, 0.7 part of TiO2 nanoparticles, 0.3 part of SDS and 93 parts of asphalt.
Comprises the following components; the core of the invention lies in the selection of raw materials and the proportion of the raw materials, and the effect is that the asphalt has heat storage capacity, thereby achieving the purpose of temperature regulation in the using process.
Use ofTetradecane-n-octanoic acid composite phase-change material as core material and TiO2The phase-change temperature-regulating asphalt prepared by the phase-change microcapsule with the composite wall material prepared by filling polyvinyl alcohol modified melamine formaldehyde resin with the nano particles.
The invention provides phase-change thermoregulation asphalt, which comprises the following steps:
step 1, according to the mass ratio of (50-51): (51-49), weighing tetradecane and n-octanoic acid, pouring into a beaker, placing the beaker on a magnetic stirrer, and stirring for 30min to obtain a uniformly mixed tetradecane-n-octanoic acid binary phase change system A;
step 2, according to the mass ratio of (1-1.5): (3-4.5) adding melamine and 36-38% by mass of formaldehyde solution into a three-neck flask, adding polyvinyl alcohol (PVA) and deionized water, and stirring and mixing uniformly to obtain a mixed solution; wherein, the adding mass of the polyvinyl alcohol (PVA) is 0.5 percent of the total mass of the melamine and the formaldehyde; the volume of the deionized water is the sum of the volumes of other solutions;
step 3, adjusting the pH value of the mixed solution obtained in the step 2 to 8 by using a NaOH solution, then installing a thermometer and a condensing reflux pipe on the three-neck flask, and carrying out constant-temperature water bath reaction for 30min at the temperature of 70 ℃; obtaining PVA modified melamine formaldehyde resin;
step 4, adding TiO into the PVA modified melamine formaldehyde resin obtained in the step 32Stirring the nano particles for 40-60 min by magnetic force to obtain the doped TiO2PVA modified melamine formaldehyde resin wall material prepolymer B of nano particles, wherein TiO2The mass of the nano particles is 0.5 percent of the total mass of the PVA modified melamine formaldehyde resin;
step 5, mixing the tetradecane-n-octanoic acid binary phase change system A and water according to the volume ratio of 1:2, adding the mixture into a three-neck flask with a condensation reflux pipe and a thermometer to obtain a mixed solution of the composite core material A and water;
then, regulating the pH value of a mixed solution of the composite core material A and water to 3-4 by using citric acid;
heating to 70 deg.C in a constant temperature water bath, and adding SDS (sodium dodecyl sulfate), SDS (sodium dodecyl sulfate)The mass of the phase change system is 0.2 percent of that of the tetradecane-n-octanoic acid binary phase change system A, and then the phase change system A is stirred vigorously, emulsified and dispersed for 30min, wherein the doped TiO is dripped into the phase change system A under the vigorous stirring of an electric stirrer2PVA modified melamine formaldehyde resin wall material prepolymer B of nano particles, tetradecane-n-octanoic acid binary phase change system A and doped TiO2The mass ratio of the PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles is (0.8-1): (1-1.2), slowly stirring after dripping, continuously reacting for 3 hours under the condition of water bath at 70 ℃, adjusting the pH of the mixed solution to 9 by adopting a NaOH solution with the mass fraction of 20% in the process, and obtaining a phase-change microcapsule dispersion liquid after the reaction is finished;
step 6, filtering the phase change microcapsule dispersion liquid obtained in the step 5 to obtain a primary product; after filtering, washing the obtained primary product by using an ethanol solution with the concentration of 30%, and then filtering again to obtain a secondary product; finally, drying the secondary product in a vacuum drying oven at 50 ℃ to obtain tetradecane-n-octanoic acid phase-change microcapsules;
and 7, heating and weighing the asphalt, slowly adding the tetradecane-n-octanoic acid phase change microcapsule with the mixing amount of 1-10% into the asphalt in multiple times, and slowly stirring the mixture until the mixture is uniformly mixed to prepare the phase change temperature-regulating asphalt.
The invention can adjust the temperature of the asphalt according to the change of the external environment, and the principle of the invention is to utilize the characteristics of the phase change material, namely the phase change material can exchange heat with the outside, for example, water becomes ice to release heat, the ice becomes water to absorb heat, and the phase change process is the phase change process. This application utilizes phase change material to become solid-state by the liquid in low temperature environment, and is exothermic to can delay the cooling rate of pitch to a certain extent, reach the purpose that delays or shortens extremely microthermal appearance and duration, thereby promote the low temperature performance of asphalt binder.
Example 1
Preparing phase change temperature-adjusting asphalt with the mixing amount of 4 percent: heating asphalt in a baking oven at 140 ℃, pouring the asphalt into an aluminum pot after the asphalt is in a liquid flowing state, weighing the quality, putting the aluminum pot into a heating sleeve, and extending a temperature probe matched with the heating sleeve into the asphalt so as to ensure the control of the temperature of the asphalt in the shearing process. Converting the mass of the required tetradecane-n-octanoic acid phase change microcapsule according to the weighed mass of the asphalt, slowly adding the weighed tetradecane-n-octanoic acid phase change microcapsule into the asphalt in several times, and slowly stirring the tetradecane-n-octanoic acid phase change microcapsule by a glass rod until the tetradecane-n-octanoic acid phase change microcapsule is immersed into the asphalt during the process to prepare the phase change temperature regulating asphalt.
Inserting the rotary head of the high-speed shearing machine into the asphalt, adjusting the height of a rod connected with the rotary head to enable the rotary head to be 1-2 cm away from the pot bottom, and setting the rotating speed for shearing for 10 min. The slow and constant stirring of the pitch with a glass rod is required due to the generation of bubbles in the pitch and the resulting volume expansion during the shearing process.
Example 2
Preparing phase change temperature-adjusting asphalt with the mixing amount of 7 percent: heating asphalt in a baking oven at 140 ℃, pouring the asphalt into an aluminum pot after the asphalt is in a liquid flowing state, weighing the quality, putting the aluminum pot into a heating sleeve, and extending a temperature probe matched with the heating sleeve into the asphalt so as to ensure the control of the temperature of the asphalt in the shearing process. Converting the mass of the required tetradecane-n-octanoic acid phase change microcapsule according to the weighed mass of the asphalt, slowly adding the weighed tetradecane-n-octanoic acid phase change microcapsule into the asphalt in several times, and manually and slowly stirring by using a glass rod until the tetradecane-n-octanoic acid phase change microcapsule is immersed into the asphalt.
Inserting the rotary head of the high-speed shearing machine into the asphalt, adjusting the height of a rod connected with the rotary head to enable the rotary head to be 1-2 cm away from the pot bottom, and setting the rotating speed for shearing for 10 min. The slow and constant stirring of the pitch with a glass rod is required due to the generation of bubbles in the pitch and the resulting volume expansion during the shearing process.
Example 3
Preparing phase change temperature-adjusting asphalt with the mixing amount of 10 percent: heating asphalt in a baking oven at 140 ℃, pouring the asphalt into an aluminum pot after the asphalt is in a liquid flowing state, weighing the quality, putting the aluminum pot into a heating sleeve, and extending a temperature probe matched with the heating sleeve into the asphalt so as to ensure the control of the temperature of the asphalt in the shearing process. Converting the mass of the required tetradecane-n-octanoic acid phase change microcapsule according to the weighed mass of the asphalt, slowly adding the weighed tetradecane-n-octanoic acid phase change microcapsule into the asphalt in several times, and manually and slowly stirring by using a glass rod until the tetradecane-n-octanoic acid phase change microcapsule is immersed into the asphalt.
Inserting the rotary head of the high-speed shearing machine into the asphalt, adjusting the height of a rod connected with the rotary head to enable the rotary head to be 1-2 cm away from the pot bottom, and setting the rotating speed for shearing for 10 min. The slow and constant stirring of the pitch with a glass rod is required due to the generation of bubbles in the pitch and the resulting volume expansion during the shearing process.
Example 4
Preparing phase change temperature-adjusting asphalt with 13 percent of mixing amount: heating asphalt in a baking oven at 140 ℃, pouring the asphalt into an aluminum pot after the asphalt is in a liquid flowing state, weighing the quality, putting the aluminum pot into a heating sleeve, and extending a temperature probe matched with the heating sleeve into the asphalt so as to ensure the control of the temperature of the asphalt in the shearing process. Converting the mass of the required tetradecane-n-octanoic acid phase change microcapsule according to the weighed mass of the asphalt, slowly adding the weighed tetradecane-n-octanoic acid phase change microcapsule into the asphalt in several times, and manually and slowly stirring by using a glass rod until the tetradecane-n-octanoic acid phase change microcapsule is immersed into the asphalt.
Inserting the rotary head of the high-speed shearing machine into the asphalt, adjusting the height of a rod connected with the rotary head to enable the rotary head to be 1-2 cm away from the pot bottom, and setting the rotating speed for shearing for 10 min. The slow and constant stirring of the pitch with a glass rod is required due to the generation of bubbles in the pitch and the resulting volume expansion during the shearing process.
Performance testing
(1) And respectively preparing penetration degree, softening point and ductility test pieces according to the requirements of road engineering asphalt and asphalt mixture test procedures (JTG-E20-2011) and testing the basic performances of the common asphalt and the phase-change modified asphalt. The results are shown in Table I.
(2) The test pieces required by the temperature regulation test are respectively prepared from the following five kinds of asphalt, namely common asphalt and the phase-change temperature-regulating asphalt with the tetradecane-n-octanoic acid phase-change microcapsule mixing amounts of 4%, 7%, 10% and 13% prepared by using the common asphalt. The temperature regulation test is designed independently, aims to visually evaluate the temperature regulation capability of the phase-change temperature-regulating asphalt, and is designed as follows:
the test asphalt was heated to a fluid state, and 50g of asphalt was weighed into a test dish using a penetration mold. And (3) embedding the temperature measuring probe into the asphalt while weighing. And standing the mold containing the asphalt at room temperature for 3 hours, cooling the asphalt to a solidification state, then preserving the heat in a constant temperature box at 25 ℃ for 1 hour, testing the temperature of the asphalt by using a high-precision temperature detector, and starting a temperature regulation test if the temperature reaches 25 ℃. And (3) placing the asphalt embedded with the temperature measuring probe and kept at the temperature of 25 ℃ and the mould in a constant-temperature absolute ethyl alcohol environment box at the temperature of-2 ℃ for heat preservation. Measuring the temperature once every 1min in the heat preservation process, recording the current internal temperature of different kinds of asphalt, and testing the temperature regulation effect of the phase-change temperature-regulation asphalt through a comparison test. The results are shown in FIG. 1.
Watch 1
Figure BDA0002828711380000081
The first table shows that different tetradecane-n-octanoic acid phase change microcapsule mixing amounts have different degrees of influence on the matrix asphalt, and the trends are that the penetration degree of the asphalt is increased, the softening point of the asphalt is reduced, and the ductility of the asphalt is increased along with the increase of the tetradecane-n-octanoic acid phase change microcapsule mixing amounts. It can be seen that the tetradecane-n-octanoic acid phase change microcapsule can reduce the consistency of asphalt, thereby enhancing the low-temperature crack resistance of asphalt binder. The phase-change temperature-regulating asphalt has the capability of storing heat, can release heat in a low-temperature environment, and delays the cooling speed, so that the low-temperature crack resistance of the asphalt binder is further enhanced. On the other hand, the tetradecane-n-octanoic acid phase change microcapsule is doped to have negative influence on the high-temperature performance of the asphalt.
As can be seen from the figure 1, the asphalt is doped with the tetradecane-n-octanoic acid phase-change microcapsule, so that the cooling rate of the common asphalt in a low-temperature environment can be slowed down. Taking the 5min as an example, the phase-change temperature-regulating asphalt with the mixing amount of the tetradecane-n-octanoic acid phase-change microcapsules of 4%, 7%, 10% and 13% has the temperature respectively higher than that of the common asphalt by 2.9 ℃, 4.6 ℃, 5.9 ℃ and 6.8 ℃; from 15min, the internal temperature of the temperature-regulating asphalt starts to approach the common asphalt and gradually coincides with the common asphalt, which shows that the phase change process of the phase change material in the temperature-regulating asphalt is finished and heat can not be provided for the asphalt binder in the low-temperature environment any more.
The results show that the phase-change temperature-regulating asphalt prepared by the invention can relieve the defect of high cooling speed of the asphalt binder in a low-temperature environment to a certain extent, can improve the low-temperature crack resistance of the asphalt binder, has great practical significance for helping cold resistance and crack resistance of roads in cold regions in winter, and has great market application potential.

Claims (6)

1. The phase-change thermoregulation asphalt is characterized by comprising the following components in parts by mass: tetradecane (50-51), n-octanoic acid (49-51), melamine (15-22.5), formaldehyde (45-67.5), polyvinyl alcohol (0.2-0.5) and TiO (0.5-1)2Nanoparticles, (0.2-0.5) parts SDS, and 93 parts bitumen.
2. The phase-change thermoregulating asphalt as claimed in claim 1, which is characterized by comprising the following components in parts by mass: 50.5 parts of tetradecane, 49.5 parts of n-octanoic acid, 15 parts of melamine, 45 parts of formaldehyde, 0.4 part of polyvinyl alcohol, 0.7 part of TiO2Nanoparticles, 0.3 parts SDS, and 93 parts asphalt.
3. The phase-change thermoregulation asphalt is characterized by comprising the following steps:
step 1, weighing the following components in parts by mass: tetradecane (50-51), n-octanoic acid (49-51), melamine (15-22.5), formaldehyde (45-67.5), polyvinyl alcohol (0.2-0.5) and TiO (0.5-1)2Nanoparticles, (0.2-0.5) parts SDS and 93 parts asphalt;
step 2, mixing the weighed tetradecane and n-octanoic acid to obtain a uniformly mixed tetradecane-n-octanoic acid binary phase change system A;
step 3, mixing the weighed melamine, formaldehyde, polyvinyl alcohol and deionized water to obtain a mixed solution; adjusting the pH value of the obtained mixed solution to 8, and then carrying out constant-temperature water bath reaction to obtain PVA modified melamine formaldehyde resin;
adding TiO into the obtained PVA modified melamine formaldehyde resin2Nanoparticles to obtain doped TiO2PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles;
step 4, mixing the tetradecane-n-octanoic acid binary phase change system A obtained in the step 1 with water to obtain a mixed solution;
adjusting the pH value of the obtained mixed solution to 3-4, adding SDS (sodium dodecyl sulfate) into a constant-temperature water bath for intensive stirring, emulsifying and dispersing, and dripping the doped TiO into the mixed solution during the intensive stirring process2Slowly stirring the PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles after finishing dripping, and obtaining a phase change microcapsule dispersion liquid after finishing the reaction;
step 5, filtering, cleaning and drying the obtained phase change microcapsule dispersion liquid to obtain tetradecane-n-octanoic acid phase change microcapsules;
and 6, slowly adding the tetradecane-n-octanoic acid phase change microcapsule with the mixing amount of 1-10% into the asphalt in the molten state, and slowly stirring until the phase change temperature regulation asphalt is uniformly mixed to prepare the phase change temperature regulation asphalt.
4. A phase change temperature-regulated asphalt according to claim 3, characterized by comprising the following steps:
step 1, weighing the following components in parts by mass: 50.5 parts of tetradecane, 49.5 parts of n-octanoic acid, 15 parts of melamine, 45 parts of formaldehyde, 0.4 part of polyvinyl alcohol, 0.7 part of TiO2 nanoparticles, 0.3 part of SDS and 93 parts of asphalt;
step 2, mixing the weighed tetradecane and n-octanoic acid to obtain a uniformly mixed tetradecane-n-octanoic acid binary phase change system A;
step 3, mixing the weighed melamine, formaldehyde, polyvinyl alcohol and deionized water to obtain a mixed solution; adjusting the pH value of the obtained mixed solution to 8, and then carrying out constant-temperature water bath reaction to obtain PVA modified melamine formaldehyde resin;
adding TiO into the obtained PVA modified melamine formaldehyde resin2Nanoparticles to obtain doped TiO2PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles;
step 4, mixing the tetradecane-n-octanoic acid binary phase change system A obtained in the step 1 with water to obtain a mixed solution;
adjusting the pH value of the obtained mixed solution to 3-4, adding SDS (sodium dodecyl sulfate) into a constant-temperature water bath for intensive stirring, emulsifying and dispersing, and dripping the doped TiO into the mixed solution during the intensive stirring process2Slowly stirring the PVA modified melamine formaldehyde resin wall material prepolymer B of the nano particles after finishing dripping, and obtaining a phase change microcapsule dispersion liquid after finishing the reaction;
step 5, filtering, cleaning and drying the obtained phase change microcapsule dispersion liquid to obtain tetradecane-n-octanoic acid phase change microcapsules;
and 6, slowly adding the tetradecane-n-octanoic acid phase change microcapsule with the mixing amount of 1-10% into the asphalt in the molten state, and slowly stirring until the phase change temperature regulation asphalt is uniformly mixed to prepare the phase change temperature regulation asphalt.
5. The phase-change temperature-regulating asphalt according to claim 3, wherein the process conditions of the constant-temperature water bath reaction in the step 3 and the step 4 are as follows: and carrying out constant-temperature water bath reaction at the temperature of 70 ℃ for 30 min.
6. The phase-change temperature-regulating asphalt of claim 3, wherein in the step 4, the volume ratio of the tetradecane-n-octanoic acid binary phase-change system A to water is 1: 2.
CN202011436128.4A 2020-12-10 2020-12-10 Phase-change thermoregulation asphalt and preparation method thereof Pending CN112625454A (en)

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CN115322752A (en) * 2022-08-26 2022-11-11 中交第四公路工程局有限公司 Preparation method of self-temperature-regulating asphalt pavement phase change microcapsule in large-temperature-difference area

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